CMP v1 Iran

COMPREHENSIVE MATERIALS
PROCESSING
EDITOR-IN-CHIEF
Saleem Hashmi
Dublin City University, Dublin, Ireland
ASSOCIATE EDITORS-IN-CHIEF
Gilmar Ferreira Batalha

University of São Paulo, São Paulo, Brazil
Chester J. Van Tyne
Colorado School of Mines, Golden, CO, USA
Bekir Yilbas
King Fahd University of Petroleum and Minerals, Dhahran, Saudi Arabia
VOLUME 1
ASSESSING PROPERTIES OF CONVENTIONAL

AND SPECIALIZED MATERIALS
VOLUME EDITOR
Chester J. Van Tyne

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EDITOR-IN-CHIEF
Saleem Hashmi graduated from East Pakistan University of Engineering and Technology in 1967,
and in 1972 he completed his master’s and PhD degrees from the University of Manchester. He
was appointed as a postdoctoral fellow with UMIST, Manchester, in January 1973, and in October
1973, he joined Sheffield Hallam University as a lecturer. In 1976, he was promoted to senior
lecturer, then to principal lecturer in 1977, and to reader in 1984.
In January 1987, Professor Hashmi founded the School of Mechanical & Manufacturing Engi-
neering at Dublin City University. While in the process of establishing this school, he attracted
substantial external research funding to set up the Material Processing Research Centre (MPRC),
a research center of excellence in the field of material processing. To this day, he continues his
affiliation with Dublin City University as an emeritus professor in the school he founded 27 years ago.
In 1990, Professor Hashmi established Advances in Materials and Processing Technologies
(AMPT), a much needed international conference in materials processing. He continues to be the
Chairperson of the Steering Committee for this series of conferences. In 1998, he was appointed
as editor-in-chief of Elsevier Journal of Material Processing Technology and continued in this role
until 2008.
In 1995, Professor Hashmi was awarded the higher doctorate degree of DSc, by the University of
Manchester, the highest academic degree any university in the United Kingdom can award.
Professor Hashmi has supervised or co-supervised 110 PhD and 55 MEng research students to successful completion. Over the years,
he has also acted as an external examiner and expert assessor for PhD candidates and engineering departments with universities in Ireland,
the United Kingdom, India, Pakistan, Bangladesh, Hong Kong, Canada, Australia, and Malaysia. He is a Chartered Engineer (CEng), a Fellow
of the Institution of Mechanical Engineers, UK (FIMechE) and also a Fellow of the Institution of Engineers of Ireland (FIEI). He has
published over 430 papers and 12 books and is still publishing.
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EDITORIAL BOARD
Chester J. Van Tyne is the FIERF (Forging Industry Education and Research Foundation) professor
at Colorado School of Mines (CSM) in Golden, Colorado. He received his undergraduate and
graduate degrees from Lehigh University and worked for Bethlehem Steel as a research engineer for
a short period before joining Lafayette College in the Metallurgical Engineering Department as
a professor in 1980. In 1988, he joined the Metallurgical and Materials Engineering Department at
CSM. He is actively engaged in the research operations of the Advanced Steel Processing and
Products Research Center at CSM. His research interests are in metal deformation processes
especially forging, sheet stamping, and friction during metalworking operations.
Gilmar F. Batalha graduated as a mechanical engineer from the University of Brasilia in 1982. He
completed his MSc in Mechanical Engineering at the Federal University of Santa Catarina (1987),
his PhD in Mechanical Engineering (1995) and habilitation/livre-docencia in manufacturing
processes (2010) at the Department of Mechatronics and Mechanical Systems, Polytechnic School
of Engineering, University of Sao Paulo, where he has been a tenured professor since 1989. He has
had postdoctoral research experience at the Friedrich Alexander University Erlangen–Nuremberg,
Germany (1997–98). He was a visiting professor at Ecole Centrale de Lille, France (2004–06), and
at the Faculty of Mechanical Engineering of the Silesian University of Technology, Gliwice, Poland
(2012–13). He served as an adjunct professor at the Faculty of Engineering, UDESC, Joinville, Brazil
(1984–89). He has been an advisor on several PhD theses and master’s dissertations, coordinator
of the Laboratory of Manufacturing Engineering of the EPUSP, and is responsible for several
international and national cooperation agreements for exchange of students and researchers as well
as for consultancy with the industry. He is the volume editor for the Materials Modeling and
Characterization volume in Elsevier’s Comprehensive Materials Processing series.
Sergio T. Button received his PhD in Mechanical Engineering from School of Mechanical Engi-
neering, University of Campinas, Brazil, in 1990. He is currently full professor of Manufacturing
Processes at the University of Campinas. His main research fields include metal forming and
numerical simulation. Currently, his research is focused on cross wedge rolling and hot stamping.
He is the coauthor of 2 books and more than 100 papers in international journals and conferences.
He is the editor and reviewer of many international journals, and participates in the organization of
three national and international scientific conferences.
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viii Editorial Board
David Cameron is currently scientific advisor to Miktech Oy, Finland, and adjunct professor in
Dublin City University, Ireland. From 2003 to 2013, he was professor of Material Technology in
Lappeenranta University of Technology, Finland, where he established the Advanced Surface
Technology Research Laboratory (ASTRaL). He obtained his doctorate from the University of
Glasgow in 1980 and has spent his research career working on thin-film technology. He was
a senior research fellow at the Royal Signals and Radar Establishment in the United Kingdom until
1982 when he joined the School of Electronic Engineering at Dublin City University, becoming
associate professor. His research focus is on atomic layer deposition and its industrialization.
Joseph A. McGeough is an honorary professorial fellow in the School of Engineering at the

University of Edinburgh. He is a graduate from the universities of Glasgow (BSc and PhD) and
Aberdeen (DSc). He held research appointments at the universities of Leicester, Queensland, and
Strathclyde. As a student he gained numerous county, university, and national championship
athletic awards. His industrial training began as an undergraduate vacation apprentice for a firm of
electrical contractors based at ICI ltd Nobel Division, and he subsequently undertook postgraduate
experience at International Research and Development, Newcastle upon Tyne, before returning to
university service. He was successively a lecturer, senior lecturer, and reader in Engineering at
Aberdeen University, and then moved to Edinburgh University to take up its Regius Chair of
Engineering. His research work has dealt mainly with manufacturing processes for which he has
been awarded Institution of Mechanical Engineers and the Society for Underwater Technology
prizes. He has been the recipient of a Royal Society/SERC (Science and Engineering (now Engi-
neering and Physical Sciences) Research Council) Industrial Fellowship in order to transfer the
results of his research to industry. His publications include Principles of Electrochemical Machining,
Advanced Methods of Machining, and Micromachining of Engineering Materials (editor). His latest book
is The Engineering of Human Joint Replacements (2013), which contains details of the materials and
manufacturing processes used in this field. He is a fellow of the Institution of Mechanical Engi-
neers, International Academy for Production Engineering, Royal Society of Edinburgh, and Royal
Academy of Engineering.
Emin Bayraktar is a full university professor and research director at Supmeca/Paris, School of
Mechanical and Manufacturing Engineering, Paris, France. He was awarded a PhD degree in
Mechanical Engineering by IST/OSU and a second PhD degree in Materials Science and Engi-
neering in Paris. Subsequently, Professor Bayraktar was awarded a higher doctorate degree of
habilitation (DSc) in Mechanics of Materials in recognition of his research contributions at
Paris 6, University Marie-Curie. His teaching and research expertise lies on the processing and
manufacturing of the composite materials and damage analysis. Recently he has been appointed
as an adjunct professor in UNICAMP-Campinas, Brazil, on the new design of composites for the
application in aeronautical engineering. He is on the editorial board of a number of scientific
journals. He is also a member of the Steering Committee for the International Conference Series
on Advances in Materials and Processing Technologies (AMPT).
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Editorial Board ix
Bekir S. Yilbas received his PhD degree in Mechanical Engineering from Birmingham University.
He was awarded the Doctor of Engineering degree in 2005 by Birmingham University due to his
significant contribution to his field of study. He has published 375 journal papers in reputable
international journals and presented over 60 papers at international conferences. He has served
as an editorial board member of international journals, including International Journal of Machine
Tool and Manufacture Design, Research and Application, International Journal of Subsurface Sensing
Technologies and Applications, Journal of Materials Processing Technology, Journal of Achievements in
Materials and Manufacturing Engineering, International Journal of Nanomanufacturing, and Archives of
Materials Science and Engineering. He has received numerous awards in recognition of his research
work.
Nabil Bassim was born and raised in Cairo, Egypt. Dr. Bassim received a BSc in Chemical Engi-
neering from Cairo University in 1965. He went to the University of Virginia, United States, where
he received his MSc in Chemical Engineering (Nuclear Engineering option), and a PhD in Materials
Science in 1973. He moved to Canada where he is now professor of Materials Science and Engi-
neering at the University of Manitoba. He served for years as associate dean of research at the
Faculty of Engineering and was director of International Programs for the faculty. His areas of
research interest include mechanisms and mechanics of plastic deformation, dislocation theory,
fracture and fatigue, and nondestructive evaluations. He has patents on the use of acoustic emission
for monitoring of structures. He also has an interest in studying the behavior of materials at high
strain rates and large strains as they affect processes such as metal forming and machining. He has
published over 120 papers and supervised numerous MSc and PhD theses.
Syed H. Masood is professor of Mechanical and Manufacturing Engineering at Swinburne

University of Technology in Melbourne, Australia, where he is also the program coordinator of the
master’s program in advanced manufacturing technology. He obtained his PhD from the University
of Queensland, Australia; MEng from the University of New Brunswick, Canada; PG Dip from IIT
Delhi; and BSc Eng Hons from Aligarh Muslim University, India. Professor Masood has worked
previously at Central Queensland University, Rockhampton, and PNG University of Technology,
Papua New Guinea. He has published over 275 technical articles in international journals, books,
and conferences in different areas of advanced manufacturing. His current research interests include
additive manufacturing technologies, especially fused deposition modeling and direct metal
deposition, plastics manufacturing processes, material development, and material characterization.
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x Editorial Board
Mustafizur Rahman is currently a professor at the Department of Mechanical Engineering at

National University of Singapore (NUS), and has been with NUS since 1982. He obtained his BSc
in Engineering from Bangladesh University of Engineering and Technology (BUET), MEng and PhD
from Tokyo Institute of Technology, Japan. His research interests include micro-/nanomachining,
design and development of miniature machine tools and devices for micro-/nanomachining, and
high-speed machining of difficult-to-machine materials. He has received Outstanding Achievement
Awards from the Singapore Institute of Engineers and the Japan Society of Mechanical Engineers in
2003 and 2005, respectively.
George Krauss is currently university emeritus professor at the Colorado School of Mines and
a metallurgical consultant specializing in steel microstructural systems. Dr. Krauss received the BSc
in Metallurgical Engineering from Lehigh University in 1955 and the MSc and ScD degrees in
Metallurgy from the Massachusetts Institute of Technology in 1958 and 1961, respectively, after
working at the Superior Tube Company as a development engineer in 1956. In 1962–63, he was an
NSF postdoctoral fellow at the Max Planck Institut für Eisenforschung in Düsseldorf, Germany. He
served at Lehigh University as assistant professor, associate professor, and professor of Metallurgy
and Materials Science from 1963 to 1975, and in 1975 joined the faculty of the Colorado School of
Mines as the AMAX Foundation professor in Physical Metallurgy. He was the John Henry Moore
professor of Metallurgical and Materials Engineering at the time of his retirement from the Colo-
rado School of Mines in 1997.
In 1984, Dr. Krauss was a principal in the establishment of the Advanced Steel Processing and
Products Research Center, an NSF Industry-University cooperative research center at the Colorado
School of Mines, and served as its first director until 1993. He has authored the book Steels: Pro-
cessing, Structure, and Performance, (ASM International, 2005), coauthored the book Tool Steels, fifth
edition, (ASM International, 1998), and edited or coedited conference volumes on tempering of
steel, carburizing, zinc-based coatings on steel, and microalloyed forging steels. He has published
over 330 papers and lectured widely in technical conferences, universities, corporations, and ASM
International chapters, presenting a number of keynote, invited, and honorary lectures. He presented the Edward DeMille Campbell
Memorial Lecture of ASM International in 2000, the Howe Memorial Lecture of ISS in 2003, and the Adolf Martens Memorial Steel Lecture of
AIST in 2010.
Dr. Krauss has served as the president of the International Federation of Heat Treatment and Surface Engineering (IFHTSE), 1989–91,
and as President of ASM International, 1996–97. He is a fellow of ASM International, TMS, and IFHTSE. He has been awarded the Adolf
Martens Medal of the German Society for Heat Treatment and Materials, the Charles S. Barrett Silver Medal of the Rocky Mountain Chapter
of ASM, the George Brown Gold Medal of the Colorado School of Mines, and several other professional and teaching awards, including the
ASM Albert Easton White Distinguished Teacher Award in 1999. He is an honorary member of the Iron and Steel Institute of Japan,
a distinguished member of the Iron and Steel Society, an honorary member of ASM International, and an honorary member of the Japan
Institute of Metals.
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CONTRIBUTORS TO VOLUME 1
T. Akter C. Leppin
Dublin City University, Dublin, Ireland Suisse Technology Partners Ltd., Neuhausen am
Rheinfall, Switzerland
R. Bagheriasl
University of Waterloo, West Waterloo, E. Lucon
ON, Canada National Institute for Standards and Technology,
Boulder, CO, USA
F.G. Caballero
National Center for Metallurgical Research D.K. Matlock
(CENIM-CSIC), Madrid, Spain Colorado School of Mines, Golden, CO, USA
D.V. Edmonds M. Militzer
University of Leeds, Leeds, United Kingdom The University of British Columbia, Vancouver, BC,
Canada
H. Friebe
GOM mbH, Braunschweig, Germany R. Müller
Fraunhofer-Institut für Werkzeugmaschinen und
C. Garcia-Mateo
Umformtechnik IWU, Chemnitz, Germany
National Center for Metallurgical Research
(CENIM-CSIC), Madrid, Spain C.J.G. Plummer
Ecole Polytechnique Fédérale de Lausanne (EPFL),
J. Haider
Lausanne, Switzerland
Manchester Metropolitan University, Manchester,
United Kingdom M. Rahman
University College Dublin, Dublin, Ireland
T. Hallfeldt
Ford Werke GmbH, Köln, Germany G.S. Schajer
The University of British Columbia, Vancouver, BC,
M.S.J. Hashmi
Canada
Dublin City University, Dublin, Ireland
J.G. Speer
W. Hotz
Novelis Innovation Centre, Sierre, Switzerland
T.B. Stoughton
S. Keller
General Motors Global Research and Development
Hydro Aluminium Research & Development, Bonn,
Center, Warren, MI, USA
Germany
D.G. Tari
S. Kurukuri
University of Waterloo, West Waterloo, ON, Canada
University of Waterloo, West Waterloo, ON, Canada
E.T. Till
T. Kuwabara
voestalpine Stahl GmbH, Linz, Austria
Tokyo University of Agriculture and Technology,
Koganei-shi, Tokyo, Japan C.J. Van Tyne
M.J. Lance
Oak Ridge National Laboratory, Oak Ridge, H. Vegter
TN, USA Tata Steel Research, Development & Technology,
CA Ijmuiden, The Netherlands
xi
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xii Contributors to Volume 1
M. Vu!ceti"c M.J. Worswick

Leibniz Universität Hannover, Garbsen, Germany University of Waterloo, West Waterloo, ON, Canada
L. Wang J.W. Yoon
Automotive Steel Research Institute, Shanghai, China Deakin University, Geelong Waurn Ponds, VIC,
and Baoshan Iron & Steel Co., Ltd, Shanghai, China Australia
T.R. Watkins
Oak Ridge National Laboratory, Oak Ridge, TN, USA
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CONTENTS OF VOLUME 1
Editor-in-Chief v
Editorial Board vii
Contributors to Volume 1 xi
Contents of All Volumes xv
Preface xxvii
1.01 Introduction to Assessing Properties of Conventional and Specialized Materials 1

C J Van Tyne
1.02 Techniques for Assessing the Properties of Advanced Ceramic Materials 3
M Rahman, J Haider, T Akter and M S J Hashmi
1.03 Testing of Polymeric Materials 35
C J G Plummer
1.04 Stress-Based Forming Limit Curves 71
T B Stoughton and J W Yoon
1.05 Sheet Bulge Testing 85
T Hallfeldt, W Hotz, C Leppin, S Keller, H Friebe, E T Till, R Müller, M Vu!ceti"c and H Vegter
1.06 Biaxial Stress Testing Methods for Sheet Metals 95
T Kuwabara
1.07 Residual Stress Measurements 113
T R Watkins, G S Schajer and M J Lance
1.08 Testing of Small-Sized Specimens 135
E Lucon
1.09 Advanced High Strength Bainitic Steels 165
C Garcia-Mateo and F G Caballero
1.10 Thermomechanical Processed Steels 191
M Militzer
1.11 Quenched and Partitioned Steels 217
J G Speer, D K Matlock, L Wang and D V Edmonds
1.12 Material Properties for Numerical Calculations 227
R Bagheriasl, D G Tari, S Kurukuri and M J Worswick
xiii
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CONTENTS OF ALL VOLUMES
Volume 1 Assessing Properties of Conventional and Specialized Materials

1.01 Introduction to Assessing Properties of Conventional and Specialized Materials
C J Van Tyne
1.02 Techniques for Assessing the Properties of Advanced Ceramic Materials
M Rahman, J Haider, T Akter and M S J Hashmi
1.03 Testing of Polymeric Materials
C J G Plummer
1.04 Stress-Based Forming Limit Curves
T B Stoughton and J W Yoon
1.05 Sheet Bulge Testing
T Hallfeldt, W Hotz, C Leppin, S Keller, H Friebe, E T Till, R Müller, M Vu!ceti"c and H Vegter
1.06 Biaxial Stress Testing Methods for Sheet Metals
T Kuwabara
1.07 Residual Stress Measurements
T R Watkins, G S Schajer and M J Lance
1.08 Testing of Small-Sized Specimens
E Lucon
1.09 Advanced High Strength Bainitic Steels
C Garcia-Mateo and F G Caballero
1.10 Thermomechanical Processed Steels
M Militzer
1.11 Quenched and Partitioned Steels
J G Speer, D K Matlock, L Wang and D V Edmonds
1.12 Material Properties for Numerical Calculations
R Bagheriasl, D G Tari, S Kurukuri and M J Worswick
Volume 2 Materials Modeling and Characterization

2.01 Introduction to Materials Modeling and Characterization
G F Batalha
2.02 Phase Transformations and Characterization of a þ b Titanium Alloys
M Motyka, K Kubiak, J Sieniawski and W Ziaja
2.03 Polymeric Materials Characterization and Modeling
D J Dos Santos, D J Carastan, L B Tavares and G F Batalha
xv
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xvi Contents of All Volumes
2.04 Ultrasonic Characterization of Anisotropic Materials

F Buiochi, M A B Andrade, N Perez and J C Adamowski
2.05 Application of Optical Techniques to Materials Characterization and Modeling
F C Trigo, O Sanchez and F P R Martins
2.06 Material Behavior at a Wide Range of Strain Rates
M Alves
2.07 Damage Modeling in Composite Structures
M V Donadon and S F M de Almeida
2.08 Creep Age Forming Modeling and Characterization
G F Batalha, E F Prados, F C Ribeiro, B T Scarpin, D J Inforzato, P R Costa Jr and D N Travessa
2.09 Use of Neural Networks and Artificial Intelligence Tools for Modeling, Characterization,
and Forecasting in Material Engineering
nski, J Trzaska and A D Dobrza"
L A Dobrza" nska-Danikiewicz
2.10 Structure and Mechanical Properties of High-Manganese Steels
L A Dobrza"nski, W Borek and J Mazurkiewicz
2.11 Modeling and Characterization of Residual Stresses in Material Processing
G H Bolognesi Donato and R Magnabosco
2.12 Modeling of Plastic Yielding, Anisotropic Flow, and the Bauschinger Effect
M-G Lee and F Barlat
2.13 Modeling of Functionally Graded Materials
S L Vatanabe, W M Rubio and E C N Silva
Volume 3 Advanced Forming Technologies

3.01 Introduction to Advanced Forming Technologies
S T Button
3.02 Incremental Sheet Forming
M B Silva and P A F Martins
3.03 Hot Stamping
S Bruschi and A Ghiotti
3.04 Tube Hydroforming (Internal High-Pressure Forming)
S J Yuan and G Liu
3.05 Development of Microstructures and Textures by Cross Rolling
S Suwas and N P Gurao
3.06 Multipoint Forming
M Z Li, Q G Han, Z Y Cai, C G Liu and S Z Su
3.07 Dieless Drawing of Bars, Rods, Tubes, and Wires
P Tiernan
3.08 Forming of Metal Matrix Composites
L Ceschini, A Morri and F Rotundo
3.09 Development of Ultrafine-Grained Metals by Equal-Channel Angular Pressing
E A Prokofiev, A M Jorge Jr, W J Botta and R Z Valiev
3.10 Cross-Wedge Rolling
Z Pater
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Contents of All Volumes xvii
3.11 Improvement of Mechanical and Physical Properties in Powder Metallurgy

J M Torralba
3.12 Peen Forming
A Gariépy, H Miao and M Lévesque
3.13 High-Speed Forming of Magnesium Alloy Sheets
I Ulacia
3.14 Hot Rolling and Direct Cooling
S Serajzadeh
3.15 Advanced Techniques to Evaluate Hot Workability of Materials
K P Rao and Y V R K Prasad
3.16 Near-Net and Net Shape Forging
B-A Behrens, A Bouguecha, I Lüken, A Klassen and D Odening
3.17 Texture Control in Aluminum Sheets by Conventional and Asymmetric Rolling
J Sidor, R H Petrov and L Kestens
Volume 4 Films and Coatings: Technology and Recent Development

4.01 Introduction to Films and Coatings: Technology and Recent Development
D Cameron
4.02 Cathodic-Arc and Thermal-Evaporation Deposition
J Koskinen
4.03 Magnetron Sputtering
G Bräuer
4.04 High Power Impulse Magnetron Sputtering e HIPIMS
R Bandorf, V Sittinger and G Bräuer
4.05 Atomic Layer Deposition
M Leskelä, J Niinistö and M Ritala
4.06 Laser Ablation
D Zhang and L Guan
4.07 Surface Processing Using Cold Atmospheric Pressure Plasmas
D P Dowling
4.08 Ion Beam Deposition: Recent Developments
N Toyoda and S Matsui
4.09 Plasma Polymer Deposition and Coatings on Polymers
D Hegemann
4.10 Thermal Spray Coating Processes
P Vuoristo
4.11 Electroplating and Electroless Plating
A Yli-Pentti
4.12 Plasma Sources in Thin Film Deposition
Y Setsuhara
4.13 Hard Nanocomposite Coatings
J Musil, P Zeman and P Baroch
4.14 Protective Transition Metal Nitride Coatings
P H Mayrhofer, R Rachbauer, D Holec, F Rovere and J M Schneider
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xviii Contents of All Volumes
4.15 Advanced Carbon-Based Coatings

E Broitman and L Hultman
4.16 Photocatalytic Coatings
P Pichat
4.17 Biocompatible Coating
Y Qiao and X Liu
4.18 Antimicrobial Bioactive Polymer Coatings
R Förch, L Duque and A Lotz
4.19 Thin-Film Diffusion Barriers for Electronic Applications
P F Carcia
4.20 Diffusion Barrier Layers for Edible Food Packaging
S Desobry and E Arab-Tehrany
4.21 Large-Scale Industrial Coating Applications and Systems
R Tietema
Volume 5 Casting, Semi-Solid Forming and Hot Metal Forming

5.01 Introduction to Casting, Semi-Solid Forming and Hot Metal Forming
J A McGeough
5.02 Advanced Casting Methodologies: Inert Environment Vacuum Casting and Solidification,
Die Casting, Compocasting, and Roll Casting
P Kapranos, D Brabazon, S P Midson, S Naher and T Haga
5.03 Advanced Casting Methodologies: Investment Casting, Centrifugal Casting, Squeeze Casting,
Metal Spinning, and Batch Casting
P Kapranos, C Carney, A Pola and M Jolly
5.04 Rapid Solidification Processing and Bulk Metallic Glass Casting
S N Aqida, L H Shah, S Naher and D Brabazon
5.05 Single-Crystal Casting/Directional Solidification
H Dong and H Dai
5.06 Semisolid Processes
G Govender, H Möller and O F R A Damm
5.07 Routes to Spheroidal Starting Material for Semisolid Metal Processing
A H Ahmad, S Naher, S N Aqida and D Brabazon
5.08 Rheology of Semisolid Metallic Alloys
H V Atkinson
5.09 Alloys for Semisolid Processing
E J Zoqui
5.10 Modeling of Semisolid Flow
V Favier
5.11 Tribology in Hot Forging
B-A Behrens, A Bouguecha, I Lüken, J Mielke and M Bistron
5.12 Casting Simulation Methods
T S Prasanna Kumar
5.13 Industrial Practice and Applications
S P Midson
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Contents of All Volumes xix
5.14 Hot Forging

S Debin and Y Lin
5.15 Deformation Rules and Mechanism of Large-Scale Profiles Extrusion
of Difficult-to-Deform Materials
L Guo and H Yang
5.16 Hot Tube-Forming
H Li, H Yang and Z Zhang
5.17 Hot Stamping
J Chen, X Li and X Han
5.18 Superplastic Forming
K F Zhang and S S Jiang
5.19 Hot Shape Rolling
L Li, H Yang and L Guo
5.20 Modeling of Hot Forging
M Zhan, Z Sun and H Yang
Volume 6 Welding and Bonding Technologies

6.01 Introduction to Welding and Bonding Technologies
E Bayraktar
6.02 Welding Processes and Technologies
M Vural
6.03 Manual Metal Arc Welding and Gas Metal Arc Welding
M A Wahab
6.04 Robotic Welding Technology
T S Hong, M Ghobakhloo and W Khaksar
6.05 Mathematical Modeling of Weld Phenomena, Part 1: Finite-Element Modeling
A G Olabi and G Casalino
6.06 Mathematical Modeling of Weld Phenomena, Part 2: Design of Experiments and Optimization
A G Olabi, A Alaswad and K Y Benyounis
6.07 Welding Defects and Implications on Welded Assemblies
F Yusof and M F Jamaluddin
6.08 9% Nickel Steels and Their Welding Behavior
Q Ahsan, A S M A Haseeb, N I Syahriah Binti Hussein and S Y Chang
6.09 Weldability of Nickel-Base Alloys
J L Caron and J W Sowards
6.10 Review of Microstructures, Mechanical Properties, and Residual Stresses of Ferritic and Martensitic
Stainless-Steel Welded Joints
A G Olabi, R Lostado and K Y Benyounis
6.11 Quality Control in Welding Process
A G Olabi, R L Lorza and K Y Benyounis
6.12 Safety and Security Conditions in Welding Processes
T S Hong and M Ghobakhloo
6.13 Optimum Speed of Friction Stir Welding on 304L Stainless Steel by Finite Element Method
S Sulaiman and S Emamian
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xx Contents of All Volumes
6.14 Bonding Technologies in Manufacturing Engineering

S M Homayouni, M R Vasili and T S Hong
Volume 7 Nano- and Microscale Processing e Modeling

7.01 Introduction to Nano- and Microscale Processing e Modeling
B S Yilbas
7.02 Micro/Nano Scale Energy Transport in Metallic Films and Stress Analysis:
Analytical Approaches
B S Yilbas, A Y Al-Dweik and S B Mansour
7.03 Thermal Stresses in Micro- and Nanostructures
B S Yilbas
7.04 PVD Technology in Fabrication of Micro- and Nanostructured Coatings
M Aliofkhazraei and N Ali
7.05 Fabrication of Micro/Nanostructured Coatings by CVD Techniques
7.06 Fabrication and Properties of Micro- and Nanostructured Coatings Using Electrochemical
Depositions
7.07 Thin Film Coating for Polymeric Micro Parts
L Xie, D Abliz and D Li
7.08 Electric FieldeAssisted Chemical Vapor Deposition for Nanostructured Thin Films
M E A Warwick, L-M Romero-Nunez, A J T Naik and R Binions
7.09 AFM Applications in Micro/Nanostructured Coatings
7.10 Application and Advances in Microprocessing of Natural Fiber (Jute)eBased Composites
M M Alam, M Maniruzzaman and M M Morshed
Volume 8 Health, Safety and Environmental Issues

8.01 Introduction to Health, Safety and Environmental Issues
M N Bassim
8.02 Health and Environmental Impacts in Metal Machining Processes
J Haider and M S J Hashmi
8.03 Health and Safety Issues in Emerging Surface Engineering Techniques
M Rahman, J Haider and M S J Hashmi
8.04 Health Effects Associated with Welding
J M Antonini
8.05 Ceramic Manufacturing Processes: Energy, Environmental, and Occupational Health Issues
E Monfort, A Mezquita, E Vaquer, I Celades, V Sanfelix and A Escrig
8.06 A Review of Engineered Nanomaterial Manufacturing Processes and Associated Exposures
M A Virji and A B Stefaniak
8.07 Administrative Evil and Patient Health: A Critique of the Impact of Manufacturing Systems
on Health Care
L Stapleton
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Contents of All Volumes xxi
8.08 Assessment of Impacts to Health, Safety, and Environment in the Context of Materials
Processing and Related Public Policy
M V Pohjola
8.09 Environmentally friendly Manufacturing Processes in the Context of Transition
to Sustainable Production
D Fratila
8.10 Health and Safety in Today’s Manufacturing Industry
S Geldart
8.11 Economic Implications of Impact of Manufacturing on Environment and Health
M N Bassim
Volume 9 Laser Machining and Surface Treatment

9.01 Introduction to Laser Machining and Surface Treatment
B S Yilbas
9.02 Laser Heating and the Phase Change Process
B S Yilbas
9.03 Laser Treatment of Steel Surfaces: Numerical and Experimental Investigations
of Temperature and Stress Fields
S S Akhtar and B S Yilbas
9.04 Laser Plasma Interaction and Shock Material Processing
J L Ocaña, M Morales, J A Porro, M Díaz, L Ruiz de Lara and C Correa
9.05 Laser Surface Patterning
H Hocheng, H Y Tsai, U U Jadhav, K Y Wang and T C Lin
9.06 Laser Drilling of Metallic and Nonmetallic Substrates
A K Nath
9.07 Laser Drilling of Metallic and Nonmetallic Materials and Quality Assessment
K T Voisey
9.08 Laser Drilling and Efficiency Analysis
A Z Sahin, B S Yilbas and T Ayar
9.09 Thermal Modeling of Laser Machining Process
S Subramonian
9.10 Laser Machining and Laser-Assisted Machining of Ceramics
X Dong and Y C Shin
9.11 Laser Cutting Efficiency and Quality Assessments
A Z Sahin, B S Yilbas and T Ayar
9.12 Laser Applications in the Field of Plastics
L Santo, F Trovalusci and J P Davim
9.13 Laser GaseAssisted Nitriding of Ti Alloys
P Schaaf, J Kaspar and D Höche
9.14 Laser Duplex Treatment of Surfaces for Improved Properties
B S Yilbas
9.15 Laser Surface Treatment and Efficiency Analysis
A Z Sahin, B S Yilbas and S S Akhtar
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xxii Contents of All Volumes
Volume 10 Advances in Additive Manufacturing and Tooling

10.01 Introduction to Advances in Additive Manufacturing and Tooling
S H Masood
10.02 Additive Manufacturing: An Overview
O Diegel
10.03 Stereolithography
K Salonitis
10.04 Advances in Fused Deposition Modeling
S H Masood
10.05 Selective Laser Sintering/Melting
S Kumar
10.06 Electron Beam Melting
L E Murr and S M Gaytan
10.07 Laser Powder Deposition
R Vilar
10.08 Three Dimensional Printing
D Dimitrov, N de Beer, P Hugo and K Schreve
10.09 Tissue Engineering Applications of Additive Manufacturing
K-F Leong, D Liu and C-K Chua
10.10 Recent Advances in Additive Biomanufacturing
R F Pereira and P J Bártolo
10.11 Laser-Assisted Additive Manufacturing for Metallic Biomedical Scaffolds
S H Riza, S H Masood and C Wen
10.12 Direct Rapid Tooling
S Rahmati
10.13 Indirect Rapid Tooling
Nagahanumaiah and B Ravi
10.14 CAD Issues in Additive Manufacturing
E S A Nasr, A Al-Ahmari and K Moiduddin
Volume 11 Advanced Machining Technologies

11.01 Introduction to Advanced Machining Technologies
M Rahman, A B M A Asad and Y S Wong
11.02 Machine Tools for Micro- and Nanometer Scale Processing
H Shinno
11.03 Continuum Micromechanics and Molecular Dynamics Simulation
X Li
11.04 Fast and Fine Tool Servo for Ultraprecision Machining
A Senthil Kumar, M R Aravind Raghavendra, W K Neo and M Rahman
11.05 Compound and Hybrid Micromachining Processes
M Rahman, A B M A Asad, Y S Wong, M P Jahan and T Masaki
11.06 Compound and Hybrid Micromachining: Part II e Hybrid Micro-EDM and Micro-ECM
M Rahman, Y S Wong and M D Nguyen
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Contents of All Volumes xxiii
11.07 Micromilling
T Matsumura
11.08 Fundamentals and Modeling of Micro-End Milling Operation
M Arif and M Rahman
11.09 Diamond Turning
X Q Zhang, K S Woon and M Rahman
11.10 High-Speed Machining
Z Wang and M Rahman
11.11 Machining with Least Quantity Lubrication
T Obikawa
11.12 Burr Formation in Machining Processes: A Review
I A Choudhury and S A Lawal
11.13 Heat-Assisted Machining
A K M Nurul Amin and T L Ginta
11.14 Micro-Electrical Discharge Machining (Micro-EDM): Processes, Varieties, and Applications
M P Jahan, M Rahman and Y S Wong
11.15 Electrochemical Micromachining
S S Joshi and D Marla
11.16 Ultrasonic Vibration Diamond Cutting and Ultrasonic Elliptical Vibration Cutting
E Shamoto and N Suzuki
11.17 Ultrasonic Vibration Cutting: Part II e Ductile Cutting and Analytical Force Models
for the Elliptical Vibration Cutting Process
C Nath, X Zhang, A Senthil Kumar and M Rahman
11.18 Electrolytic In-Process Dressing (ELID) Grinding for Nano-Surface Generation
T Saleh and M Rahman
11.19 Microelectrochemical Deposition
M A Habib
Volume 12 Thermal Engineering of Steel Alloy Systems

12.01 Introduction to Thermal Engineering of Steel Alloy Systems
G Krauss
12.02 Introduction to Steel Heat Treatment
L C F Canale, J Vatavuk and G E Totten
12.03 Hardenability of Steel
L C F Canale, L Albano, G E Totten and L Meekisho
12.04 Controlling the Cooling Process e Measurement, Analysis, and Quality Assurance
E Troell, H Kristoffersen, J Bodin and S Segerberg
12.05 Calculation of the Heat Transfer Coefficient Based on Experiments by the Liscic Probes
B Li!s!ci"c and S Singer
12.06 Metallo-Thermo-Mechanical Coupling in Quenching
T Inoue
12.07 Intensive Quenching
N I Kobasko and M A Aronov
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xxiv Contents of All Volumes
12.08 Residual Stresses Produced by Quenching of Martensitic Steels

T Ericsson
12.09 Distortion Engineering: Basics and Application to Practical Examples of Bearing Races
T Lübben, F Hoffmann and H-W Zoch
12.10 Austenite Formation and Microstructural Control in Low-Alloy Steels
K D Clarke
12.11 Quench and Tempered Martensitic Steels: Microstructures and Performance
G Krauss
12.12 Microstructure and Properties of Gas Carburized Steels
J Grosch
12.13 Development of Compound Layer and Diffusion Zone during Nitriding and Nitrocarburizing
of Iron and Steels
M A J Somers
12.14 Case Structure and Properties of Nitrided Steels
H-J Spies and A Dalke
12.15 Induction Hardening: Technology, Process Design, and Computer Modeling
V I Rudnev and D Loveless
12.16 Microstructures and Mechanical Performance of Induction-Hardened Medium-Carbon Steels
A B Nissan and K O Findley
Volume 13 Sensor Materials, Technologies and Applications

13.01 Introduction to Sensor Materials, Technologies and Applications
M S J Hashmi
13.02 Review of Physical Principles of Sensing and Types of Sensing Materials
E Spain and A Venkatanarayanan
13.03 Review of Recent Developments in Sensing Materials
A Venkatanarayanan and E Spain
13.04 Coatings for Optical Fiber Sensors
J Goicoechea, M Hernáez, C R Zamarreño and F J Arregui
13.05 Issues of Connectivity, Durability, and Reliability of Sensors and Their Applications
I A Choudhury, A Hossain and S H Bhuiyan
13.06 Commercialization and Application-Driven Economic Viability of Sensor Technology
M Niedermayer
13.07 Structural Properties and Sensing Characteristics of Sensing Materials
T-M Pan and S Mondal
13.08 Developments in Semiconducting Oxide-Based Gas-Sensing Materials
M M Arafat, A S M A Haseeb and S A Akbar
13.09 Properties and Customization of Sensor Materials for Biomedical Applications
C Zuliani, V F Curto, G Matzeu, K J Fraser and D Diamond
13.10 Recent Developments in Miniaturization of Sensor Technologies and Their Applications
13.11 Optical Spin Generated by a Modified Add-Drop Filter for Network Sensors
P P Yupapin
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Contents of All Volumes xxv
13.12 Development of an Integrated Electrochemical Sensing System to Monitor Port Water Quality
Using Autonomous Robotic Fish
V I Ogurtsov, K Twomey and G Herzog
13.13 Wireless Sensor Networks: From Real World to System Integration e Alternative Hardware Approaches
J Portilla, A Otero, V Rosello, J Valverde, Y E Krasteva, E de la Torre and T Riesgo
13.14 Vision-Based Sensor Technologies e Webcam: A Multifunction Sensor
U Buyuksahin
13.15 Application FieldeSpecific Synthesizing of Sensing Technology: Civil Engineering Application
of Ground-Penetrating Radar Sensing Technology
A Benedetto and F Benedetto
13.16 Sensor Technology for Monitoring of Health-Related Conditions
Y Omura
13.17 Developments of Laser Fabrication Methods for Lab-on-a-Chip Microfluidic
Multisensing Devices
A B Azouz, M Vázquez and D Brabazon
13.18 Sensor Technology for a Safe and Smart Living Environment for the Aged
and Infirm at Home
C D Nugent, S I McClean, I Cleland and W Burns
13.19 Sensor-Controlled Intelligent Vehicle Systems: Demand and Needs for a Global Automotive Landscape
A Hossain and A Rahman
13.20 Technical and Economic Feasibility of Sensor Technology for Health/Environmental
Condition Monitoring
A N M Karim, A N Nordin and S Begum
13.21 Multimodal Sensing by a Vision-Based Tactile Sensor Using a Deformable Touchpad
Y Ito, G Obinata, Y Kim and C Nagai
13.22 Review of Sensor Applications in Tool Condition Monitoring in Machining
M S H Bhuiyan and I A Choudhury
13.23 Review of the Reliability and Connectivity of Wireless Sensor Technology
M M Ahsan, M Hasanuzzaman, A G Olabi and M S J Hashmi
Index
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PREFACE
In recent years considerable advances have taken place in materials and their processing technologies, the pace
of which is progressing at an accelerated rate. It is therefore vitally important that researchers, academics, design
engineers, and manufacturing technologists be up to date with these new developments. Such developments
open up excellent opportunities to improve effective utilization of material resources, improve efficiency,
reliability, durability, and cost effectiveness of the products. This comprehensive series will serve researchers all
over the world in keeping them fully abreast of such new developments.
Comprehensive Materials Processing is a one-stop resource consolidating and enhancing the literature of the
materials processing and manufacturing universe. The work addresses recent progress in materials technologies
and science as well as covering recent developments in specific manufacturing processes involved with materials
for applications in engineering, biomedical, environmental protection, health and safety, and sensor materials
and technologies. The authoritative analysis of these processes will assist scientists and engineers in the selec-
tion, design, and usage of materials, whether required in the lab or in action across industry.
As the editor-in-chief of this comprehensive series, a truly collaborative work, I am greatly indebted to the
volume editors, internationally renowned experts in their fields, for guiding and selecting the topics for their
respective volumes, commissioning authors, and reviewing the content so meticulously. Their true dedication to
the scientific community is reflected in the time and energy they have given to this project. My sincere thanks are
also due to all of the authorseresearchers and materials practitioners who have contributed extensive coverage
of literature review as well as recent works of research to this huge project. Their insight and specialist knowledge
in their respective fields is reflected in the high quality of this work.
Myself, the three associate editors-in-chief, and all of the volume editors are greatly appreciative of all the
hard work undertaken to turn this idea into a publishable work. Our special thanks go to Gemma Tomalin, the
project manager, along with Joanne Williams, and the rest of the team at Elsevier who served successively to
keep the project on track through friendly nudges in order to ensure timely completion. We are also hugely
grateful to Mohamed Imrankhan for his dutiful coordination of the proofs.
The extensive academic discussion of core theories and applications, supplemented by applied case studies
and advanced multimedia features has drawn together numerous areas of research and I sincerely hope that this
work will prove to be of great help to both the young and experienced members of the international research
community, academics, and industrial practitioners for many years to come.
Saleem Hashmi
Editor-in-Chief
xxvii
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1.01 Introduction to Assessing Properties of Conventional
and Specialized Materials
CJ Van Tyne, Colorado School of Mines, Golden, CO, USA
! 2014 Elsevier Ltd. All rights reserved.
The basic properties of materials play a dominant role in their processing. It is important not only to obtain quantitative values for
the behavioral properties of a given material during a process, but also to understand how the properties were measured. The goal of
this volume of the work is to provide pertinent information on how some important material properties are measured, as well as to
provide a degree of insight into some developing (i.e., specialized) materials so that manufacturing engineers can begin to meet the
challenges of industrial production by taking advantage of the unique properties for these emerging materials.
The initial chapter on the testing of polymeric materials covers some of the basic techniques that are used for characterizing
polymers, both in research and in industry, for a wide variety of applications. The chapter focuses on how these polymers can be
used in processing and discusses their final application performance. Special attention is given to the rheological and mechanical
testing methods, as well as the determination of the given polymers’ physical and morphological characteristics.
Sheet metal forming limit criteria are routinely used by the metal forming industry to obtain more robust manufacturing
processes and improved product performance characteristics. The chapter on forming limits gives vital information on these
important criteria. In essence, these criteria are a material property that delineates the level of strain or stress that can be imparted to
the sheet before failure (i.e., necking) is expected. Forming limit criteria help optimize performance requirements early in the
product development cycle and can reduce the dependence on physical testing to achieve optimal product performance. These
criteria are essential to computer-aided engineering during product design and manufacturing process development for analysis of
predicted stress and strain histories of the deformation process.
Tension tests are conducted and accepted worldwide as standardized testing procedures to determine properties for sheet
materials. Due to the uniaxial loading condition that is normally present during a tension test, only a limited strain range can be
measured to determine the true stress–true strain curve. In order to extend the validity of the hardening curve, the bulge test has been
developed, since a larger strain range can be achieved under biaxial loading conditions. Although the bulge test has been a recog-
nized testing method for several years, there is no unanimous agreement about the precise testing and evaluation methods.
Standardization is needed to alleviate these difficulties and to obtain greater confidence in the results from bulge tests. The chapter
on bulge testing describes the bulge test and its standardization.
An accurate constitutive equation for the work-hardening behavior is essential so that the processing of sheet metals can be
modeled. The chapter on biaxial testing methods introduces a method to quantify the deformation behavior of sheet metals under
biaxial compression, biaxial tension, combined tension–compression, and in-plane stress reversal. Examples are given both for
material testing methods and for modeling results.
In many processing methods, the material will have residual stresses when the operation is completed. The chapter on residual
stresses discusses major methods for determining these residual stresses. It provides a starting point for residual stress character-
ization, an understanding of what measurements are possible, and sufficient guidance to select an appropriate measurement method.
The more common methods of measuring residual stresses are described, including diffraction, hole drilling, and piezo-spectroscopy.
The limitations of each method, cautions, safety concerns, calibrations, caveats, and other relevant issues are also discussed.
A situation that occurs frequently is the requirement to evaluate a material’s mechanical properties based on a small sample
available for testing. This requirement is particularly relevant when embrittlement and property degradation are suspected, due
to exposure to high temperatures, aggressive environments, or neutron irradiation. As a result, it may be necessary to extract
data from the component itself, so that both metallurgical conditions and actual mechanical properties can be directly
assessed. The chapter on the testing of small specimens provides helpful advice and useful insights into the proper meth-
odologies to be used.
Although steels have been commercially produced for over a century and a half, there have been several very important devel-
opments in new specialized steels. The automotive industry is one of the greatest markets for steels – and one that is undergoing
continuous changes, due mainly to governmental requirements concerning fuel efficiency, safety regulations, and exhaust emissions.
New materials are being proposed to replace steel in automotive applications. Far from being intimidated, the steel community has
used these new challenges to develop new processing methods and ‘new’ steels that may better address the issues. The chapter on
advanced bainitic high-strength steels provides insights on how these types of steels can be formed and the properties that can be
obtained. The chapter on thermomechanical processed steels provides an overview of the thermomechanical-controlled process as
a state-of-the art and cost-efficient manufacturing route to create high-quality steels for a wide range of applications. The chapter on
quenched and partitioned steels introduces a new thermal treatment that is designed to employ carbon partitioning from martensite
into untransformed austenite, with the purpose of generating austenite-containing microstructures in low-alloy steels with attractive
performance characteristics. All three chapters illustrate the creative way in which steel research has been used to produce a material
with a better combination of properties due to the processing that it received.
This volume concludes with a chapter on material properties for numerical calculations. As more processes are being modeled
or simulated on a computer, the issues associated with the materials properties used in these calculations must be understood.
This chapter examines the accuracy of numerical simulations of metal forming processes. The interplay between material
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2 Introduction to Assessing Properties of Conventional and Specialized Materials
characterization and constitutive modeling on the accuracy of the numerical model is also addressed. Examples of the behavior of
light metals are presented, especially for the warm forming of aluminum and magnesium alloys.
The authors of these various chapters have provided the technical community with a useful compendium of material testing
methods and information on the development of new specialized materials. It is essential to understand the properties of materials
and the way in which these properties are measured to ensure the efficient operation of current processing methods and for the
future development of new material processing methods.
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1.02 Techniques for Assessing the Properties of Advanced Ceramic Materials
M Rahman, University College Dublin, Dublin, Ireland
J Haider, Manchester Metropolitan University, Manchester, United Kingdom
T Akter and MSJ Hashmi, Dublin City University, Dublin, Ireland
1.02.1 Introduction 3
1.02.2 Evaluation of Microstructural, Chemical, and Physical Properties 4
1.02.2.1 Morphology 5
1.02.2.2 Crystal Structure 6
1.02.2.3 Chemical Composition 9
1.02.2.4 Size and Shape of Ceramic Powder 9
1.02.2.5 Density, Surface Area, and Porosity 11
1.02.2.6 Ceramic Coating Thickness 12
1.02.3 Evaluation of Mechanical Properties 13
1.02.3.1 Hardness 13
1.02.3.1.1 Microhardness 13
1.02.3.1.2 Nanohardness 14
1.02.3.1.3 Ultrasonic Measurement Technique 14
1.02.3.2 Fracture Toughness 14
1.02.3.2.1 Crack Length Measurement Method 15
1.02.3.2.2 Rockwell C and Vickers Indentations 16
1.02.3.3 Edge Toughness 16
1.02.4 Evaluation of Tribological Properties 17
1.02.5 Evaluation of Thermal Properties 18
1.02.5.1 Thermal Expansion 19
1.02.5.2 Thermal Conductivity 20
1.02.5.3 Heat Capacity 22
1.02.6 Evaluation of Electrical and Magnetic Properties 22
1.02.6.1 Dielectric Property 22
1.02.6.2 Piezoelectric Property 23
1.02.6.3 Superconductivity Property 24
1.02.6.4 Semiconductivity Property 26
1.02.7 Evaluation of Optical Properties 27
1.02.7.1 Transitivity and Absorptivity 27
1.02.7.2 Reflection/Scattering Characteristics 28
1.02.7.3 Luminescence Property 28
1.02.8 Evaluation of Nuclear Properties 28
1.02.9 Evaluation of Biomedical Properties 29
1.02.9.1 Biocompatibility 29
1.02.9.2 Bioactivity 30
1.02.9.3 Biodegradability 31
1.02.9.4 Antibacterial Property 31
1.02.10 Conclusions and Future Outlook 31
References 32
1.02.1 Introduction
The term ‘ceramic’ covers a wide variety of inorganic materials, which are used in almost all the engineering disciplines. Ceramics are
generally crystalline in nature and are nonmetallic compounds formed between nonmetallic and metallic elements such as titanium
and oxygen (titania, TiO2), aluminium and oxygen (alumina, Al2O3), and silicon and nitrogen (silicon nitride, Si3N4). They
generally exhibit excellent physicochemical properties, such as high hardness and strength, low thermal expansion, high thermal
stability, good chemical stability, and they are frequently processed at high temperatures. The ceramic-based industry has currently
become one of the most competitive industries in the world market. The advanced ceramic market had a value of over 40 billion
U.S. dollars in 2009 (1). Although ceramics are very expensive, the major advantages associated with them are low maintenance and
longer life. In the past, the widespread application of ceramics has not been seen, mainly due to their brittleness and high cost.
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4 Techniques for Assessing the Properties of Advanced Ceramic Materials
Figure 1 Classification of advanced ceramics based on their applications.
However, expertise has been growing to change the characteristics of ceramics by modifying the microstructure. This has improved
the mechanical strength of ceramic materials.
There are two major types of ceramics materials widely used in different applications: (1) nontechnical or traditional ceramics
and (2) advanced ceramics (emerging or modern technical or functional ceramics). Traditional ceramics, such as porcelain, brick,
earthenware, pottery, tableware, sanitary ware, tiles, and refractories, are normally made of raw material powders such as ball and
china clay, silica, dolomite, talc, calcite, and feldspar. The type, size, shape, and distribution of these powders influence the
properties of the final ceramic product.
Advanced ceramics are a new, emerging, and growing family of ceramics that have usually been called nontraditional ceramics.
Advanced ceramics such as piezoelectric and semiconductor materials exhibit several enhanced and important functional properties
as compared to traditional ceramics. They can be tailored with functional properties for mechanical, electrical, electronic,
biomedical, optical, and magnetic applications, among others. A classification of advanced ceramics based on their applications and
functions, with property requirements and examples for each class, is presented in Figure 1. Advanced ceramic materials can be
categorized into four groups based on their composition: glass ceramics, such as lithium aluminosilicate; oxides, such as alumina,
zirconia, and mullite; nitrides, such as silicon nitride; and carbides, such as silicon carbide. In general, advanced ceramics comes in
three forms, as shown in Figure 2.
A detailed and consistent characterization of the structural, chemical, physical, mechanical, electrical, thermal, optical, and
biocompatible properties of advanced ceramics is crucial for several reasons. First, investigations into the properties of ceramics
would provide a correlation between manufacturing processes and the performance of the ceramic produced. This enables the
material researchers and engineers to modify the manufacturing process to produce ceramics with more tailored properties. Second,
the engineers and researchers can investigate the applicability of prospective materials for a specific need. Finally, analytical models
of the ceramics could be developed and validated by using material parameters obtained through characterization. Information
gained through the testing of ceramics has led to many new applications.
This chapter gives a brief overview of the characterization techniques that are commonly used for evaluating different properties
of advanced ceramics. The topics of ceramic material characterization are extremely broad. To consider the subject in a short chapter,
only the properties and testing methods for selected ceramic materials will be considered here. The following sections contain an
assessment of microstructural, chemical, physical mechanical, thermal, electrical, optical, nuclear, and biocompatible properties of
advanced ceramic materials. The final section provides concluding remarks and an outline of future directions in ceramic
characterization.
1.02.2 Evaluation of Microstructural, Chemical, and Physical Properties
The morphological and structural properties and composition of ceramics could strongly influence physical properties (such as
density and roughness) as well as other functional properties, which in turn influence the application of these materials in industry.
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Techniques for Assessing the Properties of Advanced Ceramic Materials 5
Figure 2 Different forms of advanced ceramics used in technical applications.
In the following sections, an evaluation of morphological, structural, compositional, and physical properties (such as thickness,
porosity, and density) of ceramic materials is presented.
1.02.2.1 Morphology
The surface morphology and roughness of ceramic materials are examined using an optical microscope, an atomic force microscope
(AFM), a scanning electron microscope (SEM), and an optical profilometer. In addition to qualitative microstructural information, an
optical microscope is useful for quantitative metallographic analysis (e.g., grain size) of the ceramic materials with the help of an
automatic image analyzer connected to the microscope. A simple schematic of an AFM instrument is given in Figure 3 (2). In an AFM
system, a small probe (10–100 nm radius of curvature) is raster scanned by a piezoelectric device over a sample to produce an image
of the sample surface, or near the surface region. The AFM as well as the optical profilometer are used to evaluate the surface
morphology and the roughness of ceramic materials. By using these techniques, 3D/2D surface structure images can be extracted and
Figure 3 A simple schematic view of the AFM system. Reproduced from Rahman, M. Plasma Nitriding and Duplex Coating of Biocompatible
Surfaces for Low Friction and Wear Resistant Applications. PhD Thesis, Dublin City University, 2006.
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different topographical properties of the material can be measured by analyzing the images. Additionally, AFM is used to generate
a contrast image of the material properties of the ceramic surface, such as electrical, magnetic, biological, and mechanical properties.
A featureless smooth surface microstructure of the diamond-like-carbon (DLC) ceramic coating on a silicon substrate from AFM
is shown in Figure 4. The scan was carried out over an area of 3.25 mm " 3.25 mm giving a root-mean-square (RMS) surface
roughness value of approximately 2–3 nm (3). SEM is very helpful in the characterization of structural morphology. Figure 5
presents a cross-sectional SEM microstructures of a porous bioceramic material (4).
1.02.2.2 Crystal Structure

X-ray diffraction (XRD) is a versatile technique that reveals detailed information about the crystallographic information of ceramic
materials. The basic principle of the X-ray diffraction is derived from Bragg’s law. This law states that when the difference in the path
lengths experienced by radiation scattered from two adjacent lattice planes is equal to the wavelength of the radiation or a multiple
of this, constructive interference will occur. This can be represented by the following equation (eqn [1]) (5):
nl ¼ 2d sin q [1]
where n, l, d, and q are the order of reflection, the wavelength, the spacing between planes, and the incident diffraction angle of the
X-ray beam (also called the Bragg angle), respectively.
The XRD machine consisted of an X-ray tube, a sample holder, slits, an optical element, and a detector, as shown in Figure 6.
In this technique, a ceramic sample is placed in the sample holder. When X-rays are emitted toward the sample, the interaction of
the incident X-rays with the sample produces constructive interference (diffracted ray) when conditions satisfy Bragg’s law, as
outlined before. These diffracted X-rays are then detected, processed, and counted. It is important to note that the size of the
3.50 1.75 0. 00
0. 00
1.75
3.50
Figure 4 Surface morphology of the diamond-like-carbon (DLC) ceramic coating observed in AFM. Reproduced from Rahman, M.; Duggan, P.;
Dowling, D. P.; Hashmi, M. S. J. Continuously Deposited Duplex Biomedical Coatings. Surf. Coat. Technol. 2007, 201 (9), 5310–5317.
Figure 5 Cross-sectional scanning electron micrographs of the porous bioceramic in different particle size ranges of the pore former:
(a) 250–350 mm, (b) 400–600 mm. Reproduced from Akter, T. Manufacturing of Biocomposite Shell Mimetic via the Powder
Compaction Method. Master of Engineering Thesis, Dublin City University, 2006.
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Figure 6 Schematic diagram of an X-ray diffraction system.
crystals has a pronounced influence on the width of the diffraction peak, and the intensity is linearly proportional to the number
of unit cells that have the same orientation. Therefore, not only can X-ray diffraction be used to determine the structure factor of
a material or the lattice spacing, but it may also provide valuable information concerning the size and crystallographic orien-
tation of crystallites.
Lattice spacing of a cubic structure (d0) can be determined using Bragg’s law, where (hkl) is the reflection plane (5).
nl ¼ 2dhkl sin qhkl [2]
d0
dhkl ¼ pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi [3]
h2 þ k2 þ l2
Therefore, by using eqns [2] and [3], it is possible to determine d0 from each reflection.
The size of a grain and imperfections within a grain have an effect on its X-ray diffraction pattern (5,6). By comparing the
modified X-ray diffraction pattern with the perfect crystal pattern, it is possible to determine the grain refinement and stress effect in
the crystals after material processing. Generally, decreasing the crystal size will result in diffraction peak broadening. This broad-
ening depends on the distance between the planes and is thus different for different {hkl} reflections. This can be is described by the
following equation (eqn [4]):
Kl
b¼ [4]
L cos q
where b is the width of the diffraction peak in radians, L is the size of the grain, and K is a factor that depends on the shape assumed
for the intensity distribution of diffraction. The value of K is close to unity. It is important to note that the broadening of the
diffraction line is due not only to the size and microstress effects but also to nonmonochromatic radiation, slit sizes, and an
imperfect focus.
Figure 7(a) shows the XRD pattern of calcium carbonate powder before compaction, which indicated that the powder contained
the calcite polymorph CaCO3. The diffraction pattern of porous bioceramics is shown in Figure 7(b). No structural change was
observed in the new porous ceramic, which confirms that complete burn out of the pore former (naphthalene powder) occurred
without forming any complex new compounds during postprocessing (4).
Raman spectroscopy is primarily a structural characterization tool that is used to find out chemical bonding and crystalline
information of ceramic materials if it is Raman-active. For example, Rahman et al. (7) confirmed the formation of anatase phase
after thermal treatment of the sputter-deposited TiO2 coating by Raman spectroscopy. In Raman spectroscopy, a sample is irradiated
with a strong monochromatic light source. A small amount will scatter from that sample at a wavelength shifted from the original
laser wavelength. This shift of wavelength is due to the light scattered by the electron clouds that make up the chemical bonds in the
sample. The scattering, in which the scattered photons have either higher or lower photon energy than the incident photon, is called
Raman scattering. In a typical Raman spectroscopy system, as shown in Figure 8, measurements can be performed in backscattering
geometry using laser excitation of a sample with a liquid-nitrogen-cooled detector for collecting a signal from the sample. With
a microscope objective, the laser can be focused on the sample surface for selective area monitoring of chemical bonding or crystal
structure of the ceramic materials.
The C–C bonding structure of the DLC ceramic coating is identified by Raman spectroscopy, as shown in Figure 9. A broad peak
around 1550, composed of a G (corresponding to the graphite phase) and a D (corresponding to the disorder phase) band, was
confirmed after Gaussian peak fitting.
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Figure 7 X-ray diffraction patterns of (a) as-received calcium carbonate (CaCO3) powder, (b) and porous CaCO3 bioceramic after compaction and
drying. Reproduced from Akter, T. Manufacturing of Biocomposite Shell Mimetic via the Powder Compaction Method. Master of Engineering
Thesis, Dublin City University, 2006.
Figure 8 Schematic diagram of Raman spectroscopy system.
Figure 9 The Raman curve-fitting spectra of the DLC coating on silicon. Reproduced from Rahman, M.; Duggan, P.; Dowling, D. P.; Hashmi, M. S. J.
Continuously Deposited Duplex Biomedical Coatings. Surf. Coat. Technol. 2007, 201 (9), 5310–5317.
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1.02.2.3 Chemical Composition

The chemical composition of ceramic materials can be determined by X-ray photoelectron spectroscopy (XPS), energy dispersive
X-ray spectroscopy (EDX), secondary ion mass spectroscopy (SIMS), and chemical analysis. Among the techniques, XPS is widely
used to measure the stoichiometry and chemical bonding status of the ceramic coatings as well as bulk material. In the XPS
technique, electrons (photoelectrons) are emitted from the core level of an atom by the absorption of photon energy, as illustrated
in Figure 10. Photoelectron emission occurs when a photon transfers its energy to an electron, and a photoelectron can be emitted
only when the photon energy is larger than the binding energy of the electron. In this technique, in general, X-rays of known and
fixed photon energy (hn), usually Mg Ka (1253.6 eV) or Al Ka (1486.6 eV), are used to excite and eject the core-level electron. The
emitted electrons (photon) have kinetic energies, given by the following equation (eqn [5]):
Eb ¼ hn ½ðknown quantitiesÞ ' Ek ðmeasured by the analyzer of XPS instrumentÞ( [5]
where hn is the energy of the absorbed photon (X-ray), Eb is the binding energy of the atomic orbital from which the electron
originates, and Ek is the kinetic energy of the ejected photoelectron. The kinetic energy of the ejected photoelectron (Ek) is analyzed
by retarding or accelerating the detected electron in the spectrometer. It is forced by an electron lens system and then dispersed in
terms of kinetic energy by a hemispherical electrostatic analyzer.
The photoelectrons are subsequently detected via a multichannel system consisting of multichannel plates, a phosphor screen,
and a charge-coupled device (CCD) camera. Therefore, the binding energy of the core-level electron, Eb, is measured by the
difference between the known energy of the X-ray photon (hn) and the kinetic energy (Ek) of the electrons (measured by the analyzer
of XPS instrument). Binding energy (Eb) measurement provides an atomic identification and chemical state information as Eb is
constant and a fixed value (fingerprint) of a particular atom. The XPS technique provides a way of identifying the elements and gives
information about their chemical states present in the outermost (w5 nm) surface due to the relatively short inelastic mean free
path of the photoelectrons. The transportation of emitted electrons to the surface generated in the solid can thus only occur from
a certain depth.
The main advantage of using the XPS technique lies in the fact that the binding energy of a photoelectron is sensitive to the
chemical surrounding of the atom, which means that there is a chemical shift in the binding energy. These shifts are very important,
since they provide a tool to identify the individual chemical states, or bonding states, of an element. As shown in Figure 11, XPS is
used to confirm the formation of titanium oxide ceramic thin film deposited by the magnetron sputtering technique. Both EDX and
SIMS are employed to evaluate the chemical composition of ceramic materials, whereas SIMS is a more surface-sensitive
measurement technique. Figure 12 presents EDX spectra of TiAlN ceramic coating, where the atomic percentages of Ti and Al are
56.53% and 43.47%, respectively.
1.02.2.4 Size and Shape of Ceramic Powder

Particle size, shape, and distribution of the ceramic powder have significant influences on the physical, mechanical, and functional
properties of ceramic materials. A particle-size analyzer is used to evaluate the size and distribution of ceramic nano- or microsize
particles. There are a number of ways of measuring the particle size and distribution, including a mechanical sieve, centrifugal
classification, and laser diffraction. However, the advantages of using the laser diffraction method, as compared to the other
methods, are that this process is quick and very reproducible. This method also produces more detailed results than those produced
by the mechanical sieve method. A laser diffraction technique mainly consists of a laser source, a quartz glass container, a stirrer, an
ultrasonic probe, and lenses.
In a laser diffraction technique, a laser light is directed into a suspension of particles that are suspended in solvent, as shown in
Figure 13 (8). The laser is scattered by the particles, and smaller particles scatter the laser at larger angles than the larger particles. The
(a) (b)
Valence band Valence band
M 3s
L 2, 3 2p
(Ek= hv– Eb )
L1 2s
e-
K 1s
Ground State Ejection of Photoelectron
Figure 10 A schematic diagram of electron energy transition in XPS: (a) ground state and (b) incident photon (X-ray) ejects K shell electron
(photoelectron). Reproduced from Rahman, M. Plasma Nitriding and Duplex Coating of Biocompatible Surfaces for Low Friction and Wear
Resistant Applications. PhD Thesis, Dublin City University, 2006.
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Figure 11 An XPS narrow scan spectra of the Ti2p peak for the TiO2 ceramic coating deposited by sputtering techniques. Reproduced from
Rahman, M.; MacElroy, J. M. D; Dowling, D. P. Influence of the Physical, Structural and Chemical Properties on the Photoresponse Property of
Magnetron Sputtered TiO2 for the Application of Water Splitting. J. Nanosci. Nanotechnol. 2011, 11 (10), 8642–8651.
Figure 12 EDX spectra of a ceramic TiAlN coating.
Figure 13 Schematic view of a laser diffraction particle size analyzer. Adapted from Anon. Principle of Laser Diffraction,
www.cgerhardt.co.uk/pages.php?page_id¼142 (downloaded on 18 July 2013).
scattered light can be measured by a series of photodetectors placed at different angles. The particle size analysis of the calcium
carbonate ceramic powder is characterized by using the laser diffraction method as show in Figure 14.
Particle size and shape can also be examined using the SEM. For SEM observation, the powder samples are mounted on a slab
covered with silver glue. In the case of nonconductive ceramics, the samples need to be coated with gold/carbon before observation
to reveal the features of the individual particles contained within the samples (4).
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Figure 14 Particle size and distribution of CaCO3 ceramic powder evaluated by a laser diffraction-based particle size analyzer. Adapted from
Akter, T. Manufacturing of Biocomposite Shell Mimetic via the Powder Compaction Method. Master of Engineering Thesis, Dublin City
University, 2006.
1.02.2.5 Density, Surface Area, and Porosity

Density, surface area, and porosity are very important properties of ceramic materials. They determine the suitability of a ceramic
material in a particular application. These properties also have strong relationships with each other. For example, generally a higher
surface area of a material indirectly indicates lower density and higher porosity. Therefore, evaluating one of these properties will
allow us to estimate the other two.
The total porosity of ceramic material can be evaluated from sample geometric density (as shown in Figure 15), rgeometry, which
is defined by the following equation (eqn [6]) (9):
4m
rgeometry ¼ [6]
pD " 2H
where h, D, and m are the sample height, diameter, and mass, respectively. As the diameter of every sample is constant, the height of
the samples is measured using the Vernier scale to an accuracy ) 0.01 mm. Then the total porosity (P) of the ceramic is calculated
using eqn [7] (9):
rgeometry
P ¼1' [7]
rpowder
where rgeometry and rpowder are the density of the ceramic block and the ceramic powder, respectively.
The BET (Brunauer, Emmett, and Teller) method is widely used to investigate the surface area, porosity, pore distribution, and
pore volume of ceramic materials. The BET technique is based on the physical adsorption of gas molecules to solid surfaces, which
can be related to their surface area. By knowing the surface area, density of material, and amount of gas absorbed, the porosity, pore
distribution, and pore volume of the material can be estimated (10). In this technique, gas at isothermal temperature is allowed to
pass through a sample and to adsorb to the surface. The gases used for absorption are mainly liquid nitrogen or helium. Before
Figure 15 A ceramic block made from compaction of ceramic powder.
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Figure 16 Effect of doping (N, C, or N þ C) on the refractive index, which indirectly indicates the density or porosity properties of the
magnetronsputtered TiO2 ceramic coating. Reproduced from Rahman, M.; Dang, B. H. Q.; McDonnell, K. A.; MacElroy, J. M. D.; Dowling,
D. P. Effect of Doping (C or N) and Co-doping (CþN) on the Photoactive Properties of Magnetron Sputtered Titania Coatings for the Application
of Solar Water-splitting. J. Nanosci. Nanotechnol. 2012, 12 (6), 4729–4735.
conducting a BET measurement, the sample must be preheated to remove any contaminants present on the surface that would affect
the results obtained.
The density/porosity of the thin-film ceramic materials can be indirectly evaluated from their refractive index property.
Spectroscopic ellipsometry is a widely used technique for measuring the refractive index of a thin ceramic film, as discussed in
Section 1.02.7.2. Generally, a material with a higher refractive index indicates higher density and vice versa. The refractive
index, and thus the density of a film, is strongly influenced by the deposition condition of thin-film processes, as shown in
Figure 16.
1.02.2.6 Ceramic Coating Thickness

The thickness of a thin-film ceramic such as TiO2, ZnO, SiO2, etc. on a substrate can be measured with a large variety of different
methods, such as the ball catering method, ellipsometry, step height (using AFM, optical profilometry, and mechanical stylus),
a cross-sectional image, and X-ray reflective spectroscopy (XRR). The thickness of a ceramic coating is widely measured using
a spectroscopic ellipsometric system. Different models (such as Cauchy and B-Spline models) are applied to fit the measured
ellipsometric data to obtain the coating thicknesses and refractive index.
Figure 17 shows the SEM cross-sectional morphology of the duplex coating substrate system (DLC coating on a plasma nitrided
substrate) used to evaluate the thickness of the DLC ceramic coating deposited using plasma-enhanced chemical vapor deposition
Figure 17 SEM cross-sectional thickness of a DLC coating layer. Reproduced from Rahman, M.; Duggan, P.; Dowling, D. P.; Hashmi, M. S. J.
Continuously Deposited Duplex Biomedical Coatings. Surf. Coat. Technol. 2007, 201 (9), 5310–5317.
www.iran- mavad.com
(PECVD) techniques (3). A uniform and dense layer of the DLC coating on the homogeneous thick plasma nitrided layer was found
in the duplex treated samples. The thickness of the coating was between approximately 0.9 and 1. 00 mm.
1.02.3 Evaluation of Mechanical Properties
Currently ceramics research is focused on producing hard and tougher ceramics with reliable performance in structural
applications such as cutting and forming tool industries, casting, and steel processing industries. These ceramics have the
capability to replace metals or plastics due to their extreme hardness and resistance to wear. Therefore, it is essential to
characterize the mechanical properties of the structural ceramics. Correct prediction of mechanical properties (such as hardness,
elastic modulus, and fracture toughness) is also very important to predict the performance of the component using finite
element analysis. The major ceramics used for mechanical and tribological applications are alumina (Al2O3), zirconia (Zr2O3),
silicon carbide (SiC), and silicon nitride (SiN). Alumina is the most common ceramic for mechanical applications (11,12).
Other hard ceramic materials include diamond, cBN, and B4C. The structural ceramics are mainly attractive due to their high
strength, light weight, high thermal and chemical stability, and high wear resistance. The principal mechanical properties of the
ceramics that are tested are hardness, strength, and fracture toughness. In the following sections, an evaluation of these
properties is discussed.
1.02.3.1 Hardness
Among the mechanical properties, hardness is very commonly measured for ceramic materials. Hardness is defined as the measure
of the resistance of a material to deformation or fracture. The hardness of ceramic materials is generally measured using conven-
tional tests such as Vickers hardness, Knoop hardness, Berkovich hardness, and Rockwell hardness.
1.02.3.1.1 Microhardness
The most conventional hardness tests involve a hard indenter (diamond, for example) that is pressed vertically into the surface of
the sample being tested. Vickers and Knoop are the two common techniques for measuring the microhardness of ceramic materials.
They measure the hardness of a material from the size of an impression produced under load by a pyramid-shaped diamond
indenter. The method most commonly used in test laboratories is the Vickers hardness test. The indenter used in this technique is
a square-base diamond pyramid with face angles of 136* . This low amount of load creates a small indent that must be measured
under a microscope. The schematic diagram of the created indent is shown in Figure 18.
The theory behind the Vickers hardness measurement is that hardness is equal to the load divided by the contact area. The
standard formulas generally used for measuring hardness are given in eqns [8] and [9] (13,14),
" #
P
Hv ¼ 1:8544 2 [8]
d
" #
P
Hk ¼ 14:229 [9]
L2
where Hv is the Vickers hardness number, P is the applied load in kg, d is the average measured diagonal lengths of the diamond
impression in mm, and L is the large diagonal length in mm. The duration of load application varies from 10 to 20 s. In general, an
average hardness value is calculated from 10 measurements, where the indentations are very clear, readable, and have no cracked or
deformed indentations. Vickers hardness results may vary from machine to machine and laboratory to laboratory (15). It is clear
Load, P
Indenter
Measurement position
Loading Position
d1 d2
Figure 18 A schematic diagram of a Vickers indenter and plan view of the indentation area.
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from the equations that hardness is inversely proportional to the square of the diagonal length of the indentation. Therefore, any
error in length measurement will result in a high variation in the hardness value.
Compared to the Vickers indenter having fourfold symmetry, the Knoop indenter has only twofold symmetry. Projected area is
considered in the Knoop measurement, whereas true contact area is considered in the Vickers method (14). Due to the geometry of
the Vickers indenter, it makes a deeper indentation than the Knoop indenter and can cause fractures in the ceramic materials
(16,17). The main shortcoming in the Vickers method is the difficulty in hardness measurement if there is cracking or fragmentation
at the indentation corners. In some cases, cracking is not visible on the surface. Therefore, the hardness measurement can give
misleading results between two measurements with and without crack. Direct comparisons between the Knoop and Vickers
measurements are also difficult due to the difference in indenter geometry, penetration depth, and sensitivities for cracking (17).
A comparison between the hardness tests of Knoop and Vickers on different ceramics showed that generally the Knoop hardness
number was lower than the Vickers hardness number for the highest values of hardness (14). The small penetration depth in the
Knoop hardness method allows us to measure the hardness of thin coatings.
Grain size is an important property of ceramic materials, which can affect the hardness. Experimental results showed that the
hardness of c-ZrO2 increased with Al2O3 doping due to the grain refinement (18). Both Knoop and Vickers hardness depend on the
size of the indentation, which is dependent on the applied load. This phenomenon is called the indentation size effect (ISE), which
causes a decrease in hardness with the increase of indentation load (17). This means that the hardness number should be quoted in
association with the tested load, and the change in hardness with the loads must be provided when hardness is used as a material
selection criterion (19). The plot of hardness versus indentation load for ceramic materials suggests that there exists a discrete
transition point where the hardness changes from load-dependent to constant, as demonstrated in Figure 19 (17,20). This transition
occurs when cracking around the indentation takes place. In order to avoid the fracture problem at the indentation, experiments are
carried out at low loads, where the change in hardness is noticeable. Low loads can only deform the material without any fracture.
However, at low load, measurement is difficult due to the small indentation size. On the other hand, high indentation load can
cause severe cracking, which can give rise to large scatter in the results. Therefore, an optimum load must be selected so that
a sufficiently large indentation can be created with little or no cracking.
1.02.3.1.2 Nanohardness
Nanoindentation is an emerging technique for characterizing the mechanical properties of ceramic materials in the nanoscale. In
general, an instrumented machine is used to apply a very small load with a Berkovich indenter. This technique simultaneously records
displacement and load during loading and unloading of the indenter rather than measuring diagonal length to measure the hardness.
Hardness and Young’s modulus are evaluated through the analysis of the data. The nanoindenter is perfectly suitable for hardness
measurement in thin ceramic coatings as the penetration depth could be as low as 20 nm. Figure 20 shows a loading and unloading
curve for a ceramic coating. Nanoindentors are even capable of measuring the hardness of individual ceramics particles (21).
1.02.3.1.3 Ultrasonic Measurement Technique

The hardness of ceramic composite material can be qualitatively measured by the ultrasonic velocity measurement technique (22).
A strong relationship between ultrasonic velocity and ceramic composite hardness has been observed. It has been shown that the
increase of hardness of the ZrO2–Al2O3 composite is indicated by the increase in ultrasonic velocity. This could be attributed to the
toughening and strengthening effects from the phase transformation of the ZrO2.
1.02.3.2 Fracture Toughness

Fracture toughness (KIC) is a macroscopic property of material and it describes the ease with which a crack or defect propagates in
the material. It is well recognized that due to their brittle characteristics, the fracture toughness of ceramics is very poor. Fracture
Vickers Hardness HV
Indentation Load
Figure 19 Vickers hardness dependency on indentation load (indentation size effect). Adapted from Quinn, G. D. Hardness Testing
of Ceramics. Adv. Mater. Process. 1998, 154 (2).
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6000
Substrate: Tungsten carbide
Coating: Nanocrystalline TiAlSiN
5000 Hardness: 35.84 GPa
Young's Modulus: 348.87 GPa
4000
Load (µN)
Loading
3000
2000 Unloading
1000
0
0 20 40 60 80
Indentation depth (nm)
Figure 20 Nanoindentation of TiAlSiN coating.
toughness values are measured to characterize the resistance to fracture of ceramic materials. Currently a number of methods are
available to measure fracture toughness of ceramic materials. Generally the crack length measurement method is used for quan-
tifying the fracture toughness of the bulk ceramics. On the other hand, the Rockwell C indentation technique is widely used for
toughness evaluation of the ceramic coatings.
1.02.3.2.1 Crack Length Measurement Method

However, fracture toughness measurement based on crack length has become quite a popular method due to its ease of use, its
nondestructive nature, the small volume of material required to conduct KIC measurements, and the easy sample preparation. This
method is derived from the conventional Vickers hardness measurement procedure with measurement of the crack length growing
in the corners of the indentation, as shown in Figure 21 (23,24). Figure 22 presents the photograph of a Vickers hardness machine
for measuring hardness and fracture toughness.
A flat ceramic sample is indented by a Vickers indenter with a certain load to develop radial cracks from the corner of the
indentation. The fracture toughness of the material is inversely proportional to the crack length. The fracture toughness measured
with this method is dependent on the hardness and Young’s modulus of the material, the crack length, and the applied load.
A simplified two-dimensional fracture mechanics approach has been employed in this method to obtain the KIC using the following
equation (eqn [10]) (23):
" #1=2 " #
E P
KIC ¼ 0:016H [10]
H c3=2
where P is the applied load in Newton, c is the crack length from the center of the indent to the crack tip in meter, E is Young’s
modulus in GPa, and H is the Vickers hardness in GPa.
Grain size can play a significant part on the fracture toughness of a ceramic material. It was shown that fracture toughness of
Al2O3-doped c-ZrO2 specimens increased with increasing Al2O3 content due to the decrease in grain size (18). However, the
accuracy of this method could be unreliable due to the development of subcritical crack and error in measuring the exact length of
the cracks (16). In some cases, very high loads (up to 500 N) need to be applied to generate sufficiently long cracks.
c
a
Indentation
Crack
Figure 21 Vickers indentation with radial cracks from the corner.
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Figure 22 Zwick hardness and fracture toughness machine (Type 5030 SKV, Indentec Ltd., UK).
1.02.3.2.2 Rockwell C and Vickers Indentations

The Rockwell C indentation technique can also be used for an evaluation of ceramic coatings in a qualitative way. In this method,
a 120* spheroconical diamond indenter is pressed against a coated sample with a certain standard load (60, 100, and 150 kg), as
shown in Figure 23. When the indenter penetrates the coating, cracks propagate from the indentation point toward the edge of the
sample. By investigating the crack around the indentation, the toughness of the ceramic coating can be compared. Figure 24
presents a magnified view of an indentation made on a DLC coating on a steel substrate.
For thin ceramic coating, coating toughness can also be evaluated through the observation of a Vickers indentation using an
optical microscope (25). Figure 25 shows an optical image of Vickers indentation performed at higher load (500 g) on a TiN-based
multicomponent ceramic coating.
1.02.3.3 Edge Toughness

The fracture resistance of ceramic materials can be related to edge chipping resistance. This test involves forming a chip by applying
an increasing force near the edge of a specimen (26). In general, the test specimens are prepared as rectangular blocks with 90* edges.
Load
Indenter
Cracks
Coating
Substrate
Figure 23 Rockwell C setup for the toughness measurement of ceramic coating.
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Crack Network
Swelling
deformation
500µm Delamination
Figure 24 Rockwell C indentation of ceramic DLC coatings on a steel substrate (load 100 kg). Reproduced from Rahman, M.; Duggan, P.;
Circular cracks
Figure 25 Optical micrograph of Vickers indentation for TiN-based multicomponent ceramic coating (TiN þ MoSx). Reproduced from
Rahman, M.; Haider, J.; Dowling, D. P.; Duggan, P.; Hashmi, M. S. J. Investigation of Mechanical Properties of TiN þ MoSx Coating on
Plasma-nitrided Substrate. Surf. Coat. Technol. 2005, 200 (5–6), 1451–1457.
With this test, the designers can experiment with various edge geometries to find out the optimum one. This test can be performed in
a dedicated edge-chipping machine or in a universal testing machine with different types of indenters (Rockwell, Vickers). This
technique is routinely used in R&D labs, quality-control labs, and failure-analysis investigations. The force required to make a chip
is proportional to the indenting distance from the edge. Therefore, force versus distance generally follows a linear trend. However, in
some cases, the trend could be best fitted with a power law depending on the material and the type of indenter. A parameter called
edge toughness is calculated from the slope of the line resulting from a linear fit and is used to quantitatively assess the edge-
chipping resistance of structural ceramics. In general, fracture toughness increases with the chipping resistance.
1.02.4 Evaluation of Tribological Properties
Evaluation of tribological properties of ceramic materials (wear and friction coefficient) is also very important in order to determine
their suitability for wear-resistant applications such as ball bearings, pump seals, and prosthetic devices. The most common way of
measuring the tribological properties is the pin-on-disk method. Generally a pin is pressed against a sample rotating disk under
a certain load, as shown in Figure 26.
The specific wear rate can be calculated by measuring the wear volume from the wear track profile using the following equations
(eqns [11] and [12]). Worn surfaces are investigated with an optical microscope, SEM, or an optical profilometer. Figure 27 shows
the wear track profiles of ceramic coatings (27).
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Load Pin
Pin r θ
l
Disk sample
Aw d
Sample
Figure 26 Arrangement of pin-on-disk for wear testing and wear profile.
(a) (b)
Wear track
DLC Coating
Wear track
TiN Coating
Figure 27 Optical micrographs of TiN (broken) and DLC ceramic coatings (intact). Reproduced from Rahman, M.; Duggan, P.; Dowling, D. P.;
Hashmi, M. S. J. Continuously Deposited Duplex Biomedical Coatings. Surf. Coat. Technol. 2007, 201 (9), 5310–5317; Haider, J.; Rahman, M.;
Corcoran B.; Hashmi, M. S. J. Deposition and Characterization of Hard-solid Lubricant Coating by Closed-field Magnetron. Surf. Coat. Technol. 2005,
200, 1080–1083.
Wear rate VW ¼ Wear volume Normal load " sliding distance [11]
VW ¼ r2sin ' 12rd ' d2r ' 2rd ' d2ðr ' dÞL " N " 10 ' 09ðm3N ' mÞ [12]
where, r ¼ radius of the pin (mm), d ¼ depth of the wear track (mm), L ¼ normal load (N) and N ¼ number of revolutions.
The sliding motion between pin and disk provides a frictional force, which is proportional to the applied load. The friction
coefficient, m, is calculated using the following equation (eqn [13]):
F
m¼ f [13]
Fn
where Ff is the measured frictional force and Fn is the applied normal force.
The friction coefficient plots for DLC coatings deposited on nitrided (duplex) and non-nitrided (nonduplex) substrates are
presented in Figure 28. A combination of the number of factors determines the wear of ceramic material operating conditions:
contact geometry, surface roughness, microstructural features, grain sizes, fracture toughness, speed, load, temperature, duration,
environment, and lubrication (28). An increase in sliding velocity can significantly increase the specific wear rate (29). Micro-
structural properties of ceramic materials such as grain size and grain boundary composition have a significant effect on the wear
resistance. On the other hand, the surface roughness of ceramic materials can play a big part in the friction coefficient (24). A
number of models exist for predicting wear in ceramics by using only the material property and operating parameters (28).
1.02.5 Evaluation of Thermal Properties
Ceramics are used especially for their high-temperature strength and resistance to hot erosion, resistance to corrosion or oxidation,
and the fact that they have relatively stable characteristics at temperatures above 500 * C. In different sectors of industries, including
high-temperature machining, material production, chemical engineering, nuclear reactors, aerospace, and power generation, high-
temperature stable materials are required. At high temperatures, ceramic materials have shown their potential uses in many different
engineering applications. Some typical examples include Si3N4-based materials for applications in ball bearings, cutting inserts, and
automobile valves; refractory ceramics such as porcelain, Al2O3, and MgO for a protective layer in structures that are in contact with
melted metal/slag; zirconia-based materials for fuel cells, rocket nozzles, and hypersonic space vehicles; and SiC-based materials for
bearing seals. Recently, ceramic materials have been intensively investigated for substrate application used for thin-film depositions,
because of their high thermal conductivity in combination with high electrical resistivity.
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Figure 28 The friction coefficients of (a) a duplex coating: DLC on top of plasma nitrided stainless steel substrate, and (b) a nonduplex
coating: only DLC layer on stainless steel substrate evaluated by a pin-on-disk wear tester. Reproduced from Rahman, M.; Duggan, P.;
However, before ceramics can be used extensively for such high-temperature applications, it is important to know not only the
physical parameters, but also the thermal properties of each constituent at the microscopic scale. The term ‘thermal analysis’ actually
includes different techniques that determine a change in a material as a function of temperature. Therefore, it is necessary to develop
and select the proper testing method for measurement of the high-temperature properties such as thermal conductivity, thermal
diffusivity, thermal expansion, and specific-heat capacity in order to provide the appropriate materials for industrial requirements
and applications.
1.02.5.1 Thermal Expansion

The coefficient of thermal expansion (CTE) is an important property in choosing ceramic materials for many different applications.
For example, glaze coating is widely used for decorating ceramic objects. If the CTE of the glaze layer is higher than that of the base
ceramic, it will cause tension in the ceramic body upon cooling, resulting in a network of cracks and a weaker finished product.
However, the tendency for thermal shock increases when materials have a high CTE.
Dilatometers are often used to determine the coefficient of thermal expansion. They are designed to determine linear dimen-
sional changes through a wide temperature range in air, vacuum, or inert gas systems. To examine a wide range of materials, they
provide all the deformation modes necessary for thermal expansion and contraction, as well as key transition temperatures. The
probe profiles, commonly used in dilatometer testing, are flat, hemispherical, pointed, and beam bending. Pushrod is one of the
dilatometer methods (as shown in Figure 29) (30) used to determine the dimensional changes, versus temperature or time, while
the sample undergoes a controlled temperature program.
The degree of expansion (Dl) divided by the change in temperature (DT) is generally called the material’s coefficient of expansion
(a), and it varies with temperature, as represented by the following equation (eqn [14]):
" #
1 Dl
a¼ [14]
L0 DT
Figure 29 Schematic view of a horizontal pushrod dilatometer system for measuring the thermal expansion coefficient of ceramic materials.
Adapted from Aubuchon, S. R. Dilatometer Technology, 2012, http://www.ceramicindustry.com/articles/print/92598-dilatometer-technology
(downloaded on 18 July 2013).
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7.00E-06
6.00E-06
Thermal Expansion
Co-efficient, (C–1)
5.00E-06
4.00E-06
3.00E-06
2.00E-06
1.00E-06
0.00E+00
0 200 400 600 800 1000 1200
Temperature, °C
Figure 30 The thermal expansion characteristic of the BW–6C boron carbide based ceramic materials from room temperature to 1100 * C.
where L0 is the initial sample length. Due to the contact forces associated with the pushrod, the measurement of a thin film in this
type of dilatometer can be problematic. The optical dilatometer introduces an innovative new measurement principle to improve
many tests and make unconventional dilatometry experiments possible.
The accuracy of the dilatometric measurements greatly depends on proper instrument selection. There are significant vari-
ations between the configurations, each being better suited for a particular measurement and application. The horizontal design
dilatometer is considered to be simple and flexible to use and shows the best temperature uniformity. However, the vertical
design is suitable to use for a sample that may shrink on heating, as it ensures the sample’s contact with the pushrod. The
noncontact optical dilatometer is an ideal choice for characterizing thin films and other materials with some restrictions on
sample preparation. This measurement technique is absolute and without contact, and no system calibration curves are
required.
Thermal expansion was measured and discussed for boron carbide based ceramics of 50–900 * C using a pushrod dilatometer.
The material was heated at a rate of 5 * C min'1 from 20 to 1100 * C in a flowing helium atmosphere. Figure 30 shows the thermal
expansivity of such a boron carbide based ceramic (BW–6C) as a function of temperature (31).
Thermal expansion analysis is applied to the study of phase segregation of Zr2Al4C5 ceramics at elevated temperatures
(20–2000 * C) under flowing argon using an ultrahigh-temperature dilatometer. The linear thermal expansion coefficient was
determined to be (7.6 ) 0.5) " 10'6 K'1 for the Zr2Al4C5 at 20–1800 * C (32). However, the thermal expansion of the Zr2Al4C5
samples increased sharply between 1800 and 1900 * C. The Zr2Al4C5 ceramic material showed obvious signs of decomposition at
approximately 1900 * C. Such information would be useful for the detection of phase decomposition temperature and the thermal
stability of materials.
The linear thermal expansion coefficient of BaTiO3-based ferroelectric ceramic material was discussed in the literature using
a Perkin–Elmer TMA7 thermal mechanical analyzer operated in expansion mode from '50 to 250 * C. The measurements showed
that such materials are isotropic and have a linear CTE of about 6 " 10'6 K'1 near room temperature. Above the ferroelectric
transition temperature, the CTE of the material increases to above 10 " 10'6 K'1. These values are significantly smaller than the
typical CTE of an organic substrate material that is typically used in the microelectronics industry. This CTE mismatch is a major
reliability concern for embedded chip capacitors (33).
1.02.5.2 Thermal Conductivity

In recent years, materials in the form of bulk ceramic or coating with a high thermal conductivity have been developed by many
researchers. The thermal conductivity of these materials is more difficult to understand than that of a single crystal, as they contain
grains and grain boundaries.
The accurate measurement of thermal conductivity requires the calculation of thermal diffusivity (a), heat capacity (Cp), and true
density (r) using the following equation (eqn [15]):
l ¼ raCp [15]
The transient plane source technique (TPS), which is sometimes referred to as the ‘hot disk’ method or the Gustafsson probe,
most commonly measures the thermal diffusivity of ceramic materials. This method has been developed with the goal of meeting
the requirements of thermophysical properties of new and specially designed materials. This technique uses plane heat source
sensors and an electrically conducting pattern in the shape of a double spiral, which is sandwiched between two thin, electrically
insulating sheets (Figure 31) (34).
One main advantage of this technique is the elimination of the thermal contact effect, which is represented by the intercalation
layer between the sensor conducting pattern and the ‘bulk surface’ of the sample. This allows for a direct measurement of the bulk
thermal conductivity and bulk thermal diffusivity of the sample. This technique offers several advantages, including the possibility
of performing measurements on samples that have a high thermal conductivity. Another advantage is a significant increase in
measuring sensitivity with a reproducibility of 0.1% obtained for homogeneous samples.
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Figure 31 The transient plane source (TPS) technique with a ‘hot disk’ sensor for thermal conductivity measurements. Adapted from Anon.
Sensors for Thermal Conductivity Measurements, http://www.hotdiskinstruments.com/products/sensors-for-thermal-conductivity-measurements.html
(downloaded on 18 July 2013).
The hot disk sensor is usually made of a double spiral of nickel wire, and is sandwiched between two halves of a sample during
the measurement. A small electric current is supplied to the sensor, which serves both as a heat source and a temperature monitor.
Results from this testing indicate that the temperature change of the sensor surface, DT, which can be determined through the
resistance measurement and is highly dependent on the thermal transport properties of the surrounding material (35–37), is
defined by eqn [16],
Po
DT ¼ DðsÞ [16]
p3=2 aK
where Po is the output power to the sensor, a is the sensor radius, and K is the thermal conductivity of the surrounding material.
A dimensionless parameter s ¼ O(kt)/a is called the characteristic time ratio, where k is the thermal diffusivity of the sample and t is
the measurement time. D(s) is a rather complicated function, but if the relationship between t and s is known, it is possible to plot
DT as a function of D(s), and a straight line should be obtained. Thermal conductivity can be calculated from the slope of this line.
The proper value of s is generally unknown, but can be determined through a series of optimization processes. In general, hot disk
measurement uses relatively thick samples (i.e., sample thickness: >O(4kt) (38)).
If only thin slab samples of a material are available, then it is still possible to perform the hot disk measurement by insulating the
two outer surfaces of the two halves of the sample. Under such a configuration, the function D(s) in eqn [16] needs to be modified
to include the contribution from all image sources.
Barium titanate (BaTiO3) based ceramics have been used widely as dielectric layers in manufacturing multilayer ceramic
capacitors. From the experimental values, the thermal diffusivity and thermal conductivity of BaTiO3 were determined at room
temperature by using a hot disk sensor technique (33).
The laser flash method is one of the most common techniques for measuring the thermal diffusivity of a ceramic material. The
measurement is made by pulsing a known amount of energy from a laser onto the sample and then measuring the rise in
temperature. Figure 32 shows a sketch of a basic laser flash method. In the laser flash system (Thermaflash 2000), the sample disk is
aligned between a neodymium glass laser and an indium antimonide (InSb) IR detector in a tantalum tube furnace. A thermocouple
is set in contact with the sample and its surroundings at any temperature between 20 and 2000 * C. Once the sample reaches the
desired temperature, the laser is fired several times over a span of a few minutes and the necessary data are collected for each laser
shot. The laser beam energy is absorbed in the front surface of the sample and creates a heat pulse that travels through the sample’s
thickness. This temperature rise ranges from 0.5 to 2 * C and is kept at the optimum range by adjustable filters between the laser and
the furnace. A high speed A/D converter records the temperature rise signal over time.
Heat flux
Back surface IR radiation

Laser energy
Sample width
Figure 32 A simple schematic diagram of the laser flash technique.
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Figure 33 Schematic diagrams of (a) power compensation and (b) heal flux differential scanning calorimetry. Adapted from Clas, S. -D.;
Dalton, C. R.; Hancock, B. C. Differential Scanning Calorimetry: Applications in Drug Development. Pharm. Sci. Technol. Today 1999, 2, 311–320.
Thermal conductivity measurement carried out by the laser flash method is applicable to many types of ceramics. Lanthanum
hexa-aluminate, abbreviated as LHA, has the potential to be applied as a high-temperature thermal barrier coating due to its relative
low thermal conductivity and low sinter ability at temperatures higher than 1100 * C (39). For Si/SiC ceramic materials, low thermal
conductivity is detected due to the presence of voids and excess glassy carbon surrounding the SiC grains (40). Before measuring the
thermal conductivity of this particular material, the surface is coated with a gold layer of 60 nm thickness, followed by a coating of
carbon black.
1.02.5.3 Heat Capacity

The specific heat (Cp) of a material is defined as the amount of energy (Q) required to raise a unit mass (m) of material by one unit of
temperature (DT) at constant pressure (eqn [17]).
Q
Cp ¼ [17]
mDT
Differential scanning calorimetry (DSC) is widely used to determine the heat capacity of ceramic materials. This method
monitors the difference in heat flow between a sample and a reference material as the sample is heated, cooled, or held under
isothermal conditions. There are two types of DSC instruments in commercial use today.
One is known as a ‘heat flux’ design, while the other is referred to as a ‘power compensation’ instrument, as shown in Figure 33
(41). For a power compensated unit, the sample and reference materials are held separate; each is with a self-contained calorimeter
with its own heater element. The fundamental measurement of either DSC device is a temperature differential, which is converted to
energy flow via a mathematical equation, and is an indirect approach as compared to the pure energy flow measurements in power-
compensated DSC.
1.02.6 Evaluation of Electrical and Magnetic Properties
Some of the advanced ceramics can display electrical conductivity or insulation and are used in many new industrial applications,
such as high dielectric capacitors, nonvolatile memories, data and information storage, sonar, energy conversion, and environ-
mental monitoring. The electrical and magnetic properties of these types of advanced ceramic materials are presented in this section.
1.02.6.1 Dielectric Property

A material that can be polarized by an applied electric field and can store energy is called dielectric material. Material that exhibits
a dielectric property is an electrical insulator and is used for making insulators, capacitors, and resistors.
Due to miniaturization, a decrease in applied potential, and an increase in the system complexity of microelectronic components
(such as a metal-oxide-semiconductor field-effect transistor) for further extending Moore’s law and scaling up components/devices,
a real need in the electronics industry is to use high dielectric constant materials (high-k dielectric). The high-k ceramic materials
facilitate in creating a far greater filtering effect, reducing current leakage and noise, lowering power loss, and decoupling
requirements. These materials also need to be able to withstand in range of temperature and high energy densities. Among the
possible materials available, ceramics are a promising one to fulfill these necessities. Ceramics exhibit high dielectric constant values
(high permittivity or high ability to polarize and hold charge) such as SiNx with 4 < k < 10, Ta2O5, Al2O3, ZrO2, HfO2 with
10 < k < 100, and PZT with k < 10. Ceramics with high breakdown voltages (dielectric strength) and good temperature stability are
the preferred dielectric for capacitors and memory cells.
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Figure 34 A typical dielectric strength test instrument.
On the other hand, some ceramic materials exhibit a low-k dielectric property (low permittivity or low parasitic capacitance, or
low ability to polarize and hold charge) such as nanoporous SiO2 and DLC (42) with a k value of approximately 2, and a capability
of faster switching speeds and lower heat dissipation. These ceramics are also very good insulators for isolating signal-carrying
conductors from each other.
The dielectric property of the insulating materials can be evaluated by measuring dielectric strength (Ds), dielectric constant (k),
and the dissipation factor or loss tangent (tan d). The dielectric strength of the ceramics can be defined as the maximum level of
electric field strength that it can withstand as an insulator material just before breaking down its insulating properties. The following
equation (eqn [18]) is used to determine the dielectric strength of a given ceramic:
Eb
Ds ¼ [18]
t
where Eb (V) and t (cm) are the breakdown voltage and the gap between two electrodes or the thickness of the insulator plate. This
equation can be used when the applied electric field is homogeneous. A high voltage test instrument (Figure 34), with an integrated
computer control and measuring system (such as a power circuit) including a voltage regulator, a high voltage generator, a detector
for monitoring optoelectronic breakdown impulse, and programmable logic controllers, is used for evaluating the dielectric
strength of the ceramic. The applied current can be direct or alternative current.
The dielectric constant (k), also called relative permittivity (εr), is a measure of the charge (electrostatic lines of flux) stored on an
electrode material that is brought to a given voltage. The k of ceramic materials is the ratio of its permittivity (ε0) to the permittivity
in a vacuum (ε0) (43). The dielectric constant of ceramic materials can be measured by the ratio of the capacitance of a ceramic
capacitor (Cc) and the capacitance of a similar capacitor in vacuum (C0). The equation for calculating k is given by eqn [19],
εc Cc
k ¼ εr ¼ ¼ [19]
ε 0 C0
The capacitance of a parallel-plate capacitor (Cc) is constructed of two parallel conductive plates with an area of A and separated
by a distance t (wthickness of ceramic) as expressed by eqn [20],
A
Cc ¼ εr ε0 [20]
t
The capacitance of capacitors, containing dielectric ceramic materials, can be measured by using commercial available digital
capacitance meters. The dissipation factor or loss tangent tan d of ceramic materials can be defined as the ratio of effective
conductance to susceptance and measured by using an impedance bridge.
The dielectric strength of ceramic materials is significantly influenced by the level of porosity, surface quality, and structural
properties of the ceramic materials. In generally, the dielectric strength of a particular type of ceramic materials, with a defect in it, is
noticeably lower as compared to the defect-free ceramics. By tuning the porosity levels and structure, low-k dielectric ceramic
materials, such as nanoporous silica, can be developed. Additionally, a recent development of advanced computational techniques
(such as first-principles-based density-functional theory (DFT)) is serving as an outstanding method to study the properties of the
electronic system of ceramic materials, such as the structural, vibrational, and dielectric properties. These techniques can be used for
faster development and better understating of new low- or high-k dielectric materials (44).
1.02.6.2 Piezoelectric Property

A piezoelectric ceramic is a smart material that converts a mechanical effect (such as pressure, movement, or vibration) into an
electrical signal and vice versa. Due to the electromechanical effect, piezoelectric ceramics are used in a wide range of applications
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such as motion sensors, watches, ultrasonic power transducers, lithotripters, ultrasonic cleaning, ultrasonic welding, active vibration
dampeners, high-frequency loudspeakers, actuators for atomic force microscopes, and many others. Lead zirconate titanate (PZT),
barium titanate (BT), and strontium titanate (ST) are the most widely used piezoelectric ceramic materials.
The piezoelectric nature of ceramic materials can be evaluated by measuring parameters such as the piezoelectric charge coef-
ficients (d constant), the piezoelectric voltage coefficients (g), and the piezoelectric coupling factors (k). Due to the anisotropic
nature of piezoelectric ceramic materials, constants d and g of the ceramic materials relate to both in the direction and the directions
perpendicular to the applied electric field or mechanical force. The d constant of ceramic materials is the ratio between the
mechanical strain developed per unit of electric field or polarization experienced per unit of mechanical stress, applied to
a piezoelectric material. Whereas, the g constant of ceramic materials can be defined as the mechanical strain developed per unit of
electric displacement, or electric field generated per unit of mechanical stress, applied to a piezoelectric material. High d is desirable
in ceramic materials used as actuators, such as in an AFM, where well-controlled motion and vibration are required during surface
scanning. The g is related to the d by the following equation (eqn [21]):
d ¼ εg [21]
where ε is the relative permittivity or dielectric constant of piezoelectric ceramic materials and is defined as the dielectric
displacement per unit electric field. The piezoelectric charge coefficients (d) can be measured by means of quasistatic (45,46)
and interferometric (47,48) methods. In the quasistatic technique, a static force is applied to a specific area of the piezo-
electric ceramic materials. The d is the ratio between the charge generated (Q) in ceramic materials to the static force (F)
applied to a defined area of the ceramic materials. However, the application of the quasistatic method is limited in many
cases as the measurement does not consider frequency dependencies and neglects the charge/polarization effect from the
space charges. In the interferometric technique, the change of the piezoelectric ceramic materials is detected as a function of
applied AC voltage between two ceramic materials. However, this technique usually requires a reflecting mirrorlike surface
and therefore can only be used for ceramic materials that exhibit mirrorlike surface. A material’s piezoelectricity can also be
assessed with the dynamic, resonance, and acoustical methods (49) to overcome the limitation described earlier. For
example, in the dynamic method, the charge signal of a piezoelectricity effect is periodic at a controlled frequency, when
a periodic force is applied. In this technique, the charge signal due to the piezoelectricity can be easily separated from any
other charge signal contributions.
The high piezoelectric voltage coefficients are required in materials intended for use as sensors and to generate voltage in
response to the mechanical energy. The overall ‘strength of the electromechanical effect’ of piezoelectric ceramic materials can be
expressed by the piezoelectric coupling factor. The piezoelectric coupling factors (k) can be defined by the following equation
(eqn [22]) (43),
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Electrical Energy Output Mechanical Energy Output
k¼ ¼ [22]
Total Mechanical Energy Input Total Electrical Energy Input
1.02.6.3 Superconductivity Property

Superconductivity is a phenomenon when the resistance of a material becomes zero to direct currents if the material is cooled below
its critical temperature (Tc). Below the critical temperature, a superconductive material will also exclude magnetic fields,
a phenomenon called the Meissner effect (50). The conditions for obtaining a superconductive property and different functional
properties of a ceramic superconductor are shown in Figures 35 and 36, respectively.
Figure 35 Critical phase diagram of the surface superconductive property of ceramic materials.
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Figure 36 Functional properties of ceramic superconductor materials.
Ceramic materials would exhibit superconductive property when H, J, and T are less than Hc, Jc, and Tc, respectively, where Hc, Jc,
and Tc are the critical magnetic field, current density, and temperature for superconductivity, respectively.
Superconductive ceramic materials can be used for a wide range of applications due to their unique functional properties as well
as their excellent mechanical, chemical, physical, and structural properties. For example, properties such as (1) zero resistance and
high current density, (2) low resistance at high frequencies and extremely low signal dispersion, (3) rapid single flux quantum
transfer and very high speed transmission, (4) magnetic field exclusion, and (5) the high sensitivity of superconductors to magnetic
field, enable ceramic materials to be used in applications for electric power transmission, communications technology, high-speed
computing, high-speed rail (magnetic levitation), and high-sensitivity sensors, respectively.
The critical temperature depends on the type of material. Materials with a higher critical temperature have especially
received a great deal of attention so that superconductivity could be maintained with liquid nitrogen for more practical
uses. Ceramic materials often exhibit multiple phases, and optimally doped ceramic material exhibits a superconductive
property with Tc much higher than metallic superconductors (51). For example, some types of ceramic materials (such as
YBa2Cu3O7 and Ti2Ba2Ca2Cu3O10) (52), which are generally insulators, have recently been found to be promising materials
that exhibit superconductive properties at high critical temperatures (Tc ¼ w90–125 K).
The superconductive characteristic of ceramic materials is evaluated by the critical temperature (Tc) and critical current density
(Jc). These properties can be assessed by using a magnetometer:
l To determine the Tc of the ceramic, the temperature dependence of the magnetization is measured in a constant external
magnetic field (H) at a range of temperatures.
l To estimate the critical current density, magnetization hysteresis loops of the ceramics are taken at different temperatures. The
external magnetic field is swept between specific magnetic fields for different temperatures. The width of the hysteresis loop is
proportional to the critical current density according to the Bean model (53) and is used to estimate Jc by the following equation
(eqn [23]), derived from the extended Bean model (54),
$ %" #
20 Mþ ' M' L1 '1
Jc ¼ 1' [23]
L1 3L2
where Mþ and M' are magnetization moments at increasing and decreasing field, respectively (hysteresis loop width at a particular
magnetic field strength, H), and L1 and L2 are sample dimensions perpendicular to the field.
The high critical temperature (Tc) and current density (Jc) are required for practical application of superconductive ceramic
materials in many applications. These properties are strongly influenced by the structure and chemical composition of ceramic
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materials. Schilling et al. demonstrated that by changing the number of CuO2 layers per unit cell, superconductivity above 134 K in
the Hg–Ba–Ca–Cu–O system is obtainable (52). The superconductive property of the ceramic materials is strongly influenced by the
amount and type of doping material (55). For example, the cuprate-based ceramic material exhibited superconductive properties
only if it was doped with a fraction between 0.1 and 0.2 (51).
By improving structural quality at the grain boundary and the stress-field pinning effect, Jc can be improved. Ozturket et al.
demonstrated that by Yb doping, the intergrain contact surface and number of flux pinning centers of a bulk YBa2Cu3O7'x ceramic
material significantly improved with an indirect enhancement of the ceramic’s superconductive property (56).
1.02.6.4 Semiconductivity Property

Transition-metal oxide ceramics from II to IV, such as TiO2, ZnO, NiO, Fe2O3, SnO2, and others, exhibit semiconductor properties,
and are used mainly for the applications of gas sensors, solar energy, and in the electronics industry. A semiconductor ceramic is
a material that has electrical conductivity between that of a metal and an insulator. The conductivity of the semiconductor is tunable
by doping with different types of anions and cations. For example, SnO2 and hematite (Fe2O3) were found be to potential materials
for a gas sensor application. Although pure hematite or tin oxide exhibited poor conductive properties, Si-doped hematite or
F-doped SnO2 exhibited very good conductivity due to an increase in the charge carrier density of the material. In solar energy,
a band gap (the energy gap between conduction and valance band) of semiconductor oxide ceramic material is a very important
property. The type of semiconductor (n-type or p-type), the conductive property, and the band-gap property are mainly influenced
by the type and amount of doping. The selection of the band gap depends on the application. Ideally, for solar energy a lower band-
gap oxide ceramic is required, which could absorb a larger amount of light from the solar spectrum. For example, the n-type
semiconductor titanium dioxide (TiO2) has been a prime candidate for photoelectrodes in the application of a photo-
electrochemical cell using solar energy due to its stability, nontoxicity, and relatively low cost. However, the band-gap size of the
TiO2 photocatalyst is w3.2 eV, which indicates that it only absorbs a small UV fraction of solar light (about 3–4%) which can be
utilized to induce electronic photoexcitation into the conduction band with the creation of holes in the valence band (10,57). This
leads to its relatively low photoactivity as an electrode. Doping the TiO2 lattice with various metals and nonmetals is a potential way
to improve the photoactivity of TiO2 in the visible region through reduction of the band edge. The semiconductor nature of ceramic
materials can be mainly assessed by their conductivity, band gap, and light absorption properties.
The conductivity of the semiconductor can be measured by using the four-probes IV measurement system as shown in Figure 37.
Electrochemical impedance spectroscopy (EIS) can be used to find the carrier density in the material through use of the Mott–
Schottky plot, which indirectly indicates the conductivity of a ceramic (58). The method of assessing the absorption properties
of ceramic materials is presented in Section 1.02.7.1.
The optical band gaps of TiO2 films can be calculated by eqn [24] using the data associated with the high absorbance region of
the UV–Vis transmittance spectra as follows (59):
$ %m
ahn ¼ A hn ' Eg [24]
where a is the absorption coefficient (equal to –lnT/d (60)), hn is the photon energy, Eg is the optical band gap, d is the thickness of
the coating, and A is a constant. The value of m may be taken as, m ¼ 2 and 1/2, a characteristic value for the indirect allowed and
direct forbidden transitions, respectively. For a polycrystalline coating, both direct and indirect optical transitions are possible,
depending on the band structure of the material. By plotting (ahn)1/2 versus hn and (ahn)2 versus hn (called Tauc’s plot), the indirect
and direct band gap (Eg) of the sputtered deposited TiO2 coating can be determined by the intercepts of the tangent to the plots,
respectively (7). Optical band-gap measurement using UV–Vis absorbance data of photoactive TiO2 ceramic coating for an indirect
allowed transition is shown in Figure 38.
Figure 37 Schematic diagrams of a four-point probe system.
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Figure 38 Optical band-gap measurement using UV–Vis absorbance data of photoactive TiO2 ceramic coating deposited at low and high
working pressure, (ahn)1/2 versus hn curves for indirect allowed transition. Reproduced from Rahman, M.; MacElroy, J. M. D; Dowling, D. P.
Influence of the Physical, Structural and Chemical Properties on the Photoresponse Property of Magnetron Sputtered TiO2 for the Application
of Water Splitting. J. Nanosci. Nanotechnol. 2011, 11 (10), 8642–8651.
1.02.7 Evaluation of Optical Properties
Due to inherent mechanical, chemical, and thermal properties as well as the development of nanotechnology, optical ceramics have
recently received a great deal of attention, particularly in the search for new applications, such as laser materials. Optical ceramics
can be defined as materials used for the construction of devices whose functions are to alter or control electromagnetic radiation in
the spectral region of ultraviolet, visible, infrared, or X-ray radiation. These ceramics are used for the fabrication of a wide range of
optical elements, such as lenses, mirrors, windows, prisms, polarizers, detectors, glass, optical fibers, optical switches, laser
amplifiers, and modulators. Based on their applications, optical ceramics can be classified into three main groups: transparent
ceramics, glass coloring, and luminescence ceramics. When choosing a special optical ceramic, depending on the type of appli-
cation, the most important optical properties are often spectral dependent transparency, absorbance, reflectance, luminescence, and
the refractive index. The structural uniformity, mechanical and thermal stability, and chemical resistance properties of the ceramic
materials might also need to be considered. In this section, different techniques used for assessing the optical properties of the
ceramic material are briefly presented.
1.02.7.1 Transitivity and Absorptivity

An optical ceramic that is transparent to visible or to infrared or ultraviolet radiation is widely used in many advanced engineering
applications such as solar energy or optical fiber. Transmittance (Tl), which is the indicator of transparency, is the fraction of an
incident light at a defined wavelength passing through a material (61,62) according to the Beer–Lambert law (eqn [25]). On the
other hand, absorbance or the absorption factor (Al) is the fraction of radiation absorbed by a sample at a specified wavelength and
can be evaluated by eqn [26].
I
Tl ¼ [25]
I0
I0 ' I
Al ¼ [26]
I0
In this case, I0 is the intensity of the incident radiation and I is the intensity of the radiation coming out of the sample. In these
equations, scattering and reflection are considered to be close to zero. In general, a spectrophotometer system is commonly
employed to measure the transmission properties of optical ceramics as a function of wavelength. This technique is also widely used
for obtaining information on material absorption, reflectance, and diffusivity properties using different controls and calibrations. In
a spectroscopic system, light from the source lamp is passed through a monochromator and is focused upon a sample. A fraction of
the light is transmitted or reflected based on the characteristics of the sample. Transmitted light is then passed through another
monochromator. The function of the second monochromator is to separate the light wavelengths and focus each of them onto the
photodetector.
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1.02.7.2 Reflection/Scattering Characteristics

Ceramic materials with special light reflecting properties have the potential to be used in a wide range of applications, including
optically pumped laser cavity reflectors, intense pulsed light therapy reflectors, reflectors in high-temperature luminaries, solar cell
manufacturing, and thermophotovoltaics (63). Ceramic materials made from binary and ternary group metal oxides exhibit high
reflective properties due to their high band gap, which allows very small amounts of light between the ultraviolet and infrared
spectra to be absorbed. Additionally, by controlling the refractive index, a highly reflective ceramic mirror could be produced, which
can be used in many optical components, including telescopes, optoelectronic devices, and sensors. Surfaces of ceramics can be
composed of mirrorlike (so-called specular reflection) and scattering (diffusion reflection) structures. This means that the incident
light will be spread out over a range of angles. Specular reflection and diffuse reflection (scattering) can occur when the particle size
of a ceramic surface is smaller or greater than the wavelength of incident light, respectively.
Reflectance spectroscopy is an emerging technology that can be used to measure internal, specular, and diffuse reflection from
a ceramic surface (64). It quantitatively measures the intensity of reflected light as a function of wavelength. The reflected light
maintains the same wavelength (elastic scattering), although different wavelengths are absorbed, transmitted, and reflected to
different degrees (65). Reflectance spectroscopy systems have three main components: light sources, fiber optic probes, and
spectrometers.
The reflective property (R) of ceramic materials can also be estimated using eqn [27],
" #
n1 ' n2 2
R¼ [27]
n1 þ n2
where n1 and n2 are the refractive index of air and ceramics, respectively. The refractive index can be measured using a spectroscopic
ellipsometer (66). The ellipsometric data can be recorded at different incident angles. A number of mathematical models including
Cauchy and B-Spline are applied to fit the measured ellipsometric data to obtain the refractive index.
1.02.7.3 Luminescence Property

Recently, the study of luminescent ceramics including AlN, BeO, and 3Al2O3$2SiO2 (mullite) has attracted a great deal of interest for
the application of personal radiation dosimetry, dental ceramic, tiles, optical communications, and solar concentrator (67). For
example, transparent luminescent ceramic material can be used in fiber optics and solar concentrators for amplifications of light
intensity to improve performance. Luminescence is an emission of light that can be produced by several means, including after light
(photo) absorption, chemical reactions, electrical energy, and stress in material. The luminescent properties of ceramics could be
measured by using methods such as photoluminescence (PL), thermoluminescence (TL), and optically stimulated luminescence
(OSL). Photoluminescence is the luminescence of a material that proceeds when the material is irradiated with light (ultraviolet
or visible).
PL, TL, and OSL are characterized mainly by either emission spectra or excitation spectra. Emission spectra are obtained when
material is irradiated/heated with a fixed wavelength/energy for a specific time period and is plotted as emission intensity versus
emission wavelength at fixed irradiation. In contrast, excitation spectra are plotted as emission intensity versus irradiation wave-
length or energy at a fixed emission wavelength.
PL and OSL experiments, as well as some TL experiments, can be carried out using a spectroscopic system that mainly consists of
(1) a lamp as a source of UV light with a grating monochromator, (2) a prism monochromator and photomultiplier tubes, or
a grating monochromator equipped with a CCD camera for analyzing the luminescence signal, and (3) a heating source with
a temperature controller. Radiation (such as beta, gamma, X-ray, and UV light) assisted TL and OSL measurements can be carried
out by using a TL/OSL reader with linear heating (using hot gases) and an optical multichannel analyzer. A beta/gamma source is
generally built inside readers, whereas UV irradiation can be obtained from a metal halide, deuterium, or other lamp (68).
Bailife et al. (69) used TL and OSL techniques to investigate the luminescent properties of BeO, a dental ceramic used for
manufacturing crowns and prosthetic teeth. The OSL response of this ceramic was recorded to be linear over a range of absorbed
doses (<100 mGy to >5 Gy, where Gy ¼ Gray is the SI unit equivalent to joules per kilogram), which is suitable for the needs of
retrospective dosimetry. The luminescent property was observed in mullite ceramics for the application of a solar concentrator after
conducting a substitutional type of doping of Cr3þ for Al3þ in mullite.
1.02.8 Evaluation of Nuclear Properties
Due to the excellent physical, thermal, and mechanical properties of some advanced ceramic materials, such as MgAl2O4 (spinel)
(70), PuO2, and UO2, researchers and engineers predict that, in the near future, they could be widely used in a hostile nuclear
environment. These include such things as structural components for fusion reactors, ceramic containers for the transportation and
permanent storage of nuclear waste, cladding materials for gas-cooled fission reactors, and inert fuel matrices for actinide trans-
mutation, where efficient use of energy is a primary concern. In addition to excellent physical, thermal, and mechanical stability, one
of the prime requirements for most of these applications is the need for ceramic materials to be stable under radiation. Radiation
can induce defects in ceramics by structural modifications, such as swelling, phase transformations, polygonization, amorphization,
and topological or chemical disorders, which depend on the type of ceramic, type of irradiation, radiation energy, and other factors.
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The radiation stability and the nature of radiation defects of nuclear ceramic materials can be evaluated by performing different
types of interactions (such as nuclear collision, electronic excitation, and the synergetic process of nuclear collision and electronic
excitation) associated with the slowing down of energetic particles by the ion beams. Various types of accelerators are used to deliver
the ion beams with a broad energy range (KeV to GeV) (71). Radiation damage that builds up in ceramic materials can be char-
acterized by Rutherford backscattering spectrometry (RBS). Additionally, advanced material characterization techniques, such as
transmission electron microscopy (TEM), X-ray diffraction (XRD), and Raman spectroscopy can be employed to evaluate the
damage buildup, radiation defects, change of phase, and structure in ceramic materials to gain a better understanding of the
mechanisms involved in the damage caused by the radiation (71).
1.02.9 Evaluation of Biomedical Properties
Due to their biocompatible properties, ceramic materials have attracted a lot of attention as a biomaterial for repairing or replacing
diseased and damaged body parts (72–74). Generally two techniques are used for testing biomedical properties of ceramic
materials: in vivo and in vitro. In vitro is a first phase laboratory test, where a test material is immersed in physiological fluid that has
the same ion concentration as that of living bodies to get the approval for whether the material can be used in the living body
conditions or not. Furthermore, in vitro tests can be helpful in understanding and predicting the performance of the material after
the implantation in a living body. In vivo test involves the implantation of a test material in a living animal body in order confirm its
suitability as a biomaterial by investing the interaction of the material with the living tissues. This is a second phase test of material
before the implantation in the human body. This section will focus on the in vitro aspects of biocompatibility testing.
Broadly bioceramic materials can be classified into three categories according to the tissue response when implanted (Figure 39).
The first one is a bioinert ceramic such as alumina, which shows little or no tissue reaction. The second one is bioactive ceramic such
as bioglass, which reacts with local tissue in a positive way to form bonds with the bone or even with the soft tissue of a living
organism. The third one is resorbable or biodegradable ceramic material such as calcium phosphate, which could be a porous or
nonporous structures and it is gradually replaced by tissue (75).
1.02.9.1 Biocompatibility
In simple terms, biocompatibility is a way of measuring the degree of compatibility of a material or device with a biological system.
Biocompatibility refers to the ability of a material to perform a specific physiomechanical function without causing any harm to the
surrounding tissue or biological systems (76). Biocompatibility of a material depends on a number of factors, such as the elemental
characteristics of the material, tissue characteristics around the implant material, and length of exposure. Therefore, to accept
a material as biocompatible, a number of tests are performed to determine any potential harmful effect on the living body. In vitro or
in vivo biocompatibility tests are performed either directly on the material or on material extracts. In general, materials are extracted
using a culture medium. In vitro testing methods for biocompatibility can be found in a number of references (75,77,78).
The first step for assessing the biocompatibility of ceramic materials is an in vitro toxicity test such as cytotoxicity (79,80).
Cytotoxicity refers to an activity of an agent, which causes destructive action on certain cells leading to both functional and structural
damage. Cytotoxicity is evaluated using a variety of methods and parameters, such as morphological studies of cell, quantification
of cell damage or growth, and measurement of specific cellular activity. Although a number of cell types can be used for cytotoxicity
tests, generally a human or mouse fibroblast cell type is preferred. A large number of cytotoxicity screening assays are available for
Figure 39 Different types of bioceramics.
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measuring biocompatibility. They are very helpful in screening materials before conducting in vivo tests. Cytotoxicity assays measure
the cell death caused by the implanted material or their extracts. The most commonly used technique for studying biocompatibility
is cell culture (81).
Cytotoxicity test can be performed either by direct or indirect methods. In the direct method, the cytotoxicity of cells is assessed
through direct contact with the material. The monolayer cells are placed directly in contact with the test materials. The cells are then
incubated in a culture medium in a controlled environment (37 * C) for a certain period of time. After incubation, the monolayers
are evaluated in terms of the presence or absence of a zone of cellular effects beneath and surrounding the sample. A popular
technique for cytotoxicity test is MTT, which is a colorimetric assay for measuring the activity of enzymes that reduce MTT to
formazan, giving a purple color (77,78). Cytotoxicity, cell viability, and cell proliferation are assessed by this assay. Cytotoxicity
study with a fibroblast cell line showed that dental ceramics are biocompatible with no toxic effect. Three different methods, namely
the agar overlay test, the Millipore filter test, and the MTT test, were used for the cytotoxicity tests (82). The indirect method is
designed to assess the toxicity to the cells from the leachable extracts of the ceramic materials. Among the indirect methods, the
MEM (minimum essential medium) elution test is commonly used (83). In this method, materials are extracted in a cell culture
media. The extracts are transferred onto a layer of cells. Subsequently, the cells are incubated and examined microscopically for
indications of cytotoxicity.
The cytotoxicity effect can be evaluated either qualitatively or quantitatively (84). Qualitative evaluation of cell prolif-
eration can be carried out by microscopy examination of the cultured cells such as light, transmission electron, and scanning
electron microscopes (78). Any visible sign of toxicity from the bioceramic is indicated by a change in the size, appearance,
and configuration of the cells leading to malformed, degenerative, or lysed cells. Cell proliferation or cell viability study is
used to measure the cytotoxic effect of ceramic materials. Cell viability can be measured using a Trypan blue dye exclusion
assay, which selectively colors only dead cells blue (85). This distinctive blue color can be observed under a microscope.
Another technique is called LIVE/DEAD assay, which simultaneously determines live and dead cells with different colors.
The counting of viable cells is used as a measure of the relative cell growth, which is calculated using the following formula
(eqn [28]) (85):
ðK ' EÞ
% of viable cells ¼ " 100% [28]
ðK ' K0 Þ
where K0 is the cell number at the time of the addition of sample, K is the cell number after cultivation for a certain period of time
without the sample, and E is the cell number after cultivation for the same period of time with the sample.
1.02.9.2 Bioactivity
The ability of material to bond biologically through the growth of a layer on the implant is defined as bioactivity. In general, the
layer is characterized as a biologically active hydroxyapatite (HA), which helps in the formation of direct bone bonding. Therefore,
bioactive ceramic materials are very useful for bone repairing. The simulated body fluid (SBF) test is generally considered to be the
most efficient method to characterize the bioactivity of ceramic materials in a physiological environment (86–89). The test evaluates
the bone-bonding ability of a material through an examination of apatite formation on the material surface in SBF. In vitro
bioactivity tests are carried out by soaking ceramic specimens in the SBF at physiological conditions of temperature (37 * C) and pH
(7.4). Figure 40 presents an example of a ceramic sample in SBF for a bioactivity test. Careful consideration is given in preparing the
SBF solution in which the formulation contains ion concentrations very close to those of human blood plasma. The detailed
Figure 40 Ceramic specimen in a simulated body fluid (SBF) for a bioactivity test. Adapted from Kokubo, T.; Takadama, H. How Useful is SBF
in Predicting in Vivo Bone Bioactivity? Biomaterials 2006, 27 (15), 2907–2915.
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procedure for preparing the SBF solution has been outlined by Kokubo and Takadama (86). The solution is filtered in a standard
filtering system.
The volume of SBF employed for testing is calculated based on the following equation (eqn [29]):
Sa
Vs ¼ [29]
10
where Vs is the volume of SBF in ml and Sa is the specimen surface area (mm2). This formula is used for solid material. However, for
the porous materials, the volume of SBF used is more than the calculated volume.
The specimen is soaked for different periods within 4 weeks, as it generally takes this duration for any bone bonding material to
form apatite on the specimen surface. The specimen is removed from the SBF and dried without heating to characterize the
properties (crystallinity, morphology, etc.) of the apatite formed by using XRD and SEM coupled with X-ray energy dispersive
spectroscopy (EDS).
A bioactivity test carried out on composites filled with silicate and borate glasses showed evidence of apatite formation on the
surface (90). Precipitation started to form after 3 days, as observed by SEM. After 7 days the specimens were fully covered with
a homogeneous layer of precipitates, which represented the characteristics of hydroxyapatite with needlelike crystalline. EDS and
XRD results also confirmed the formation of calcium phosphate. The bioactivity test with SBF on nanocrystalline hydroxyapatite
ceramic material also showed good response in forming an apatite layer (91).
1.02.9.3 Biodegradability
The biodegradable characteristics of ceramic materials can be exploited for biomedical applications such as drug delivery and
fracture fixation. The degradation rate of the material will determine how long the material will remain in the body (92–94). In vitro
biodegradability tests of ceramic materials are performed by the weight-loss method. Ceramic samples are prepared and weighed in
a high-precision microbalance. Subsequently the samples are immersed in a bottle of phosphate buffered saline (PBS) solution
(pH ¼ 7.4) and left in a controlled environment (37 ) 1 * C) for 1–8 weeks. PBS solution is regularly replaced to maintain a constant
pH value. At the end of the test period, the sample is washed, dried, and weighed. The degradation characteristics of the sample are
calculated as the remaining weight with the following equation (eqn [30]):
W2
Remaining weight ð%Þ ¼ [30]
W1
where W1 is the sample weight before degradation and W2 is the sample weight after degradation. The variation in the remaining
weight (%) is monitored over time to calculate the degradation rate. Degraded samples are characterized by microscopy techniques.
Biodegradability study with polyurethane (PU)/nanohydroxyapatite (nHA) composites with different nanohydroxyapatite
compositions (0, 10, 20, 30, and 40 wt.%) showed that weight loss occurred in all materials (93). The maximum degradation was
observed for pure nHA, with a weight loss of 5%.
The bioresorbable properties of an a-tricalcium phosphate (a-TCP) ceramic porous body were evaluated by the released
amounts of calcium and phosphate ions from the porous body in a buffered solution. A strong relationship between dissolution
and porosity was found. This means that an increase in porosity increases the dissolution rate (95). An in vitro degradation test was
conducted on biodegradable polymer (polyhydroxybutyrate-cohydroxyvalerate, PHBV) and bioceramic/polymer composite
(nanosized hydroxyapatite, nHA/PHBV) scaffolds to assess the biodegradation rates (i.e., the mass loss rate) and changes in material
or structural properties. PHBV and nHA/PHBV scaffolds degraded over time in phosphate-buffered saline at 37 * C as indicated by
mass losses, molecular weight loss of PHBV, decrease in compressive mechanical properties, increase in polymer crystallinity, and
loss of structural integrity (96).
1.02.9.4 Antibacterial Property

Methicillin-resistant Staphylococcus aureus (MRSA) is an increasing problem all over the world. A great deal of attention has been
drawn to the photocatalytic antibacterial and self-cleaning activity of titanium dioxide (TiO2) ceramic material (97,98), whose
activity is independent of temperature. Antibacterial properties of the TiO2 ceramic surface can be evaluated by using bioactivity
facilities. Staphylococcus (S. aureus and S. epidermidis) can be used as organisms for the antibacterial surface studies (99). The bacteria
can be cultured overnight in Brain-Heart-Infusion media, subcultured into fresh media, and inoculated onto the surface. The efficacy
of the surface material is assessed through viable cell counting. Microscopically, bacterial activity is analyzed through fluorescent
probes under a confocal microscopic and an AFM, with cell morphology assessed under an SEM. The material’s antibacterial activity
can be characterized under various time and temperature conditions.
1.02.10 Conclusions and Future Outlook
Ceramic materials are widely used in advanced engineering applications and cannot be replaced by other materials due to their
unique properties for enhancing the performance of components in service. In order to tailor ceramic materials with a specific
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property, a good knowledge of the correlation between property and process is required. In this chapter, the authors have attempted
to give a brief overview of the assessment of the physical, mechanical, and functional properties of advanced functional ceramic
materials. Both traditional and advanced characterization methods have been discussed to facilitate understanding of the ceramic
properties. No particular method was found to be the single best testing method to measure these properties.
Any new developments in ceramics will require further understanding of material properties and processing routes. Recent
developments in advancement characterization technologies (such as nanoscale material testing tools), modeling tools, and data
analysis techniques with better computation methods are expected to explore novel properties and applications of advanced
ceramics. However, a considerable amount of work will still need to be done for the development of standardized test methods for
the newly developed advanced ceramics of all forms. Standard testing methods will need to be developed for very high temperature
characterization of the ceramic materials used in nuclear and space applications. For biomedical applications, standard test methods
are still lacking for accurate prediction of long-term mechanical stability and reliability of bioceramic materials. In vitro tests need to
be further developed for accurately measuring the biocompatibility of ceramic materials before doing the in vivo tests. Future work
should be focused on utilization of existing modern equipment for detailed investigation of ceramic properties as well as the
development of further techniques.
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1.03 Testing of Polymeric Materials
CJG Plummer, Ecole Polytechnique Fédérale de Lausanne (EPFL), Lausanne, Switzerland
1.03.2 Polymeric Materials 36
1.03.3 Characterization of Basic Physical Properties 38
1.03.3.1 Molar Mass Distribution 38
1.03.3.2 Thermal Properties 40
1.03.3.3 Microstructural Characterization 42
1.03.3.4 Chemical Analysis 44
1.03.4 Polymer Rheology 44
1.03.4.1 Shear Rheometry 45
1.03.4.2 Oscillating Shear and Time–Temperature Superposition 46
1.03.4.3 Extensional Flow Rheometry 48
1.03.5 Solid-State Mechanical Properties 48
1.03.5.1 Dynamic Mechanical Analysis 48
1.03.5.2 Large-Strain Testing 50
1.03.5.3 Rate-Dependent Testing 52
1.03.5.4 Creep and Dynamic Fatigue 52
1.03.6 Fracture and Impact Testing 53
1.03.6.1 Impact Tests 54
1.03.6.2 Linear Elastic Fracture Mechanics Testing 55
1.03.6.3 Elastic–Plastic Fracture Mechanics Testing 56
1.03.6.4 Time-Dependent Crack Propagation 58
1.03.6.5 Fatigue Crack Propagation 58
1.03.6.6 Test Methods for Elastomers 59
1.03.7 Fiber-Reinforced Polymer Composites (FRPs) 60
1.03.7.1 Mechanics of Composite Materials 60
1.03.7.2 Mechanical Testing of Composites 61
1.03.7.2.1 Tensile Tests 61
1.03.7.2.2 Compression Tests 61
1.03.7.2.3 Flexural Tests 61
1.03.7.2.4 Shear Tests 61
1.03.7.3 Fracture Testing of Composites 63
1.03.7.4 Single-Fiber Debonding 65
1.03.7.5 Nondestructive Testing 65
1.03.8 Environmental Testing 67
1.03.8.1 Thermal Aging 67
1.03.8.2 Weathering 67
1.03.8.3 Thermal Degradation and Fire Resistance 68
1.03.8.4 Biodegradation 68
1.03.9 Conclusions 69
References 69
1.03.1 Introduction
Polymeric materials (1,2) have gained enormous practical importance since the establishment of the basis for modern polymer
science in the period leading up to World War II (3). Synthetic polymers are most widely exploited in the form of plastics; namely,
formulated thermoplastic or thermoset resins (thermosets represent around 10% of total production) (4,5), and fiber-reinforced
plastic (FRP) composites (6). The building and construction and transport industries require significant volumes of all of these
materials. Consequently, service lifetimes are often measured in decades, and a major challenge is to render plastics sufficiently
robust with respect to both short- and long-term loading, often in the presence of a relatively aggressive environment. However,
around 40% of thermoplastics production is destined for packaging applications, where the turnover rate may be extremely high. In
this case, the emphasis lies on the disposal or recycling of plastics in ways that are both economically and environmentally
acceptable. Moreover, while commodity plastics in use today (high- and low-density polyethylene (HDPE and LDPE), isotactic
polypropylene (PP), atactic polystyrene (PS), atactic polyvinyl chloride (PVC), and others) have long been considered to be

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36 Testing of Polymeric Materials
inexpensive materials that are also inexpensive to process once the necessary infrastructure is in place, there is increasing concern
over the dependence on petroleum for their production. This concern is currently driving two apparently contradictory trends. On
one hand, resin producers have a huge interest in developing a new generation of economically viable bio-based (and, in some
cases, biodegradable) plastics to replace not only petroleum-based commodity plastics (and bio-based polylactides (PLA) and
starch-based plastics have already made significant inroads into the packaging market) but also higher performance ‘engineering’
plastics (7). On the other hand, there is a resurgence in interest in plastics in general and composites in particular, regardless of
whether they are derived from petroleum, as efforts intensify to reduce energy costs through the use of lightweight materials (8,9).
The focus in this chapter is on polymer testing for bulk plastics and composite applications, whose success is primarily
dependent on achieving adequate mechanical and structural performance in a part or in an assembly of parts (which may include
other types of material) with the required shape, as well as maintaining this performance during service. This requires at least some
knowledge of the physical characteristics of the polymer. After a brief introduction to polymeric materials in Section 1.03.2, some
basic physical property measurement techniques are introduced in Section 1.03.3 and cover molar mass, thermal properties,
morphology, and chemical structure. Given the substantial investment associated with typical melt-processing routes, such as
injection molding, in which the plastic is subject to complex flow fields under highly nonisothermal conditions (owing to the low
thermal conductivity of most plastics), modern process design relies extensively on numerical simulations of both the processing
route and the final properties of a given part. As these simulations become more elaborate, the requirements for input data will also
require more elaboration. The flow behavior is of primary importance in this context, and particular attention will therefore be given
to rheological characterization in Section 1.03.4, including steady-state and dynamic-shear rheometry, capillary, and elongational
rheometry. Prediction and tailoring of the in-service performance involve a range of solid-state test methods, which are discussed in
subsequent sections: low-strain dynamic mechanical analysis, conventional large-strain tensile testing and its variants, high-speed
testing, and static and dynamic fatigue (Section 1.03.5); fracture mechanics-based testing, impact testing, and slow crack growth
(Section 1.03.6); and test methods for polymer composites (Section 1.03.7). Finally, environmental testing will be briefly
considered in Section 1.03.8.
Testing in all of these areas has become highly standardized, mainly due to the importance of obtaining reliable data for design
and computer-aided engineering. A large number of standard test methods have been published by associations such as ASTM
(United States/international) (10), DIN (Germany) (11), JIS (Japan) (12), and ISO (international) (13), and practice varies
substantially in different countries. These standards are too numerous to be discussed systematically here, and indeed it is not the
goal of the present work to provide detailed test protocols (for which the standards literature should be consulted), but rather to give
an overview of the scope of the basic methods, some of which are not yet standardized. Moreover, many polymer applications (such
as those in the biomedical and electronics industries) depend on other very specific aspects of their functionality, and it is not
possible to cover all of these aspects in any useful depth in the present work. As a result, many important physical properties are not
treated, including optical, acoustic, and electrical properties; tests specific to certain classes of application, such as textiles, coatings,
and adhesives; and methods for the direct testing of structures in industry.
1.03.2 Polymeric Materials
Polymers are materials composed essentially of macromolecules; namely, relatively long sequences of covalently linked, generally
organic monomers (1). Plastics are polymeric materials that contain various additives that ensure adequate properties in service and
during processing (plasticizers, lubricants, ultraviolet (UV) stabilizers, flame retardants, tougheners, etc.) (4,5,14). The basic
macromolecular architectures are summarized in Figure 1 and cover most of the architectures found in bulk polymer applications.
Commercial polystyrene (PS) is a linear homopolymer derived from vinyl polymerization of a styrene monomer, hence the name
Figure 1 Classification of macromolecules according to their monomer sequence and chain architecture.
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Testing of Polymeric Materials 37
‘polystyrene.’ Styrene acrylonitrile (SAN) is a linear random copolymer prepared from styrene and acrylonitrile. Styrene butadiene
styrene (SBS) is a block copolymer consisting of blocks, which are extended sequences of styrene and butadiene linked to one another
by covalent bonds. In this case, it would be a triblock copolymer that consists of two styrene blocks separated by a butadiene block.
Acrylonitrile butadiene styrene (ABS), widely used in plastic housing for consumer electronics goods, consists of butadiene blocks
and random sequences of SAN.
Most commercial thermoplastic polymers are composed of flexible linear or branched macromolecules with weight average
molar masses, Mw (see Section 1.03.3.1), upward of around 30 000 g mol'1, depending on the synthetic procedure. In the absence
of external constraints, these long chains spontaneously adopt coiled conformations that show a high degree of interpenetration
when the polymer is in the condensed state. Thus, while a thermoplastic polymer melt may be able to flow at sufficiently elevated
temperatures, its viscosity is typically very high and depends on the molar mass distribution, degree of branching, and flow rate.
Melt processing is possible and widely used for thermoplastics, but this process usually requires large shear forces. On the other
hand, these very high Mw are also at the origin of the unique properties of polymers, as compared with their low molar mass organic
counterparts.
One important characteristic of many polymers is the ease with which they may be vitrified. Because of their limited mobility,
macromolecules are at best able to crystallize only partially from the melt at cooling rates typical of industrial processes, and
polymers containing random sequences of comonomers, extensive branching or cross-linking, or random orientations of asym-
metric units (as in the case of PS) may be unable to crystallize at all. Such ‘amorphous’ polymers nevertheless become rigid when
cooled through their glass transition, and, in many cases, their glass transition temperature, Tg, may be well above room temperature
(e.g., Tg is about 100 * C in the case of PS), which results in a room-temperature shear modulus, G, of the order of 1 GPa, as sketched
in Figure 2. Moreover, the absence of any long-range organization in glassy amorphous polymers, coupled with their lack of
absorption in the range of wavelengths corresponding to visible light, means that they are often highly transparent.
While glassy polymers are generally referred to as plastics, which implies a certain macroscopic ductility, many, including PS,
show relatively brittle behavior at room temperature, particularly when deformed in tension. This is due to the excessive localization
of plasticity in the form of crazes. Crazes are cracklike fibrillar deformation zones that are often associated with crack nucleation and
propagation (15). The competition between crazing and homogeneous plastic yielding (associated with macroscopically ductile
behavior) as a function of material parameters and external variables, such as temperature, has been a major focus of investigations
into the microdeformation behavior of both amorphous and semicrystalline polymers, and has also been driven by the need to
understand and control the fracture and impact resistance of plastic components in many of their applications (16–19).
Figure 2(a) also shows that in amorphous thermoplastics, G does not fall to zero at temperatures immediately above Tg, contrary
to what one would expect for a low molar mass glass-forming substance. This is due to the persistence of entanglement effects – the
topological constraints on relative chain motion that stabilize large deformations in glassy polymers. Thus, G remains roughly
constant at some three orders of magnitude less than in the glassy state, and also remains roughly constant over a range of
temperatures that increases strongly with Mw. Within this ‘rubbery’ plateau, polymers are capable of large reversible extensional
deformations at low loads, facilitating processes such as fiber spinning and blown film extrusion. However, for processes such as
Figure 2 Schematic evolution of the shear modulus, G, with temperature for (a) amorphous thermoplastics with different molar masses, M; (b) a lightly
cross-linked amorphous polymer; and (c) a semicrystalline thermoplastic.
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injection molding, it is necessary to work at higher temperatures, where the polymer melt behaves more as a highly viscous fluid and
where the viscosity scales roughly as M3w.
The mechanical properties become strongly time-dependent in the vicinity of the transitions between these different regimes of
behavior, as reflected by the tendency of polymers to show extensive stress relaxation at constant deformation (1,18–20). An
important consequence of these trends is that the choice of Mw for an industrial thermoplastic usually represents a compromise
between processing and final performance: if Mw is too high, many types of processing may no longer be feasible, while too low an
Mw will result in poor mechanical properties in the solid state. It follows that cross-linked polymers, whose Mw is effectively infinite,
cannot be melt processed. The cross-linking reaction must therefore take place subsequent to shaping of an un-cross-linked
precursor, which may itself be a polymer, as in the case of many elastomers; or a low-viscosity monomeric or oligomeric resin, as in
the case of conventional thermoset resins. In elastomers, light cross-linking is used to extend the rubbery plateau and to stabilize
large deformations in the rubbery state (Figure 2(b)); whereas in rigid thermosets, the much higher degrees of cross-linking may
result in exceptional heat stability and chemical resistance (21).
Certain thermoplastic polymers, including HDPE, LDPE, and PP, are capable of partial crystallization, and hence remain
relatively rigid between Tg and their melting point, Tm (Figure 2(c)). The Tg of many industrially important semicrystalline
polymers is well below room temperature, so their mechanical properties under service conditions are highly dependent on their
microstructure and degree of crystallinity, as well as on solidification conditions. The degree of crystallinity is also influenced by the
chain architecture, with LDPE showing more branching than HDPE (Figure 1(b)), which restricts crystallization and leads to
a softer, more ductile mechanical response at room temperature. On the other hand, in high-Tm engineering semicrystalline
thermoplastics such as polyether ether ketone (PEEK), Tg is also relatively high, and the amorphous regions are generally glassy,
which results in exceptional combinations of mechanical properties and heat stability. As shown in Figure 2(c), depending on Mw,
melting often occurs beyond the limit of the rubbery plateau, so that melt processing is possible immediately above Tm. In contrast,
crystallization results in significant shrinkage during solidification, so that injection molding of high-quality semicrystalline plastic
parts requires careful control of the temperature and pressure throughout the processing cycle.
Both amorphous and semicrystalline polymers may also show spontaneous molecular ordering in the melt state, given
a sufficiently rigid chain architecture, in which case they are referred to as thermotropic liquid crystalline polymers (LCPs). LCP-based
plastics generally show excellent flow properties and high temperature resistance, but remain expensive and may show excessive
mechanical anisotropy, depending on their processing conditions (22).
While Figure 3 shows that the Young’s moduli (0.2–10 GPa) and tensile strength or yield stress (typically in the range of
10–100 MPa) of solid polymers are relatively modest compared with those of metals and ceramics, plastics are highly versatile
materials, with price performance ratios that render them suitable for a huge range of applications that require adequate mechanical
properties and complex shapes, particularly where their low density and excellent corrosion resistance bring added value (23).
Process optimization is essential for plastic production, given the often high initial outlay for polymer-processing equipment, but
numerous techniques have developed to the point where flow behavior, nonisothermal solidification in the presence of complex
flows, and the final mechanical performance of a plastic part (stiffness, strength, vibrational response, and others) may be reliably
predicted, and the same models can be used to optimize mold design without the need for expensive trials, if adequate materials
data are available. If these plastics are to be used as high-performance structural materials, however, they must be reinforced. This
has led to enormous investment in the field of structural FRP composites, which combine low density with mechanical perfor-
mances comparable to those obtained with metals or ceramics (Figure 2(b)). However, many FRPs show highly anisotropic
properties, which place particular requirements on design and consequently on test methods (6,9,24,25).
A further important consideration in the context of both plastics and FRPs is their stability with respect to environmental
degradation during service and end-of-life disposal. Plastics generally show far better corrosion resistance than metals, for example,
but they are highly sensitive to ionizing radiation and thermo-oxidative degradation even at modest temperatures, with potentially
undesirable consequences for both service performance and processing (26). They also tend to be inflammable, often giving off
toxic degradation products during combustion. As a result, many of the additives used in industrial plastics are specifically aimed at
limiting degradation and improving their fire resistance. Environmental and fire testing are central to optimization of these additive
packages, and can provide design limits for long-term failure (14). Where recycling is not an end-of-life option for plastics, as is
frequently the case, it is also important to establish conditions under which they may be safely eliminated, for example, by
incineration or composting (27,28).
1.03.3 Characterization of Basic Physical Properties

1.03.3.1 Molar Mass Distribution
Because of the stochastic nature of typical industrial polymerization processes, the molecular weight of the individual macro-
molecules that constitute a polymer may vary widely within a given batch and depend strongly on the reaction conditions.
Therefore, one usually refers to either a number average molar mass:
N
P
ni Mi
Mn ¼ i¼1N [1]
P
ni
i¼1
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1000
1. Modulus-density Diamond Engineering WC-Co
Sl3N4
Young's modulus E B SiC ceramics
(G = 3E/ 8; K = E.)
MFA:88-91 Be Aluminas
Mo W-Alloys
Sialons Zr O2 Alloys
Si BeO Ni Alloys
CFRP Steels
Uni-ply Glasses Ge Cu Alloys
100 Pottery TiAlloys
KFRP Al Zn Alloys
GFRP Alloys
Tin
CFRP Rock, stone Alloys
½ Cement, concrete
(E )
Engineering Laminates
m s ¯1 composites GFRP Lead
KFRP alloys
104 Ash
Oak
Mg Porous
Young's modulus, E (GPa)
Pine Alloys ceramcs

Fir
10
Parallel
MEL Engineering
To grain PC alloys
Balsa Epoxies
Wood PS
PMMA
products
PVC
Woods Nylon Engineering
polymers
3 x 103 Ash PP Polyesters
Oak
1.0 Pine
Fir
HDPE
Lower E limit Perpendicular
for true solids to grain Guidelines for
PTFE minimum weight
Spruce LDPE design
Balsa E =C
Plasticized
PVC
103
0.1
Hard Elastomers
butyl PU
2 ¹⁄²
3 x 10 E =C
Cork
Polymers
Silicone ¹⁄³
Soft
foams butyl
E =C
0.01
0.1 0.3 1.0 3 10 30
Density, (mg m–3)
Figure 3 Comparison of the Young’s (tensile) modulus and density of different classes of materials, including plastics, elastomers, and FRPs. After
Ashby, M. Materials Selection in Mechanical Design; Pergamon: Oxford, 1992.
where ni is the total number of chains with molar mass, Mi, or a weight average molar mass:
N
P
ni M2i
i¼1
Mw ¼ N [2]
P
ni Mi
i¼1
and a polydispersity index, P ¼ Mw/Mn, which is a measure of the broadness of the molar mass distribution.
As Section 1.03.2 implies, the distribution of M is fundamentally important to plastic performance and processing. Many
techniques used to characterize the molar mass give a single parameter (e.g., Mn (osmometry), Mw (light scattering), or Mv (the
viscosity average molar mass, which is obtained from the solution viscosity and whose value is influenced by polymer–solvent
interactions (1))). However, it is also possible to access the full distribution by gel permeation chromatography (GPC), which is the
most widely used technique for this purpose. GPC involves passing a dilute polymer solution through a column containing
a discontinuous porous medium with pore volumes that have the same order of magnitude as the hydrodynamic volume, Vh, of the
macromolecules, which increases monotonically with M. The range of the measurement is therefore limited by the choice of pore
size, which should ideally be adjusted to suit the characteristics of the polymer to be measured – in the case of very broad
distributions, it may be necessary to use several different columns. The pores are less accessible to the larger polymer molecules, and
these large molecules pass through the column more rapidly than the smaller molecules. The concentration of the solution is
measured as a function of elution time from changes in the refractive index, absorption, or light scattering, according to the choice of
detector, which may also provide complementary information on chemical composition or, in the case of light scattering, M
itself (29).
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In conventional GPC calibration, a relative molar mass distribution is determined from a calibration curve that relates the
retention volume (the volume of eluent entering the column between injection and the appearance of the maximum concentration
of a given component) to M for a series of nearly monodisperse standards. Because the available standards may not be chemically
similar to the polymer to be characterized, this cannot necessarily provide a reliable indication of the absolute values of M.
However, with the addition of a viscosimetric detector, it is possible to make on-line measurements of the intrinsic viscosity,
h ' ho
½h( ¼ lim [3]
4/0 ho 4
as a function of retention volume, where 4 is the polymer concentration, h is the solution viscosity, and ho is the solvent viscosity.
Assuming that the retention volume depends uniquely on Vh, regardless of the chemical structure, the distribution in M may be
calculated from the relationship Vh ¼ [h]M and a ‘universal calibration curve’ in which log([h]M) is determined as a function of Vh
for a series of standards. These measurements also give access to the Mark–Houwink constants k and a, defined by
½h( ¼ kMa [4]
which may provide considerable insight into the polymer structure, as a is highly sensitive to the degree of chain branching (29,30).
While GPC is a very powerful technique, it requires expensive apparatus and skilled operation, suitable solvents may not be
available for a given polymer, and it may be difficult to interpret data for polymers with complex architectures or that interact
strongly with the column (although a suitable choice of column medium and solvent may substantially reduce these types of
specific specimen–column interactions). For rapid comparison of different lots of a given polymer, it is often more convenient to
resort to simpler methods, such as solution viscosimetry, which provides [h] and hence Mv through the use of eqn [4]. Another
commonly used measure is the melt flow index (MFI), which is defined as the mass of a quantity of a polymer, in grams, that flows
through a capillary of a specific diameter and length at fixed temperature, T, and pressure, P, in 10 min. Because the melt viscosity
increases strongly with Mw, polymers with low Mw typically show a relatively high MFI, but other factors, such as polydispersity and
chain architecture, also play important roles, so that the MFI does not provide a direct indication of molar mass. On the other hand,
the MFI does reflect the ease of flow of the melt of a thermoplastic polymer, which may ultimately be of more interest for assessing
the polymer’s processing characteristics.
1.03.3.2 Thermal Properties

Many fundamental thermal properties of practical importance (Tg, Tm, and the heat capacity at constant pressure, Cp), as well as
reaction rates, crystallization rates, or any phenomenon that results in a change in enthalpy or heat capacity, may be characterized by
differential scanning calorimetry (DSC) (Figure 4). In a basic DSC measurement, one monitors the difference in power required to
maintain a constant T or heating rate, dT/dt, simultaneously in an empty aluminum pan and a similar aluminum pan containing
a few milligrams of the specimen. With proper calibration and knowledge of the specimen mass, this difference may be converted
directly into an effective Cp. A stepwise increase in Cp with T in a heating scan is usually associated with the glass transition, as shown
in Figure 4(b), while a positive or negative peak indicates a change in enthalpy. With many modern instruments, it is also possible
to modulate a temperature scan by superposition of a small periodic fluctuation in T, and hence distinguish between reversing and
nonreversing components of the signal (Figure 4(c)) (31). This is useful, for example, for separating the Cp variations associated
with Tg, which appear in the reversing signal, from enthalpic peaks in the same temperature range.
DSC is a key tool for the investigation of the solidification kinetics of semicrystalline thermoplastics. Crystallization rates have
direct implications for both processing and the final degree of crystallinity and melting range, which are in turn important for
mechanical properties, as Section 1.03.2 discusses. The enthalpy is monitored as a function of time, t, either under isothermal
conditions or at a constant cooling rate, and is used to calculate a degree of solidification or a degree of crystallinity, X(t), using
theoretical values for the enthalpy of crystallization of a 100% crystalline specimen (Figure 4(d)). X(t) is often analyzed in terms of
the Avrami equation, which is a model-dependent expression for the rate of crystallization (32), and may need to be complemented
by direct observations of the microstructure; for example, by hot-stage optical microscopy.
The analysis of nonisothermal measurements is complicated by systematic lag between the specimen temperature and the
program temperature, which depends on the specimen mass and scanning rate. This influences not only the apparent crystallization
rates during cooling scans but also the Tm measurements. While Tm for an ideal single-phase crystalline substance corresponds to
onset of the melting peak in a heating scan, the local melting temperature typically varies widely within a single polymer specimen,
due to variations in the local crystalline lamellar thicknesses, which are in turn highly sensitive to the initial crystallization
conditions. This may result in a very broad peak with an ill-defined onset. Tm is therefore typically taken to correspond to the peak
temperature, which is strongly scanning rate dependent, and precise measurements therefore require a combination of low scanning
rates and small specimen masses. Low melting–point lamellae may also melt and recrystallize during the scan, so that the main
melting peak is not necessarily representative of the initial state of the specimen, resulting in an apparent Tm that varies little with
crystallization conditions. Note that a modulated DSC allows one to separate contributions from recrystallization and melting to
the overall signal to some extent, but this requires careful adjustment of the measurement parameters (31).
Dilatometry is an alternative method for the investigation of Tg and crystallization kinetics. Because the crystalline phase is denser
than the amorphous phase at a given T, measurements of the specific volume provide an indication of the degree of crystallinity,
while the glass transition is marked by a sharp decrease in the thermal expansion coefficient with decreasing T. These measurements
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Figure 4 (a) View of the interior of a DSC cell showing the reference and specimen platforms, which are heated independently; (b) DSC heating and
cooling scan of a typical semicrystalline thermoplastic (in this case, polyamide 6,6 (PA6,6)), showing the melting peak and the corresponding recrys-
tallization peak during subsequent cooling; (c) different signals obtained from a modulated DSC heating scan of an initially amorphous specimen of
polyethylene terephthalate (PET), showing both crystallization and melting, as well as a clear glass transition; and (d) baseline-corrected heat flow in
polyoxymethylene (POM) cooled from the melt and crystallized isothermally at 120 * C, along with the corresponding evolution of the degree of solidi-
fication, expressed as the integral of the heat flow curve up to time t divided by the total area of the heat flow curve.
depend on direct determinations of the volume and, as a result, can be extended to very low rates, contrary to DSC measurements,
where the signal is proportional to the rate of heat flow. However, the most important use of dilatometry is perhaps for the systematic
determination of pressure–volume–temperature (PVT) diagrams (Figures 5(a) and 5(b)) (33). PVT diagrams are extremely important
for processes that involve solidification in closed molds, such as injection molding, where shrinkage can result in warping, internal
voiding, and trapped internal constraints, which may promote long-term crack growth. Such measurements require pressure dila-
tometry. One approach to pressure dilatometry is to use a piston to maintain the specimen under constant P, while T is varied and the
volume, V, monitored, as shown in Figure 5(c). However, fluid confinement (Figure 5(d)) using mercury, for example, is required to
apply a uniform hydrostatic pressure (and the use of a piston may lead to significant shear stresses in solid specimens). The resulting
PVT diagrams then show V(T) for different pressures at a constant cooling rate. While the cooling rate influences both Tg and the
degree of solidification at a given temperature, basic fixed cooling rate diagrams of this type remain a valuable guide to injection
molders, for example, who may need to optimize hold times and pressures during the mold filling cycle, in order to compensate for
shrinkage, particularly with semicrystalline plastics. Currently available pressure dilatometers are typically incapable of operating at
the very high cooling rates generally associated with industrial processing. Other common applications for pressure dilatometry
include the study of the pressure dependence of polymer phase transitions, reaction rates, and constitutive behavior.
Thermal transitions may also be monitored by static force thermal mechanical analysis (TMA), in which an indenter is brought into
contact with the specimen at a constant load and its displacement monitored as a function of T. Variants include zero-force thermal
mechanical analysis, also referred to as thermodilatometry (although it is more limited in scope than true dilatometry), which is
widely used to measure thermal expansion coefficients in solid polymers. A simplified form of static force TMA is also used for
determining the Vicat softening point, which is a commonly used industrial standard for plastics. In this case, the softening point
(which is related to Tg in the case of a glassy polymer) is defined as the temperature at which a loaded, flat-ended needle penetrates
the specimen surface during heating by a certain distance. The heat deflection temperature or heat distortion temperature (HDT) is also
widely used in industry as a measure of the high-temperature mechanical stability of solid polymers, and can provide an indication
of the temperature at which it is safe to eject injection molded thermoplastic parts. In this case, a specimen loaded in bending under
standard conditions is heated until it deflects by a given fixed amount. As with the Vicat softening point, the somewhat arbitrary
definition of the HDT implies that it has no direct physical meaning. On the other hand, the intrinsic rate dependence of
phenomena associated with the glass transition means that even measurements based on changes in fundamental properties
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Figure 5 (a) PVT diagram for a glassy amorphous polymer (PS), showing the decrease in thermal expansion coefficient associated with the glass
transition; (b) PVT diagram for a semicrystalline polymer (PP), showing the stepwise increase in density associated with crystallization; (c) piston-
operated pressure dilatometer; and (d) fluid confinement pressure dilatometer. After Zoller, P.; Walsh, D. Standard Pressure Volume Temperature Data for
Polymers; Technomic: Lancaster, 1995.
(specific volume, Cp, modulus, dielectric constant, etc.) have limited significance if the experimental technique and conditions are
not specified (1,20).
Another important thermal characterization technique is that of thermal gravimetric analysis (TGA), in which the specimen weight is
monitored as a function of temperature under a controlled atmosphere. TGA may be used, for example, to determine the inorganic
contents of filled specimens (by pyrolysis of the polymer), volatile contents, or degradation kinetics at different T or heating rates (see
Section 1.03.8.3), and is also often combined with mass spectrometry to produce a more detailed analysis of the degradation products.
Finally, a number of methods exist for determining the thermal conductivity of polymers, which are required as input for many
process simulations. The most usual and most rapid are transient source techniques, which make use of either a plane or line heat
source coupled with a temperature sensor. In the transient line source method, these elements are combined in a needle probe that
may be inserted into a polymer melt. If a known quantity of heat is supplied to the heater, one can calculate the thermal
conductivity from the measured rise in temperature over a given time interval as the specimen heats up (34).
1.03.3.3 Microstructural Characterization

Plastics laboratories are typically equipped for a range of direct morphological characterization techniques, including optical
microscopy (OM), scanning electron microscopy (SEM), occasionally transmission electron microscopy (TEM), and, increasingly, atomic force
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microscopy (AFM). The choice of technique depends on the scale of the features to be observed and also on the required range of useful
magnifications. SEM, for example, is particularly suited for combining detailed observations with overviews of a given specimen at
low magnifications with a far greater effective depth of field than conventional OM. Subnanometer resolution is possible with TEM
or AFM in principle, given suitable specimen preparation. However, in structural polymers, one is often more interested in features at
length scales of the order of 10 nm, characteristic of crystalline lamellar thicknesses; the internal structure of deformation induced
defects, such as crazes; and microphase separation in block copolymers. A spatial separation of 10 nm is routinely attainable with the
latest generation SEM, TEM, and AFM, but is well beyond the diffraction limit of around 200 nm in classical OM. On the other hand,
for much routine work on the morphology of semicrystalline polymers, phase dispersions, reinforcement, the quality of molded
parts, failure analysis, and other types of diagnostics, OM is largely sufficient, provided there is adequate contrast (35).
Transmission OM and TEM of bulk specimens require thin sections of material, of a thickness less than 100 nm in the case of
TEM, while thicker sections that depend on the transparency and contrast of the material in question are used for OM. Such sections
may be prepared from plastics by microtoming, but cryomicrotomy may be necessary for rubbers or low-Tg semicrystalline poly-
mers (35,36). For materials that are difficult to section, such as composites that contain hard inclusions (e.g., glass fibers), alter-
natives include petrographic polishing for OM, and field ion beam milling (FIB) for SEM and TEM, which may be adapted for serial
sectioning and three-dimensional reconstruction (36,37).
In transmitted light OM, the inherent lack of contrast in many types of polymer specimens may be overcome by various
techniques, such as phase contrast imaging, polarized light microscopy for birefringent specimens (e.g., semicrystalline polymers
(Figure 6(a)) or LCPs), or Nomarski differential interference contrast. Fluorescent labeling or autofluorescence is also widely used in
studies of segregation or phase separation and is often combined with laser-scanning confocal OM, which permits a precise choice
of the incident excitation wavelength and 3D reconstruction from thick transparent specimens. In TEM, contrast is again a problem
with pure polymer specimens, particularly since beam damage may result in the rapid loss of fine structure. However, selective heavy
metal staining of multiphase specimens gives not only excellent contrast in many cases (Figure 6(b)) but also relatively stable
images, even at high-beam doses (35). Staining is also suitable for use with SEM in backscattered electron (BSE) imaging modes
(Figure 6(c)), with the advantages that there is no need for thin sectioning and that the straightforward observation of large
specimen areas is possible. TEM of replicated selectively etched surfaces was formerly popular for the observation of multiphase
specimens, and it remains useful for nondestructive examination of the surface morphology of bulk polymers (35). However,
replication has now largely been superseded by high-resolution SEM and AFM, although AFM is less adapted to specimens with
large height variations (such as fracture surfaces). Reflected-light OM is another option for low-resolution observation, but the low
reflectivity of many polymers necessitates metallization if the surface topography is of primary interest. Note that metallization or
carbon coating is also used routinely in SEM to reduce charge accumulation. With relatively flat specimens, AFM may be used in
conjunction with a wide variety of contrast mechanisms. The energy dissipation contrast obtained in intermittent contact mode
phase imaging is especially convenient for the observation of polymers containing phases with contrasting rigidity (block copol-
ymers (Figure 6(d)), blends, semicrystalline polymers, composites, and others), bearing in mind that cryomicrotomy may be
needed to obtain sufficiently flat surfaces to eliminate the artifacts that are associated with surface topography (35,38). As with OM,
AFM imaging may be carried out in air or in a liquid environment, contrary to conventional TEM and SEM, which require a high
vacuum. However, environmental SEM (ESEM) and related TEM techniques make it possible to work with relatively high partial gas
pressures in the vicinity of the specimen, and are useful for the observation of hydrated specimens, for example.
Three-dimensional structures may also be indirectly investigated by scattering techniques such as X-ray and neutron scattering (41).
In small-angle scattering experiments, interpretation depends on models to at least some extent, but this interpretation tends to provide
average information, in contrast to direct microscopical observation, in which individual specimens examined are not necessarily
representative of the majority of cases. X-ray and neutron scattering also result in relatively little damage to the specimen as compared
with electron irradiation, although high-resolution or in situ measurements of deformation mechanisms require high-intensity sources,
and therefore also require access to large-scale facilities. Another technique that is increasingly popular is micro-X-ray tomography,
Figure 6 Common microstructural features observed in plastics by the use of various microscopic techniques. Reproduced from Gensler, R. The
Effect of Thermooxidative Degradation on the Mechanical Performance and the Microstructure of Polypropylene. Ph.D. Thesis No. 1863, Ecole Poly-
technique Fédérale de Lausanne, 1998 and Lalande, L. Structure et mécanismes de microdéformation de polymethylmethacrylates renforcés au choc.
Ph.D. Thesis No. 3891, Ecole Polytechnique Fédérale de Lausanne, 2007. (a) OM of spherulites in a microtomed section from a semicrystalline PP molding
observed between cross-polarizers; (b) TEM of lamellar structure in polypropylene (microtomed section stained with RuO4, in which the amorphous
regions appear dark); (c) core–shell rubber particles in impact modified PMMA observed by SEM in BSE mode of a microtomed surface stained with RuO4
(the rubber-rich regions appear light); and (d) AFM intermittent contact mode phase image of a PMMA–PBD–PMMA triblock copolymer.
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Figure 7 Micro-computed tomography (micro-CT) scan from a polylactide foam: (a) Single slice; and (b) 3D reconstruction. Reproduced from Delabarde,
C. Bioresorbable Nanocomposite Foams for Bone Tissue Engineering. Ph.D. Thesis No. 5111, Ecole Polytechnique Fédérale de Lausanne, 2011.
which is used for investigations of porosity, including damage-induced porosity in deformed specimens, composite materials, and
foams (Figure 7) (42). Further techniques principally used for the investigation of damage in FRPs will be reviewed in Section 1.03.7.5.
1.03.3.4 Chemical Analysis

Chemical analysis of polymers and plastics is a vast subject that involves a wide range of techniques (44) that can be only touched
upon here. Fourier transform infrared spectroscopy (FTIR) is perhaps the most widely used technique for routine analysis; it detects
absorptions associated with specific chemical groups. The attenuated total reflection (ATR) mode is particularly convenient, because
little or no specimen preparation is required. FTIR is used not only for rapid identification of polymers by fingerprinting, but also for
monitoring degradation and reaction kinetics, and, in certain cases, the degree of crystallinity (45). FTIR and Raman spectroscopy
may also be combined with direct imaging to provide chemical surface mapping. In conventional FTIR microscopy, the maximum
resolution is typically on the order of a micron, whereas Raman spectroscopy may be combined with scanning confocal OM to
provide 2D mapping in transparent specimens with a resolution approaching 200 nm (noting the limitation that Raman spec-
troscopy is not suitable for fluorescent specimens). Higher resolution mapping requires techniques such as TEM or SEM combined
with X-ray spectroscopy, or TEM combined with electron energy loss spectroscopy (EELS). SEM and X-ray spectroscopy are
commonly used in industry for the identification of second-phase inclusions in plastic parts, such as catalyst residues, which may
often play an important role in failures. However, application of such techniques to the analysis of the polymers themselves is
limited, as they have a tendency to degrade rapidly in the electron beam (35).
1.03.4 Polymer Rheology
Because the effective melting points of thermoplastics are much lower than those of typical metals and ceramics, melt processing
may be carried out at relatively low temperatures. However, polymer melts show distinct rheological characteristics that must be taken
into account in process design. As shown in Figure 2 (discussed in this chapter), amorphous polymers retain solidlike behavior,
albeit with a reduced modulus, in the regime of temperatures corresponding to the rubbery plateau immediately above Tg, whose
extent increases with Mw. However, even in regimes of T where the behavior tends to that of a viscous fluid, that is, beyond the upper
limit of the rubbery plateau or Tm (whichever is higher), the shear viscosity, h, of a molten thermoplastic is typically between 103
and 105 Pa s depending on T and Mw, whereas molten steel has a viscosity of the order of 0.01 Pa s (and even low M thermoset resins
may have viscosities of up to 1 Pa s prior to cross-linking). The h may be reduced somewhat by increasing T, but thermal degradation
places severe restrictions on maximum processing temperatures, so that, as Section 1.03.2 indicates, polymer melt processing is
inevitably associated with large stresses, and processing equipment must be adapted to adequately deal with these large stresses.
A polymer melt also continues to show considerable melt elasticity in nominally viscous regimes, depending on the timescale of
the deformation. This has far-reaching practical implications, such as those for die swell and instabilities during extrusion. As
a result, the melt is by definition viscoelastic (20), and its behavior may deviate substantially from that of a classical Newtonian
fluid, for which the shear stress
s ¼ hðTÞdg=dt [5]
where h(T) is independent of the shear rate, dg/dt. Indeed, as Figure 8 shows, molten plastics (and many polymer solutions) often
show pronounced shear thinning (a decrease in h with dg/dt at high dg/dt) owing to molecular orientation in the flow direction,
which may be represented by a power law
s ¼ Kðdg=dtÞn [6]
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Figure 8 Steady-state shear response of PP at 220 * C: (a) Rotational shear rheometry with the cone-plate geometry; and (b) capillary rheometry.
The inset shows a schematic representation of the response of a typical shear-thinning polymer melt. Reproduced from Houphouet-Boigny, C. Fiber
Reinforced Polypropylene Nanocomposites. Ph.D. Thesis No. 3851, Ecole Polytechnique Fédérale de Lausanne, 2007.
where K is the consistency index. Such behavior may lead to highly nonuniform shear rates even in relatively simple flow geometries,
although in the low dg/dt regime, whose extent depends on the polymer in question, eqn [5] remains a reasonable approximation
in many cases. The simplest constitutive laws for use in simulations of polymer melt flow are often combinations of eqns [5] and
[6], with the range of dg/dt corresponding to common process routes (100–1000 s'1 for extrusion and 10 000–100 000 s'1 for
injection molding) generally extending well into the power law regime (cf. Figure 8).
A basic goal of polymer melt rheology is to investigate how the stress varies with flow rate in order to determine the dependence
of the flow behavior on materials and processing parameters, both as a means of basic quality control (in which case measurement
of the MFI may suffice; see Section 1.03.3.1) and to provide input for process design. At the same time, it is a powerful tool for
studying the basic physics underlying the dynamics of long-chain molecules, as well as their reaction kinetics, degradation, phase
separation, or any other phenomenon that has a direct impact on flow behavior.
1.03.4.1 Shear Rheometry

While the above discussion leads one to the conclusion that there is no clear-cut distinction between a polymer solid and a polymer
melt, shear rheometers are better adapted to measurements on viscous specimens that require some degree of confinement, as
opposed to dynamic mechanical analysis (DMA, whose practical aspects will be covered in Section 1.03.5.1), which is designed for
more rigid, self-supporting specimens. In the case of a highly viscous polymer melt, it is usually sufficient to sandwich the specimen
between two rigid, flat, parallel plates with a well-defined separation (Figure 9(a)). The plates may then be subjected to either
a linear or a rotational relative displacement or force in order to shear the polymer. The cone-plate geometry (Figure 9(b)) is also
routinely used for testing polymers in rotation. In this case, the effective plate separation is
dzrtan a
where r is the radial distance from the axis and a is the cone angle. The increase in d with r compensates for the increase in
displacement rate of the rotating part of the fixture (usually the cone), given by rU, where U is the angular velocity, so that
dg/dt ¼ U/tan a throughout and the macroscopic shear rate is well defined (with a fixed plate separation d, the local shear rate will
Figure 9 A rotational rheometer along with schematics of various specimen holder geometries used in rotational shear rheometry: (a) Plate–plate
geometry; (b) cone plate geometry; (c) coaxial cylinders; (d) Mooney geometry; and (e) solid torsion bar.
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depend on r). On the other hand, this configuration is restricted to low effective d (cone angles are typically <4* ) and is
sensitive to misalignment, whereas d may be varied arbitrarily in the plate–plate geometry, allowing one to investigate
suspensions that contain relatively large second-phase inclusions, such as short glass fibers, in which case d should ideally be
10–100 times the effective diameter of the inclusions. However, the use of a large d to investigate non-Newtonian melts may
lead to significant through-thickness variations in dg/dt, considerably complicating the analysis, even where the constitutive
behavior of the fluid is known beforehand. While the possibility of varying d allows one to test for such effects, as well as other
artifacts (such as wall slip), it is frequently desirable to restrict d as far as practically possible when attempting to investigate the
behavior of complex fluids. The coaxial cylinder or ‘Couette’ geometry (Figure 9(c)) is clearly less versatile in terms of d, but is
also widely used because it provides better confinement in the case of low-viscosity specimens, such as polymer solutions or
weak gels. Finally, the Mooney coaxial disc geometry (Figure 9(d)) is popular in the rubber industry because it allows one to
work under an applied hydrostatic pressure, reducing wall slip, which can be particularly problematic in commercial rubber
formulations (47).
In all the configurations shown in Figure 9, the torque or rotational displacement rate applied to the mobile part of the fixture
may be either constant or oscillatory (see Section 1.03.4.2). Measurements of the displacement rate or torque, respectively (along
with the normal force in many cases), are typically made as a function of time, t, angular frequency, u, or T, although measurements
of static stress relaxation or creep in response to a steplike change in displacement or torque are possible, depending on whether the
instrument operates in stress- or strain-controlled mode. Both types of instrument are widely used, although it should be borne in
mind that they may not give equivalent results in nonlinear regimes of behavior. Rotational rheometers are also commonly adapted
to combine rheological measurements with optical or electrical measurements, chemical analysis, photo-cure (photo-rheology), or
in situ monitoring of fiber orientation (47,48).
A further variant on shear rheometry is capillary rheometry, in which the fluid is forced through a tube under conditions of
laminar flow at a fixed pressure drop or flow rate, while monitoring the flow rate or pressure respectively. This approach is
widely used in industry, mainly because it is better suited to measurements at dg/dt >100 s'1 (cf. Figure 8) than rotational
rheometry, namely, in the range that directly corresponds to injection molding and extrusion. It may also be extended to
microfluidic set-ups for very small quantities of liquid. However, this method is not adapted to oscillatory or static measure-
ments, and it needs to be used carefully for thermosets to avoid blocking the capillary. Finally, torque rheometers, which measure
the torque on the mixing screws or rotors in standard process configurations, also provide indications as to the ease with which
a given material may be processed and/or process-induced changes in the material properties, but do not provide a direct
measure of the viscosity.
1.03.4.2 Oscillating Shear and Time–Temperature Superposition

Oscillatory measurements play a particularly important role in polymer rheometry and DMA, because they allow one to
discriminate directly between the elastic and viscous contributions to the mechanical response (1,19,20). Consider a sinusoidal
applied strain, g ¼ go sin ut. A linear elastic solid will follow Hooke’s law:
s ¼ Gg ¼ Ggo sin ut [7]
where G is the shear modulus; whereas in a Newtonian fluid, the stress depends on the shear rate (cf. eqn [5]), so that
s ¼ hdg=dt ¼ hgo ucos ut [8]
In the intermediate case of a linear viscoelastic material, as illustrated in Figure 10(a), there is a phase difference, 0 < d < p/2,
between the stress and the shear, such that
s ¼ so sinðut þ dÞ ¼ h0 go ucos ut þ h00 go usin ut [9]
Figure 10 (a) Schematic of the signals monitored in an oscillatory measurement; and (b) dynamic response of a cross-linked polyurethane at constant
frequency in the temperature range corresponding to the glass transition (DMA measurement at 1 Hz in tension).
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where
so so
h0 ¼ sin d; and h00 ¼ cos d [10]
ugo ugo
correspond to the viscous and elastic contributions to the overall response and the quantity tan d ¼ h0 /h00 is a measure of the energy
dissipation per cycle. It is often more convenient in solid-state measurements to express the dynamic response in terms of the storage
and loss moduli, G0 and G00 , which are defined from
s ¼ G0 go sin ut þ G00 go cos ut [11]
where
so so
G0 ¼ cos d; G00 ¼ sin d [12]
go go
and tan d ¼ G00 /G0 . It follows from eqn [9] that G0 h uh00 and G00 h uh0 . As a result, as d tends to 0, G00 tends to 0 and G0 tends to G
(eqn [7]), and as d tends to p/2, h00 tends to 0 and h0 tends to h (eqn [8]).
Figure 10(b) shows the dynamic response of a typical amorphous polymer in a constant-frequency DMA scan in tension in the
temperature regime corresponding to the glass transition (so that results are given in terms of the tensile storage and loss moduli, E0
and E00 , rather than G0 and G00 ). E0 shows essentially the same trends as E and G in static measurements (Figure 2), that is, a decrease
of two to three orders of magnitude as T increases through the glass transition, and a rubbery plateau whose extent depends on Mw
(effectively infinite for the cross-linked polyurethane in Figure 10(b)). A strong peak in tan d appears in the glass transition zone,
referred to as the a peak in amorphous polymers, and further peaks in tan d are visible at lower T (referred to as b, g, and so on in the
order in which they appear as T is reduced). These peaks reflect additional secondary transitions, which are known to be of
importance for ductility in solid polymers (1,19).
Because the moduli vary strongly with T, it may be necessary to combine different experimental configurations in order to cover
wider ranges of T. This problem is compounded in the frequency domain, where it would be necessary to extend an isothermal
measurement over many orders of magnitude of u in order to obtain data representative of all the regimes of behavior shown in
Figure 10(b). In practice, it is difficult to vary u by more than 3–4 orders of magnitude, because of both time constraints and the
limitations of the experimental apparatus. However, it has been established that within certain ranges of T, and, if necessary, with
small corrections to take into account density changes and the dependence of the rubbery modulus on T,
G0 ðu; To ÞzG0 ðaðTÞu; TÞ [13]
where a(T) is a shift factor (20). In principle, one could construct an extended isothermal frequency sweep by scanning over limited
ranges of u at different T, and then using eqn [13] to increase the effective frequency range at a selected reference temperature, To. In
practice, given that a(T) is not well known a priori, this is done empirically by shifting curves measured at different T along the u axis
to build up a master curve, as shown in Figure 11 (49). Note that a(T) may be predicted for T immediately above Tg, using the
phenomenological Williams–Landel–Ferry (WLF) relationship with universal constants (20), but this is not accurate enough for
many practical purposes. To justify such a time–temperature superposition (TTS) procedure, the same a(T) should also superpose G00
and tan d, and is strictly applicable to a linear regime only. However, where these criteria are met, TTS allows one not only to increase
the effective range of frequencies in dynamic tests, but also to predict the response of specimens to static loading (creep or relax-
ation) at times well beyond those that are practically accessible. Moreover, the general principle of time–temperature equivalence is
widely evoked in many other practical situations where it is necessary to infer the time or frequency dependence of physical
phenomena from their variation with T (18).
Figure 11 Time–temperature superposition: (a) A master curve obtained by time–temperature superposition of isothermal frequency scans of
a cross-linked polyurethane at different temperatures covering the whole of the glass transition; and (b) the corresponding shift factors (reference
temperature 37 * C). Reproduced from Azra, C. Unpublished Results, Ecole Polytechnique Fédérale de Lausanne, 2011.
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Figure 12 Experimental configurations for extensional rheometry: (a) Simple instrumented haul-off device coupled to a capillary rheometer; and (b)
paired wind-up drums for carrying out extensional measurements using a rotational rheometer. After Sentmanat, M.L., US Patent 6691569.
1.03.4.3 Extensional Flow Rheometry

In many practical situations, such as fiber spinning, injection molding, and blow molding, the polymer will be subjected to
predominantly extensional flow rather than shear flow, but obtaining uniform extensional flow in a fluid under controlled
conditions is not straightforward, and the precise test configurations used in elongational flow rheometry depend greatly on the
range of viscosities to be measured. As a result, capillary break-up measurements may be feasible in low-viscosity fluids, but for most
polymer melts, it is necessary to deform free-standing specimens in tension. Test configurations range from simple instrumented
haul-off devices coupled to a capillary rheometer (Figure 12(a)) that simulate fiber drawing but are ill suited to isothermal
measurements, to dedicated instruments designed to submit fibers or films to controlled tensile deformations at a constant true
extensional strain rate, that is, in which the deformation rate increases exponentially in order to compensate for the increase in
specimen length at high strains (Figure 12(b)) (47,50).
1.03.5 Solid-State Mechanical Properties
While melt rheology is primarily aimed at assessing processing characteristics, the final performance of plastics in structural polymer
applications greatly depends on their mechanical performance in the solid state, namely, their stiffness under various modes of
solicitation; the ultimate properties, including fracture properties, will be treated separately in Section 1.03.6. The stiffness is
typically characterized in terms of elastic constants derived from the low-strain linear response to applied stresses. On the other
hand, solid specimens tend to show strongly nonlinear behavior at high strains, culminating in either yielding or catastrophic
failure, so that there is no direct equivalent to steady-state rotational rheology at a constant shear rate. Two widely used approaches
to the testing of solid specimens are DMA and large-strain tensile or compression testing at a constant strain rate, which is carried out
using conventional tensile test apparatus (19). Such apparatus may also be adapted for shear, relaxation, and creep measurements,
and, in some cases, to dynamic fatigue (large-strain cyclic deformation) (51). Figure 13 summarizes these basic modes of static
mechanical solicitation. As with melt rheology, the deformation rate is crucially important for the mechanical response of the
specimen in the solid state, and test procedures must often be adapted to the assessment of high-speed performance in regimes of
temperature relevant to applications where the component is potentially subject to impact loading (as in car bumpers). Moreover,
in cases in which one is interested in the intrinsic constitutive behavior, which may be required as input for numerical simulations
(such as when it may be important to compensate for instabilities such as plastic necking), it is possible to obtain this by measuring
and controlling the local strain rate, rather than relying on a constant cross-head displacement. This scenario, as well as the need for
noncontact extensometry for many types of specimens, has led to the development of optical and video test control methods, which
will be discussed briefly at the end of this section (52).
1.03.5.1 Dynamic Mechanical Analysis

As stated in Section 1.03.4, modern DMA is essentially the solid-state counterpart of rheometry, and may be used for both oscil-
latory and static measurements. The time and temperature regimes investigated using the two techniques overlap substantially.
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Figure 13 Schematic representation of the tensile stress–strain response of solid-state polymer specimens under displacement and stress control,
schematically showing the evolution of the stress and strain in each case: (a) Constant strain rate tensile test; (b) stress relaxation at constant strain; and
(c) creep at constant stress.
Moreover, a standard rotational rheometer may be used to test rigid solids in torsion, as shown in Figure 9(e). It is also possible to
use DMA to investigate viscous liquids, provided that there is adequate mechanical support: for example, this method could be used
to investigate a sample of a compliant solid foam. As with shear rheometry, DMA instruments are available with both stress (force)
and strain (displacement) control, but given that glassy or semicrystalline polymers and elastomers are self-supporting, measure-
ments are generally carried out in tension–compression and bending, rather than rotation, as shown in Figure 14. Moreover, the
emphasis is mostly on low-strain testing in the linear elastic regime, and the detection and analysis of thermal transitions such as the
glass transition and the sub-Tg relaxations referred to in Section 1.03.4.1. Under these conditions, simple specimen geometries
suffice and the deformation may be measured directly from the cross-head displacement. Analyzers based on free resonance or
damping of free vibrations have also been widely used to investigate damping behavior, and can provide an indication of the
various thermal transition temperatures (19,20). However, while these processes are relatively simple to implement, they are
considerably less versatile than force- or displacement-controlled instruments.
Figure 14 Simple tensile test configuration, along with different specimen geometries commonly used in solid-state testing: (a) Tension; (b)
three-point bending; (c) four-point bending; (d) single cantilever; and (e) uniaxial compression.
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1.03.5.2 Large-Strain Testing

Routine tensile testing is typically carried out under displacement control on specimens with standard geometries deformed to
failure (either fracture or plastic yielding depending on the characteristics of the specimen) at a constant nominal strain rate dε/dt,
where ε is the nominal strain, defined as
l ' lo
ε¼
lo
where l is the instantaneous length and lo is the initial gage length of the specimen. Many research and service facilities are equipped
with screw-driven tensile test machines that are capable of operating at different strain rates and temperatures with interchangeable
load cells and specimen grips, which provide access to a wide range of maximum loads. If fatigue or high-speed testing is required,
however, it may be necessary to resort to hydraulic or all-electric apparatus that are equipped, where necessary, with test fixtures
designed to limit inertial effects, as Section 1.03.5.3 will describe.
In basic set-ups, such as that shown in Figure 14, a clip-on extensometer is usually attached to the barrel of a dog bone–shaped
test specimen, whose dimensions are defined by the various standards. While this type of specimen geometry avoids excessive slip or
deformation in the grips, the use of an extensometer is preferred, because the cross-head displacement no longer provides an
accurate measure of the strain. Determination of the Young’s modulus may nevertheless be problematic where it is not possible to
identify an initially linear region of the stress–strain curve, in which case it may be defined as the tangent to the stress–strain curve at
zero strain. Care must also be taken to avoid artifacts linked to misalignment of the specimen during the early stages of loading,
particularly when the strain is measured from the cross-head displacement. A transverse extensometer is often used to calculate
Poisson’s ratio, n, from the ratio of the transverse to the axial strain, allowing a complete description of the low-strain elastic
response of isotropic specimens. However, while the assumption of uniform deformation of the gage length may be reasonable at
small deformations, plastic instabilities often occur in ductile specimens at large strains, resulting in localized necking, as Figure 15
shows (1,19). The local strains and strain rates associated with necking may be very different from the nominal values inferred from
the extensometer. Moreover, given that large strain deformations occur at an approximately constant volume in many plastics, there
is an accompanying decrease in specimen cross-sections. This implies that the ‘true’ stress at large strains differs substantially from
the nominal stresses calculated from the load and the initial specimen cross-section, Ao.
The tendency of ductile specimens to neck in simple tension may be partially attributed to the geometrical instability associated
with yielding; that is, with ductile materials whose true stress–strain curve flattens off at large strains, as sketched in Figure 15(b).
The true stress, st, is defined as the measured force F divided by A, the instantaneous cross-sectional area. For constant volume
deformation, lA remains constant, so that the nominal stress
F F st
s¼ ¼ ¼ [14]
Ao Að1 þ εÞ 1 þ ε
ds 1 dst st
¼ ' [15]
dε 1 þ ε dε ð1 þ εÞ2
Hence, given that dst/dε decreases strongly with increasing ε, there may be a critical value of s, given by eqns [14] and [15], beyond
which ds/dε is negative, so that s decreases with further increases in ε. This critical value of s and the corresponding value of ε may
be determined graphically using Considère’s construction, illustrated in Figure 15(b). Thus, any region in which s is locally high
(which may be due to slight nonuniformities in the specimen cross-sectional area) is able to deform at a lower nominal stress than
the rest of the specimen, and deformation will therefore localize to this region, which results in neck formation. Because most
Figure 15 (a) Nominal tensile stress–strain curves for a brittle polymer (PS) and a ductile polymer (HDPE), showing the different stages of ductile
neck formation; and (b) a schematic of the true stress–strain behavior of a ductile polymer, showing Considère’s criterion for the geometrical instability
leading to necking, that is, the point at which the tangent to the true stress–strain curve is equal to st/(1 þ ε).
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polymers also show intrinsic strain hardening, that is, dst/dε begins to increase again at ε well beyond the yield point
(Figure 15(b)), the neck will stabilize at some natural draw ratio characteristic of the polymer in question and propagate into the
rest of the specimen as deformation proceeds. As shown in Figure 15(a), such behavior is reflected by a decrease in nominal stress,
or yield drop at the onset of yielding, and strain hardening manifests itself in the nominal stress–strain curve only once the neck has
propagated throughout the gage length (the true stress–strain curve may also show an intrinsic yield drop associated with physical
aging effects in glassy polymers, which reinforce the tendency for neck formation (1)).
Because the local strain rate may be much higher in the neck than in the rest of the specimen, there has been a great deal of recent
interest in the use of video feedback techniques to obtain direct measurements of the true stress–strain curve at a constant strain rate,
as illustrated in Figure 16. By using an hourglass-shaped specimen so that the position of the initial neck is predetermined, the local
axial and transverse strains may be measured by using a video camera to follow fiducial marks on the specimen surface (52). These
may then be used to calculate the true stress locally. Moreover, the strain measurements may be used to control the cross-head speed
so as to maintain a uniform strain rate within the neck, which allows for direct measurement of the intrinsic behavior. While video
feedback control of this type generally requires a servohydraulic machine, passive video extensometry is also widely used with
screw-driven machines for many reasons. It is convenient and versatile, avoids damage to the specimen surface, and allows relatively
simple dilatometric measurements to be made in situ; for example, it can be used on specimens that show extensive internal
cavitation.
As with DMA, the same basic test apparatus may readily be adapted to other loading geometries, including shear (which will be
discussed in detail in Section 1.03.7 in the context of FRPs), bending, and compression testing. An important consideration for
large-strain bend tests is that in the three-point loading configuration (Figure 14(b)), the maximum bending moment occurs at the
midpoint of the beam – whereas in four-point loading (Figure 14(c)), the bending moment is uniformly distributed between the
loading points, since the imposed radius of curvature is constant. Hence, a greater volume of the beam is subjected to the maximum
bending moment in four-point bending, so the results obtained in this configuration may be considered to be more representative
of the majority of cases. However, it may also lead to reduced values for the flexural strength in brittle materials, because a larger
number of localized defects along the specimen length are subjected to close to the maximum stresses, and as with brittle tensile
specimens, failure will tend to occur at the weakest point of the specimen. In all bend configurations, including the cantilever test
(Figure 14(d)), calculation of the effective modulus depends on the fourth power of the specimen thickness, and as a result, it is
particularly important to work with well-characterized specimen geometries.
Compression testing, aimed at determining the modulus, compressive yield stress, or strength of bulk plastics, is normally
carried out on cylindrical or rectangular cross-section specimens, which are compressed uniaxially between smooth parallel plates.
The main practical concerns are misalignment and frictional resistance to lateral deformation at the specimen ends, which may lead
to inaccuracies in stress measurements and inhomogeneous deformation of the specimen in the form of ‘barreling’ (Figure 17(a)).
These latter effects may be reduced by use of a lubricant but are difficult to eliminate entirely at high strains. It is also recommended
to limit the aspect ratio of compression specimens in order to avoid buckling. Compression tests are often used to investigate the
yield behavior of plastics that do not yield in tension owing to crazing and/or brittle failure. However, in view of the aforemen-
tioned limitations of uniaxial compression tests at large strains, as well as the possibility of plastic instabilities and brittle failure,
such measurements are often carried out in plane strain compression using configurations such as those illustrated in Figure 17(b)
Figure 16 Schematic of a video feedback loop for the strain rate control of a tensile test. After G’sell, C.; Hiver, J. M.; Dahoun, A.; Souahi, A. Video-
Controlled Tensile Testing of Polymers and Metals beyond the Necking Point. J. Mater. Sci. 1992, 27, 5031.
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Figure 17 Various configurations for compression testing: (a) Uniaxial compression illustrating the problem of barreling; (b) conventional plane strain
compression test; and (c) plane strain compression using a channel die.
and 17(c), which have the advantage of a greater degree of constraint and a constant loading area, although again use of a lubricant
is important if accurate force measurements are to be obtained (19).
1.03.5.3 Rate-Dependent Testing

Because polymers are viscoelastic materials and because viscoelastic effects persist even in the solid state, as reflected by the existence
of sub-Tg transitions (Section 1.03.4.1), rate effects remain extremely important for the testing of solid polymers. Therefore,
numerical simulation may require data that correspond to a wide range of speeds and cover those associated with crash tests in the
automobile industry, for example. Moreover, particularly in tensile deformation, brittle failure and ductile yielding mechanisms
may coexist in a given polymer, and so are in competition. As the time and temperature dependence of the different mechanisms is
generally different, one or the other may predominate under different test conditions, leading to characteristic ductile-brittle
transitions (17–19). As a result, it is essential to carry out solid-polymer testing over a range of rates and temperatures. While it is
relatively straightforward to vary the test temperature (cf. Section 1.03.4.2), the scope for varying the test speeds is limited both by
the time available and by any technical restrictions. Thus, with a conventional screw-driven test machine, maximum cross-head
speeds are limited to around 100 mm min'1, whereas hydraulic apparatus permits an increase in speeds up to about 30 m s'1,
which corresponds to an effective strain rate of about 103 s'1 in a standard tensile test specimen.
Figure 18 shows a test configuration for high-rate tensile testing using a hydraulic machine. In this case, a pick-up unit permits
delayed contact between the specimen fixture and the cross-head, while the hydraulic piston accelerates to the final test speed.
When combined with ultralight specimen fixtures, this results in quasiinstantaneous acceleration of the specimen to the final test
speed (53). However, at speeds on the order of 1 m s'1, inertial effects begin to become important. Too abrupt an acceleration
may lead to significant stress oscillations, and in these cases, it is necessary to use a damped contact to ensure a smooth accel-
eration of the specimen fixture to the final test speed. While the test speed is ill defined at low strains, this approach enables the
determination of yield stresses and/or ultimate tensile strengths under quasistatic conditions up to 10–30 m s'1, as confirmed by
photo-elastic analyses (54). A number of ad hoc methods have been implemented to investigate deformation at still higher test
speeds, which correspond to effective strain rates of up to 106 s'1, including mechanical or explosive impact tests and gas gun or
explosively driven plate impact tests. Not only inertial forces but also adiabatic heating effects become important in these regimes
(so that elastic wave and shock wave propagation must be taken into consideration), so that it is no longer possible to assume
isothermal test conditions (55).
1.03.5.4 Creep and Dynamic Fatigue

Static creep and relaxation tests (Figures 13(b) and 13(c)) are widely used at low strains to characterize the long-term viscoelastic
response of plastics, but creep tests, in particular, are also of importance for investigating the phenomenology and mechanisms of
long-term failure under relatively high loads in applications such as pressure vessels or piping. Fatigue testing is used to assess the
progressive damage induced by cyclic deformation, as well as the practical implications of long-term dynamic loading (as in integral
hinges, shock absorbers, prostheses, and other items that undergo long-term dynamic loading). Creep testing at high loads is indeed
sometimes referred to as ‘static fatigue.’
Dynamic fatigue tests typically use hydraulic or all-electric machines, which are usually better adapted to applying cyclic loads
over long times than screw-driven machines, and also use essentially the same configurations as for tensile and flexural testing. The
principal experimental parameters are the stress or strain amplitude of the loading cycle and the test frequency. Polymers are
particularly sensitive to these factors, in view of their intrinsically time-dependent deformation behavior, and at large deformations
there may also be significant local heat generation during cyclic loading, which severely limits the range of frequencies over which
fatigue tests may be considered to be isothermal. Therefore, it is important to monitor the local specimen temperature using an
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Figure 18 High-speed tensile testing using a damped pick-up unit. After Béguelin, P. Approche expérimentale du comportement mécanique des
polyméres en sollicitation rapide. Ph.D. Thesis No. 1572, Ecole Polytechnique Fédérale de Lausanne, 1996.
infrared camera, for example, particularly since thermal fatigue failure is also of considerable practical relevance to these types of
tests. In engineering design, fatigue tests on unnotched, defect-free specimens correspond to the ‘total-life’ approach, in which
fatigue failure is a consequence of both crack nucleation and subsequent growth. The number of cycles to failure of an unnotched
bulk specimen, N, is a function of the mean applied load, which may include a static component, as well as other extrinsic test
parameters such as temperature, the surface quality of the specimen, the presence of internal flaws, and others. Results are then
presented in the form of an ‘S–N’ curve, which gives the applied cyclic load or nominal stress as a function of N (51). However, it is
also common practice to subject notched specimens to fatigue testing, in which crack growth may be analyzed using fracture
mechanics, as Section 1.03.6 will discuss further.
A common problem to both creep testing and dynamic fatigue up to failure is that measurements may take a long time. Given
that static testing is relatively simple to implement, it is generally carried out using ad hoc test set-ups in which a creep oven is
equipped with a system for suspending dead weights on tensile test specimens and multichannel data acquisition systems, which
enables long-term testing to be performed on multiple specimens. However, even in cases when dedicated apparatus is available for
both static and dynamic fatigue tests, one is often interested in accelerating the test in order to provide predictions of service
lifetimes in components that are designed to last for decades or more, based on shorter laboratory tests. One way of doing this is to
extrapolate data obtained at different elevated temperatures, during which lifetimes tend to be reduced, although this may not be
a reliable testing method for materials that show changes in deformation mechanisms in different temperature regimes, and the
existence of temperature-induced ductile-brittle transitions may render such procedures highly misleading (56). Similarly, changes
in load may lead to markedly different regimes of behavior. For example, low load, high cycle fatigue, or long-term creep loading
may favor the propagation of subcritical defects, leading ultimately to catastrophic brittle failure when these reach some critical
size – whereas high loads may induce ductile yielding, followed by ductile failure, as illustrated by the results in Figure 19 (57).
(In these particular tests, the failure time was shorter at 10 MPa than at 15 MPa, due to the onset of brittle failure.)
1.03.6 Fracture and Impact Testing
The use of simple tensile and compressive testing and static and dynamic fatigue tests combined with bulk specimens generally
implies a ‘strength-of-materials’ approach to design, in which one seeks to avoid notches and other stress-concentrating features, so
that the properties of a given structure reflect the cohesive strength of its components. However, there has also been considerable
interest in developing a fracture mechanics approach to polymer testing, in order to explicitly account for the role of flaws or other
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Figure 19 Strain–time curves for specimens of polyoxymethylene (POM) subjected to different nominal stresses in tension at 100 * C. After
Scaramuzzino, P. Analyse de la structure et de l’endommagement mécanique du polyoxyméthylène. Ph.D. Thesis No. 1818, Ecole Polytechnique Fédérale
de Lausanne, 1998.
geometrically induced stress concentrations on ultimate specimen failure (16,17). To accomplish this goal, a precrack is deliberately
induced into the specimen in fracture testing and the load displacement behavior of the specimen up to failure is analyzed in terms
of the effective crack resistance of the specimen under a static strain rate, a constant strain rate, or cyclic loading. In impact testing, on
the other hand, specimens may be either precracked or unnotched, with the goal of providing a simple means of simulating impact
loading, as well as to extract an impact energy for comparative purposes. However, for more controlled assessment of fracture
behavior at impact speeds, it is also possible to adapt the high-speed tensile test methods as described in Section 1.03.5.3 to fracture
mechanics testing (54).
1.03.6.1 Impact Tests

In standard pendulum impact tests (Figure 20(a)), a weighted pendulum arm is held at a given height, which determines its
potential energy. On release, the arm impacts and breaks the specimen, then returns to a maximum height, whose difference with
the release height gives the impact energy of the specimen. The Izod impact test differs from the Charpy impact test in that the
specimen, which may be notched or unnotched, is held in a cantilevered beam configuration rather than a three-point bending
configuration, as shown in Figures 20(b) and 20(c). Such tests are now often instrumented with load transducers fixed to the
impacter, permitting load displacement curves to be measured, as well as measuring fracture mechanics analysis (see Section
1.03.6.2) of the impact failure of notched specimens. Impact testing provides a rapid assessment of the behavior of a given material
and may also be used to determine temperature regimes in which the impact response is predominantly ductile or predominantly
brittle. On the other hand, the range of effective test speeds is limited (2–3 m s'1 for Charpy and Izod tests), and even when the
criteria for valid fracture mechanics testing are met (Section 1.03.6.2), it is relatively difficult to extract intrinsic fracture parameters
from experimental force–displacement curves, because of dynamic and inertial effects (Section 1.03.5.3). Additionally, basic impact
tests usually do not provide data that can be directly used in component design.
A common variant is the falling-weight impact test in which a projectile, which may also be instrumented, is dropped from
a fixed height onto the specimen, which is typically a plastic or composite plaque (Figure 20(c)). In this case, the effective test speeds
are typically between 1 and 4 m s'1, and for materials with very high fracture energies, such as certain composites, it is also possible
Figure 20 (a) Schematic of an impact pendulum along with (b) Izod; (c) Charpy; and (d) falling-weight impact test geometries.
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to use a catapult device to further accelerate the projectile. Section 1.03.5.3 briefly referred to techniques for investigating the impact
response at still higher speeds.
1.03.6.2 Linear Elastic Fracture Mechanics Testing

In static fracture testing, a precrack is introduced into a specimen with a well-defined geometry, and a constant displacement rate is
typically applied to well-defined loading points using a tensile test apparatus. The macroscopic fracture stress, sf, of the cracked
specimen is then given by an expression of the form
" #1=2
EG
sf a1=2 ¼ [16]
p
where a is the crack length, E is the tensile modulus, and G is an energy for unit area extension of crack, which includes both surface
energy terms and terms linked to energy dissipation during the fracture process. In a linear elastic specimen, crack extension occurs
when the strain energy release rate per unit area crack extension, G, exceeds G. As long as plasticity is confined to a relatively small
crack tip deformation zone, G may be shown to be dominated by elastic contribution of the surrounding material, which justifies
the assumption of linear elasticity, even in the presence of small-scale crack tip yielding, given appropriate corrections to the
effective crack length. The stresses, sij, around the crack tip are obtained from
K
sij ¼ pffiffiffiffiffiffiffiffi fij ðqÞ [17]
2pr
where r and q are cylindrical polar coordinates in the plane perpendicular to the crack plane, with r ¼ 0 at the crack tip and q ¼ 0
corresponding to the crack direction, and K is a stress intensity factor that depends on the crack length, a; the applied stress, s; and
the specimen geometry. Thus, in mode I opening, when a load is applied in the direction perpendicular to the crack plane
(Figure 21),
pffiffiffiffiffiffi
KI ¼ Ys pa [18]
where Y depends on the specimen geometry. It may also be shown that
8 2
> KI
>
<
E
G ¼ GI ¼ [19]
>
> ð1 ' n2 ÞKI2
:
E
in plane stress and plane strain, respectively (in plane strain, strains in the z direction are considered negligible, whereas in plane
stress, stresses in the z direction are considered negligible) (58). Similar expressions may be derived for the other modes of crack
opening, II and III, as shown in Figure 21.
It follows that the intrinsic crack resistance of a linear elastic specimen may be expressed in terms of a critical value of either G or
K, denoted GIc or KIc, respectively, in mode I testing in plane strain. These correspond to the onset of unstable crack propagation in
a brittle material. The mode I opening is most the widely used crack-opening mode, because it is straightforward to implement in
a variety of specimen geometries (Figure 22), which may be prepared by the machining of injection- or compression-molded
plaques, for example, and because it is generally the most critical for performance. However, the other crack-opening modes may
also be important, particularly in the case of composites, as will be discussed further in Section 1.03.7.
In practice, the plane strain condition is strictly satisfied only for infinitely thick specimens but remains a reasonable
approximation for the range of thicknesses defined by standard test protocols. In general, the minimum specimen thicknesses
and crack lengths for valid linear elastic fracture mechanics testing are proportional to (KIc/sy)2, where sy is the tensile yield stress,
which is a measure of the size of the plastic zone at the crack tip. While in principle, it should be possible to meet these conditions
for any material by increasing the specimen thickness, a maximum specimen thickness of around 1 cm is usually imposed by
processing requirements, so many tough, ductile polymers are not suited to linear elastic fracture mechanics testing. It is possible
to use eqn [18] to define a critical value of G or K from the fracture stress from a nonvalid test, and such values may remain useful
Figure 21 The different crack-opening modes.
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Figure 22 Typical specimen geometries for mode I fracture toughness testing of plastics: (a) Compact tension (CT); (b) single-edge-notched tension
(SENT); (c) single-edge-notched bending (SENB); (d) double cantilever beam (DCB); and (e) tapered double cantilever beam (TDCB) (for crack
propagation measurements at constant K).
indications of crack resistance as a function of external variables such as temperature, rate, or materials parameters. However,
results obtained in this way will depend on the relative extent of plane strain and plane stress conditions through the specimen
thickness (and hence on specimen thickness) and can no longer be considered an intrinsic measure of fracture toughness
(16,17,58).
Another important condition for valid fracture testing in plastics is that the precrack must be sharp. Precracking in plastic
specimens is typically carried out by passing a razor blade across the tip of a machined notch, but this must be done carefully, due to
the propensity of polymers to undergo ductile yielding and the need to avoid introducing residual stresses into the crack tip region
(16,17,58). Fatigue precracking, which is widely used for metals, is less appropriate to many types of plastics due to difficulties with
crack tip plasticity.
1.03.6.3 Elastic–Plastic Fracture Mechanics Testing

Linear elastic fracture mechanics are applicable to a wide range of relatively brittle plastics, including highly cross-linked glassy
thermosets and thermoplastics that tend to craze readily, such as PS. However, standard fracture specimens of many engineering
plastics and toughened plastics show highly nonlinear stress–displacement curves, due to excessive crack tip plasticity (and they
may fail by ductile tearing rather than unstable crack propagation). As a result, there has been a great effort to implement theories of
crack growth that explicitly account for plastic deformation and provide protocols for fracture testing of ductile specimens that do
not meet the conditions for linear elastic fracture mechanics described in Section 1.03.6.2. These are known collectively as elastic–
plastic fracture mechanics, and their application to plastics is summarized briefly in this section.
The crack-opening displacement (COD) approach derives from the observation of a correlation between toughness and COD in
structural steels that are too tough for linear fracture mechanics testing to be applicable. Analysis of COD in terms of cohesive zone
models for mode I opening (some of which are particularly appropriate to damage zone shapes in many polymers) shows that the
crack tip opening displacement d is given by GI/sy in the small-scale yielding limit. Therefore, it was suggested that d may provide
a more general measure of toughness where elastic fracture mechanics is no longer appropriate. In practice, COD may be measured
directly either optically or by use of a clip gage in the crack tip, allowing the definition of a critical value of d corresponding to crack
extension. In polymer fracture testing, however, COD testing has been largely replaced by J-integral-based testing (58,59). The
J-integral derives from the extension of linear fracture mechanics to the case of a nonlinear elastic material, and has been widely used
to describe fracture that involves a relatively large plastic zone at the crack tip, based on the assumption that during loading of
a fracture specimen, the stress increases monotonically everywhere in the specimen up to crack extension (so that there is no
unloading). The elastic–plastic failure parameter is termed JIc, the nonlinear equivalent to GIc, which it reduces in the linear limit.
However, unlike G, there is no longer a linear relationship between J and the applied load and the specimen geometry and crack
length, and J can no longer be considered to be equal to the strain energy released as the crack advances, but rather a difference in
energy is absorbed by the specimen for different crack lengths. (One can also show that d ¼ J/sy, which validates the COD approach
in nonlinear specimens (58).)
One approach to J testing is to obtain load displacement curves up to loads sufficient to cause different amounts of stable crack
extension in CT or SENB-type specimens (see Figure 22), as measured for example by postmortem inspection of freeze fracture
surfaces. It is then possible to use these to plot U(a) at fixed specimen displacement, d, from which
" #
1 vU
J¼' [20]
B va d
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100
0.2 mm Offset line 0.1 (W–a o ) Exclusion line
y (Blunting line)
80
J kJ m–2
60
40
Power law fit. J = β aY
= 0.83
20
7.75 8.16
5.59
0
0 1 2 3 4 5 6
a + rp (mm)
Figure 23 Procedure for determining JIc from experimental data for mode for J as a function of crack extension in a CT specimen of POM. After
Scaramuzzino, P. Analyse de la structure et de l’endommagement mécanique du polyoxyméthylène. Ph.D. Thesis No. 1818, Ecole Polytechnique Fédérale
de Lausanne, 1998.
where U is taken from the area under the load displacement curve, and B is the specimen width. Finally, one obtains J as a function
of crack extension, Da, which is referred to as the ‘R curve,’ as illustrated in Figure 23. A standard procedure for obtaining a critical
value of J for the onset of crack propagation, that is, JIc, is to define a crack-blunting line
J ¼ 2sy Da [21]
which accounts for apparent crack extension during ductile crack tip blunting on initial loading. JIc is then defined as the intercept
between the blunting line and J(Da) measured at relatively large crack extensions. However, many experimental R curves do not
show a clearly defined transition between a blunting and true crack extension, in which case JIc is defined according to a blunting
line with a fixed offset in Da (usually 0.2 mm), as illustrated in Figure 23 (59).
Such procedures are cumbersome and not necessarily straightforward to implement, as crack length measurements may not
always provide a clear distinction between the crack tip and the crack tip damage zone. Crack bowing may also be a problem, due to
through-thickness variations in stress state, although side grooving can help alleviate this to some extent. However, it is also possible
to determine J from a single specimen if the possibility exists to measure the amount of crack extension in situ. This may be done by
the elastic unloading compliance method or by direct measurements of the crack position by video, for example. The ‘R curve’ itself,
which represents an energy dissipation rate as a function of crack extension, may be taken to represent a qualitative measure of the
resistance to stable crack growth in ductile specimens, but its exact interpretation is often difficult, because it is influenced by both
the intrinsic properties of the specimen and the specific specimen geometry (58,59).
As with KIc and GIc testing, valid JIc testing remains subject to geometrical restrictions, so that alternative approaches are still
required for highly ductile materials and/or specimens that are available only with reduced thicknesses (e.g., films). A popular recent
approach for plastics is the ‘essential work of fracture’ (EWF) test, illustrated in Figure 24, which is often based on double-edge-
notched tensile (DENT) geometry. EWF testing is based on the assumption that in sufficiently ductile DENT specimens, the ligament
of width L separating the notch tips will undergo full yielding prior to crack advance, giving rise to a plastic zone whose dimensions
Figure 24 The principle of essential work of fracture (EWF) testing: (a) DENT specimen showing the plastic zone and fracture zone; and (b) stress–strain
curves at different L used to extrapolate to zero to obtain we.
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scale as L2. The work necessary to create the fracture surfaces of a crack propagating across the ligament scales is given as L. Thus, the
overall fracture energy, Wf, depends on L, according to
Wf ¼ We þ Wp ¼ we tL þ wp tL2 [22]
where t is the specimen thickness and we and wp are the essential work of fracture and the plastic work, respectively. By carrying out
multiple tensile tests with different values of L and by extrapolating Wf/Lt to L ¼ 0, one obtains a measure of we, which may be
considered a materials parameter for a given value of t, and has been formally linked to Jc, although it is important to demonstrate
full section yielding and similarity in the force–displacement curves for the range of L used in the extrapolation (60).
1.03.6.4 Time-Dependent Crack Propagation

The basic fracture mechanics approaches described so far were originally developed for metals, and although they are widely applied
to plastics, they do not explicitly account for the viscoelastic nature of polymers and, consequently, the rate effects on crack
propagation (17,58). As a result, G and J are assumed to be independent of time at fixed displacement, which is clearly inconsistent
with the observation of significant stress relaxation, even in glassy polymers, and crack tip microdeformation may also be highly rate
dependent. This has led to attempts to include rate effects in fracture mechanics-based models for crack growth (61) and also to
systematic investigations of ‘slow crack growth’ as a function of time in precracked specimens that are subjected to low-level static
loading (56,62). Slow crack growth tests are of considerable practical importance for pressurized plastic piping, for example, where
subcritical defects induced by faulty installation may grow to a critical size over long periods of time. These defects result in
unexpected, catastrophic failure that involves unstable cracks that may in some cases propagate over hundreds of meters. Conse-
quently, a great deal of research in this area has focused on polymers that are widely used in such applications, such as HDPE (62).
As with unnotched tensile creep tests (see Section 1.03.5.4), there has been an effort to develop protocols for accelerated testing in
order to predict long-term behavior from relatively short-term tests, involving both elevated temperatures and the use of ten-
sioactive fluid environments in order to favor brittle failure mechanisms over ductile yielding (see Section 1.03.8). Figure 25 shows
results from a slow crack growth test on POM in air at 100 * C, in which the COD has been monitored as a function of time in
a compact tension specimen subjected to a constant load, and hence a constant nominal K (57). This illustrates the development of
a localized crazelike fibrillar damage zone at the crack tip over an extended period of time, during which the COD changes relatively
little, followed by a sharp acceleration in crack growth through the damage zone, which leads to catastrophic failure. Such tests are
crucial for establishing reliable design limits in the construction industry, where service lifetimes are typically measured in decades.
1.03.6.5 Fatigue Crack Propagation

Crack propagation in dynamic fatigue is important for quantifying slow subcritical crack growth under cyclic loading conditions,
which, as with static slow crack growth, may culminate in catastrophic failure after relatively long periods of low-level loading (51).
Fatigue crack growth tests characterize the rate at which a preexisting crack propagates as a function of the cyclic loading conditions,
namely, the range of applied stress intensity. The crack length is monitored either directly or indirectly through compliance
Figure 25 A slow crack growth measurement using a notched compact tension specimen of polyoxymethylene loaded at constant nominal K, showing
the COD as a function of time. After Scaramuzzino, P. Analyse de la structure et de l’endommagement mécanique du polyoxyméthylène. Ph.D.
Thesis No. 1818, Ecole Polytechnique Fédérale de Lausanne, 1998.
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Figure 26 da/dN as a function of DK in different grades of POM tested at 10 Hz with R ¼ 0.1. After Scaramuzzino, P. Analyse de la structure et de
l’endommagement mécanique du polyoxyméthylène. Ph.D. Thesis No. 1818, Ecole Polytechnique Fédérale de Lausanne, 1998.
measurements or resistance measurements. Such tests are often conducted in thermal and chemical environments that are repre-
sentative of those encountered in service. The resulting data may be used as a basis for lifetime predictions or to define inspection
intervals. Many materials show the following dependence over wide ranges of DK, the difference in the maximum and minimum
values of K during the cycle (20,51):
da
¼ CDK m [23]
dN
where N is the number of cycles and m is a constant. Figure 26 shows results for different grades of POM tested at room temperature
and at 10 Hz, with the ratio of the minimum to the maximum stress, R ¼ 0.1, illustrating the validity of eqn [23] (57).
1.03.6.6 Test Methods for Elastomers

Elastomers (lightly cross-linked flexible polymers deformed in the rubbery regime above Tg) typically show large quasireversible
elastic deformations at relatively low stresses. While hyperelasticity is the defining characteristic of these materials, in practice it is
also important to determine the material’s ultimate properties, such as the tensile strength or crack resistance, as well as hysteresis
during cyclic deformation and hardness (the resistance to indentation without permanent damage, which is directly related to the
elastic modulus). Analysis of fracture is nevertheless difficult with the standard geometries used for rigid polymers, because the
fracture mechanics approaches described in this chapter are inapplicable to these types of materials. Various ad hoc tests based on
the test geometries shown in Figure 27 have therefore been devised for elastomers with the aim of determining a tearing energy that
may be considered to be independent of the specimen geometry and hence a materials parameter (1,63). For this purpose, it is
necessary to calculate the rate of elastic energy, E, per unit increase in the crack area, A, at a fixed specimen displacement. This is given
by (vE/vA)d ¼ F/h for the so-called trouser test geometry (Figure 27(a)), where F is the applied force and h is the specimen thickness.
In this case, the elastic energy may then be equated to the tearing energy, which corresponds to energy dissipated in viscoelastic
processes occurring in the vicinity of the crack tip, and is consequently strongly rate and temperature dependent. In certain cases, it is
possible to use the WLF approach (Section 1.03.4.2) to describe the tearing behavior of simple rubbers over a wide range of test
conditions (1).
Figure 27 Different geometries used for the fracture testing of rubbers: (a) Trouser test; and (b) constrained tension specimen.
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1.03.7 Fiber-Reinforced Polymer Composites (FRPs)
FRPs are generally made up of a polymer matrix reinforced with relatively high-strength, rigid fibers (6,8,64,65). The fibers are
typically glass, carbon, or aramid (Kevlar"), although natural fibers such as hemp and flax are increasing in popularity, and metallic
reinforcements may be preferred in certain applications. The polymer matrix is usually an epoxy, vinylester, or polyester thermoset.
However, a wide range of FRPs are also based on thermoplastic matrices, such as PP, polyamide 6 (PA6), PET, or PEEK, which may
offer improved toughness and fatigue resistance, reduced cycle times in forming operations, and some degree of recyclability.
Structural FRPs that contain continuous fibers in a high-performance matrix will provide the focus for this section. In the case of
short fiber-reinforced and particle-filled plastics, processing and testing are similar to those for unfilled resins and will not be
considered separately here.
Continuous fibers may be introduced into structural FRPs either as woven textiles or in the fully aligned, unidirectional (UD)
state (Figure 28(a)). In this latter case, a composite part will typically be built up by laminating several layers of UD preimpregnated
(‘prepreg’) plies with different fiber orientations, which contain either an uncured or partly cured thermoset resin or a thermoplastic.
Consolidation and final curing then occur under pressure (and, if necessary, at elevated temperatures) as part of the final forming
operation (64). The resulting structures are highly anisotropic, and there is a considerable emphasis in composites testing on
multiaxial loading conditions, as well as on specific deformation and failure modes that do not have equivalents in isotropic
materials, such as those of interlaminate failure or intralaminate shear along the fiber direction. Ad hoc methods have also been
developed for testing the fiber–matrix interface, which is crucial for structural performance, as failure of the fiber–matrix interface
(pull-out) often determines the ultimate properties of structural FRPs. While this chapter is not concerned with structures per se,
reference will be made here to sandwich structures, in which laminate sheets are bonded to both sides of a honeycomb core
(Figure 28(b)), which may be fabricated from either polymeric or metallic materials (e.g., aluminum), and whose performance is
often limited by the quality of the interface between the laminate and the core, as well as the properties of the latter. Sandwich
structures not only are of considerable practical importance in their own right, but also are the basis for certain types of shear tests on
FRP laminates, as will be seen in Section 1.03.7.3.
1.03.7.1 Mechanics of Composite Materials

The elastic properties and strength of FRPs depend strongly on those of the fibers, and at high fiber volume fractions, the polymer
matrix does essentially play the role of an adhesive. Even so, the matrix properties remain critical for the response to mechanical
solicitations in directions perpendicular to the fiber trajectories, and may also be determinant for damping, environmental resis-
tance, surface properties, and other material properties.
In an ideal continuous UD FRP, the stiffness in the fiber direction is given by a simple mixing law, so that the composite modulus
E1 ¼ Ef ff þ Em ð1 ' ff Þ [24]
where Ef is the fiber modulus, Em is the matrix modulus, and ff is the fiber volume fraction. On the other hand, in the direction
perpendicular to the fiber direction,
Ef Em
E2 ¼ [25]
Em ff þ Ef ð1 ' ff Þ
where Em is typically of the order of a few GPa, whereas Ef is about 70 GPa for glass fiber (E-glass fiber) and may be up to more than
400 GPa in certain high-modulus grades of carbon fiber. Thus, a 60% UD carbon fiber–epoxy composite may have a modulus of
200 GPa in the fiber direction, but only around 10 GPa perpendicular to the fiber direction, and similar levels of anisotropy are seen
in the ultimate tensile strength and many other mechanical and physical properties. As a result, while two independent elastic
constants (e.g., E and n from a tensile test) are sufficient to describe the linear elastic response of an isotropic plastic part,
a transversely isotropic UD FRP requires five independent elastic constants, and in generally anisotropic composite materials up to
Figure 28 Composite morphologies: (a) UD FRP viewed perpendicular to the fiber orientation direction; and (b) sandwich structure with
a honeycomb core.
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21 elastic constants may need to be determined, depending on the degree of symmetry. Basic laminate theory nevertheless allows for
relatively straightforward calculation of the elastic response of a laminate from the properties of the individual UD plies, and similar
approaches may be used to model viscoelastic and ultimate properties (6,65). Even so, basic mechanical testing of composites is
time-consuming and often difficult, which has given rise to a relatively wide range of test procedures that are often specifically
designed for a flat rectangular coupon, which is usually the most convenient geometry for laminates. Test procedures may also be
adapted to other geometries, such as cylindrical shells, depending on the specific composite processing route involved (66).
1.03.7.2 Mechanical Testing of Composites

1.03.7.2.1 Tensile Tests
Tensile testing with standard rectangular coupons avoids difficulties that can arise from the machining of more complex geometries
from composite plaques (it may be necessary to polish any machined surfaces in order to eliminate flaws, even for simple
geometries). However, particularly in the case of UD composites tested in the fiber direction, the high strengths of such coupons
lead to difficulties in adequately gripping the specimens. Too high a clamping force may cause local damage and create excessive
stress concentrations, so that the specimen tends to break in the grips, and reducing the specimen thickness may result in specimens
that are no longer representative of the bulk composite. A common solution to this problem is to use tabs at the specimen ends (e.g.,
made of aluminum) in order to cushion the grip forces, as Figure 29 shows.
1.03.7.2.2 Compression Tests

Compression testing is essential, insofar as the compressive strength of an FRP may be very different from its tensile strength.
A major difficulty is that the use of flat, straight-sided coupons, while convenient from a practical point of view, may require
a reduced gage length if buckling is to be avoided in uniaxial compression, depending on the nature of the specimen. On the other
hand, if the gage length is too short, the grips will significantly influence the results. Various test protocols have been proposed based
on shear loading and end loading, as well as alternatives, such as the use of a planar specimen glued to the compressive surface of
a sandwich beam deformed in bending. An increasingly popular approach is the combined loading compression (CLC) test method
(Figure 30), which is based on a relatively small and easy-to-use test fixture that is suitable for both tabbed and untabbed straight
sided-specimens, and in which the specimen is both end loaded and loaded in shear, while the shear loading limiting crushing of
the specimen ends by the end plates.
1.03.7.2.3 Flexural Tests

Some of the problems associated with uniaxial tension and compression of composite coupons may be avoided through the use of
flexural loading, that is, three- or four-point bend testing (cf. Figure 14). Flexural loading of high-aspect-ratio beams may also be
close to the loading conditions that the material will experience in service. On the other hand, where this is not the case, the
convenience of bend testing is offset by the relatively complex loading conditions and consequent difficulties in interpretation,
particularly when quantitative data are required for design purposes.
1.03.7.2.4 Shear Tests

A number of shear test methods are in widespread use for composite specimens. These are often aimed specifically at characterizing
intralamellar shear stiffness and failure, although rigorous characterization may require determination of several independent shear
moduli and strengths. Some of the most common types of shear test are briefly described in this subsection, along with their
advantages and disadvantages from a practical point of view (67).
Iosipescu and V-notched rail shear tests. In each of these cases, a double V-notched rectangular specimen is loaded in shear by
compressive loading of the test fixture. The two types of test differ essentially in the way the specimen is loaded: in the Iosipescu test,
originally developed for metals, the load is applied to the sides of the specimen, as shown in Figure 31 – whereas in the rail shear
test, the load is introduced through the specimen faces (by clamping or adhesive bonding), allowing the testing of relatively thin
laminates. These types of tests have become relatively popular because of their versatility and the fact that they result in a relatively
Figure 29 Schematic of the preparation of tabbed specimens from UD FRP and laminate sheets.
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Figure 30 Combined loading compression (CLC) test method.
pure state of shear stress in the ligament that separates the notch tips, so they provide reliable quantitative data for many types of
material, including unreinforced plastics. A variety of other types of rail tests are also frequently used with unnotched specimens, but
result in a less well-defined shear state than in double V-notched specimens.
Short-beam shear test. A ‘short beam’ is tested in bending (usually three-point bending). Because the beam is short, shear stresses
are relatively large, as compared with the flexural stresses (tension and compression). Although the specimen is not in pure shear
and the deformation is inhomogeneous (and too low a specimen aspect ratio may result in crushing rather than shear deformation),
this test has the advantage of simplicity, and is excellent for screening specimens in cases where quantitative data are not required.
) 45* and 10* off-axis tensile shear test. These tests are essentially uniaxial tensile tests and do not require additional test fixtures, as
they use a simple straight-sided specimen from a ) 45* laminate or a UD specimen with the fiber direction offset by 10* with respect
to the specimen axis, as shown in Figure 32. In the case of the ) 45* tensile test, it is assumed that a stress state close to pure shear is
obtained along the fiber direction and that the corresponding shear strength is relatively low, so that it determines the overall tensile
Figure 31 Iosipescu shear test.
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Figure 32 ) 45* and 10* off-axis tensile shear tests.
strength (the local shear strain at small deformations may be measured using strain gages). However, the stress state in the specimen
is complex in nonideal laminates, making it unreliable as a quantitative test. For UD specimens, any fiber offset angle may in
principle be used to investigate the effects of shear along the fiber axis, although, again, stress states are relatively complex. Despite
these shortcomings, the 10* offset test has become standardized, because it minimizes the effects of biaxial stresses on the overall
response.
Staggered double-notched shear test. This test makes use of straight-sided specimens with staggered notches on opposing surfaces, as
shown in Figure 33 (there are many possible variations). Either a tensile or a compressive axial load is applied to lead to shear
stresses in the resulting ligament. The main merit of this test is once more its ease of implementation, making it attractive for
screening. However, it is unsuitable for quantitative measurements, and the concentrations of stresses at the notch tips may lead to
failure at global stress levels that are well below the intrinsic shear strength of the specimen.
Thin-walled tube torsion test. As the name suggests, a thin-walled tube is tested in torsion. This is convenient for many composite-
manufacturing processes of tubular structures, such as filament winding, and for thin walls, this test leads to relatively homogeneous
shear away from the specimen ends, although gripping requires special test fixtures. Note that the test is clearly unsuitable for other
geometries.
Cross-beam sandwich shear test. The cross-beam sandwich shear stress test makes use of the relatively elaborate specimen geometry
shown in Figure 34(a). The cross-beam sandwich, whose core may form part of the specimen (or simply provide a means of
stabilizing deformation in the individual laminates), is loaded simultaneously in positive and negative bending to produce a biaxial
state of tension and compression at the center of the specimen. The stresses in the 45* planes of the test section are assumed to be
pure shear stresses, although in practice, the stress state may be considerably more complex.
Picture frame shear test. The picture frame shear test specimen consists of two square laminates bonded to a honeycomb core.
A rigid 4-bar frame is fixed over the sandwich structure, as shown in Figure 34(b), and the load is introduced by tensile and/or
compression of opposite corners of the frame to produce shear loading at 45* to the diagonals. As a general method for testing
laminates, this method suffers both from the need for a relatively complex test fixture and, yet again, from a nonuniform stress state.
1.03.7.3 Fracture Testing of Composites

Considerable effort has been undertaken to extend fracture mechanics concepts to the study of composites, but the situation is
considerably complicated by the tendency for damage to take the form of delocalized microcracks and other damage events peculiar
to FRPs, such as fiber debonding and bridging, rather than the propagation of single well-defined cracks, as in a homogeneous
isotropic plastic (58). Such behavior might be considered advantageous from a practical point of view, because FRPs seldom fail
catastrophically without the prior accumulation of detectable subcritical damage (cf. Section 1.03.7.5), but this type of behavior
Figure 33 Staggered double-notched shear test.
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Figure 34 (a) Cross-beam sandwich shear test; and (b) picture frame shear test.
also implies that fracture mechanics concepts are relevant only in certain well-defined situations. Therefore, a great deal of routine
testing tends to make use of impact tests, such as the drop weight impact test described in Section 1.03.6.1. Moreover, although there
have been attempts to adapt fracture mechanics to the study of the general effect of sharp notches and other stress concentrators on
composite panels, these are of limited practical interest, given that such features should be absent from well-designed load-bearing
elements (58).
One situation to which fracture mechanics is often applied, however, is that of delamination failure between adjacent plies in an
FRP laminate, for which self-similar growth of a dominant crack is generally a valid assumption (58,66,67). As with plastics, mode I
loading is widely used for delamination testing, and the double cantilever beam (DCB) test, shown in Figure 35(a), is particularly
convenient for this purpose. A specimen containing a delamination precrack is prepared by insertion of a thin film of nonadhesive
material, the choice of which depends on processing requirements. Hinges or blocks are fastened or glued to the specimen ends, and
the delamination crack length is monitored as the specimen arms are displaced at a constant rate, allowing the calculation of GIc for
interlaminar failure. In practice, while the conditions for LEFM are generally satisfied, crack propagation is usually stable, in which
case GIc is often found to vary significantly with crack length (66).
The mode II delamination fracture toughness is also widely investigated. In this case, a common approach is to use a specimen
containing a precrack prepared in the same way as for mode I testing and load it in three-point bending, as shown in Figure 35(b).
The shear stress at the midplane of the specimen then initiates mode II sliding failure at the tip of the precrack as the displacement is
increased. This method is commonly referred to as an end-notched flexure (ENF) test, is relatively simple to implement, and
produces pure mode II failure. Measurement of the mode III delamination fracture toughness is somewhat more challenging, due to
Figure 35 Test geometries for the fracture testing of composites.
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the difficulty of obtaining pure mode III loading at the crack tip. Figure 35(c) shows one possible test geometry – the split cantilever
beam test – although in this basic configuration, a substantial component of mode II loading persists at the crack edges.
In practice, interlamellar failure in structural applications of FRPs may involve a combination of fracture modes. As a result, there
has been a particular emphasis on mixed-mode delamination tests. The mixed-mode bending (MMB) test fixture shown in
Figure 35(d) is among the most straightforward of these. The fixture simultaneously applies a direct combination of mode I (DCB)
and mode II (ENF) loadings. One end of a precracked specimen is supported by a cylindrical bearing that allows lateral movement
of the specimen. The other end, containing the precrack, is clamped to both the base plate and a loading beam designed to introduce
various ratios of mode I to mode II loading according to the position of the central pivot. A major limitation of many such test
methods, however, remains the difficulty of determining the relative extents of mode I and mode II fracture present for a given
specimen configuration (66).
1.03.7.4 Single-Fiber Debonding

The fiber–matrix interface is of fundamental importance for FRP properties, and as a result, there has been an effort to develop tests
that provide direct insight into fiber matrix debonding. A common approach is to embed a single fiber along the axis of a tensile
specimen of the matrix material. The matrix must be sufficiently ductile to absorb the energy released when the fiber fails locally
under the applied tensile load. As the load increases toward the global ultimate tensile stress, further fiber failure occurs. These fiber
failure events and debonding along the fiber–matrix interface may readily be observed by optical microscopy, assuming a trans-
parent or translucid matrix (Figure 36(a)). Analysis of such fragmentation tests is based on the assumption that the fiber will
continue to break up into shorter lengths until shear at the fiber–matrix interface becomes insufficient for the axial stress in the fiber
to exceed its failure stress. The resulting ‘critical length’ may then be used to calculate the interfacial shear strength, assuming the
fiber-breaking strength is known from previous independent tests on single fibers (68).
Another commonly used test method is to apply a compressive load to the end of a single fiber embedded in a section taken from
a bulk FRP perpendicular to the local fiber direction. Shear between the compressed fiber and the rest of the composite may be
sufficient to cause the fiber to debond from the matrix, allowing the calculation of the interfacial strength. In a variant of this
method – the single-fiber push-out test – short lengths of fiber are pushed through a thin section that is taken perpendicular to the
fiber direction. It is also possible to pull a fiber out of the surrounding material (Figure 36(b)), provided that the fiber does not fail
before debonding takes place, but this method again requires the use of thin sections. The practical difficulties with obtaining
sufficiently thin sections (which may need to be as little as a few 100 mm in thickness) have led to the development of the bead pull-
off test, in which a bead (drop) of matrix material is placed on an individual fiber and cured if necessary (Figure 36(c)). The bead is
restrained and a tensile force applied to the fiber. The force at which the bead–fiber interface fails may then be used to calculate the
interfacial shear strength (69).
1.03.7.5 Nondestructive Testing

Nondestructive testing (NDT) of FRPs is typically used to detect subcritical defects, such as local delamination caused by low-level
impacts that are not visible from the exterior and that may lead to long-term failure through slow crack growth (in contrast with
aluminum, say, for which the immediate effect of an impact will be a visible dent). Structural integrity may be assessed using
a variety of techniques based on ultrasound, thermography, X-ray radiography, or other methods. These techniques not only avoid
damaging the composite material but also are in many cases suitable for inspection in situ. As Table 1 shows, the different tech-
niques vary in their sensitivity to specific types of defects, and each has particular advantages, so that several approaches may need to
be combined in critical applications, such as composite testing in the aerospace industry (70).
Sound-based techniques derive from modifications in the frequency response and transmission speed of a part, due to the
presence of heterogeneities. A simple example of a sound-based technique is the traditional tap test, where one taps a part and
listens for anomalies. Modern versions of this test use an instrumented handheld hammer. However, many recent test methods use
Figure 36 Methods for investigating the fiber–matrix interface in UD FRP: (a) Fragmentation test; (b) single-fiber pullout; and (c) bead pull-off test.
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Table 1 Specificity of different techniques for NDT testing of composite materials
Ultrasound Radiography Thermography Optical methods Mechanical impedance
Porosity þþ þþ þ þ þ
Debonding þþ þ þþ þþ þþ
Delamination þþ þ þþ þþ þþ
Impact damage þþ þþ þ þ þ
Fiber cracking þþ þ
Resin cracking þþ þ
Inhomogeneous cure þþ þþ þþ þþ
Inclusions þþ þ
Moisture þþ
ultrasound (50 kHz–100 MHz) generated by a piezoelectric transducer at the specimen surface. In pulse–echo systems, the same
transducer detects the signal reflected from the composite. However, it is also possible to use a second sensor to detect the trans-
mitted signal. Two main types of analysis are used: A-scan and C-scan. The A-scan method typically involves a handheld transducer
and the pulse–echo technique, with sudden changes in the measured amplitude usually indicating some form of defect in the
structure. In the C-scan method, which may be used in pulse–echo or transmission mode, the transducer scans the part auto-
matically, and the results provide a spatial representation of the internal structure of the specimen, as shown in Figure 37 (71). For
this purpose, the specimens are usually immersed in water to reduce the attenuation of the signal at the specimen surface (a viscous
couplant may be used for a handheld probe).
Electro-magnetic methods make use of various regions of the electromagnetic spectrum. For example, certain flaws may be
detected simply by looking at visible light transmission through the composite. However, carbon fiber composites are opaque and
require alternative approaches, such as thermography, in which a laminate is excited by a thermal wave. Variations in infrared
emission, which may be detected using an infrared camera, reveal various types of flaws without the need for direct contact with the
specimen. Radiography is also widely used, in which case defects and also the fibers themselves may be imaged by differential
absorption of low energy X-rays, with penetrants such as tetraboromethane (TBE) used to increase contrast from porosity or internal
cracks. Given sufficient contrast, radiography may provide significantly better in-plane resolution than C-scan images and is rela-
tively rapid. Finally, optical monitoring (e.g., laser interferometry or holography) of the surface topography may be used to detect
anomalies in the deformation of specimens subjected to mechanical loading.
The mechanical impedance technique is based on relatively low-frequency vibrations produced by a piezoelectric transmitter,
whose response to structural inhomogeneities may be detected using a suitable sensor. While not particularly sensitive to many
types of defects, it is highly suited to the detection of delaminations or other types of defects that run parallel to the specimen
surface.
Another recent trend in composite testing is to use in situ monitoring of deformation and damage accumulation by the
permanent incorporation of a network of strain-sensitive elements into composite structures (72). In the near future, it should be
possible to use such networks not only for passive damage detection but also as the basis for active components that respond to
a localized damage event by releasing a healing agent (73).
Figure 37 C-scan sequential sections through a UD laminate showing internal impact delamination damage. Reproduced from Bourban, P. -E.
Endommagement, rupture et corrosion des composites thermodurcissables de mats de fibres de verre. Ph.D. Thesis No. 1148, Ecole Polytechnique
Fédérale de Lausanne, 1993.
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1.03.8 Environmental Testing
One of the major weaknesses of polymers as structural materials is the tendency of certain polymers to fail at low loads in the
presence of hostile environments. A well-known example is the failure of unsaturated rubbers in the presence of ozone, which
rapidly attacks double bonds under ambient conditions and produces extensive surface cracking even at very low stresses. This
necessitates careful optimization of stabilizer packages for items such as car tires, by using standard tests in which the rubber is held
under stress in an ozone atmosphere. Another example is the accelerated failure of polyolefins in the presence of tensioactive fluids,
such as certain detergents, that are associated with a transition from ductile failure to brittle failure under low-level loading; and, as
already discussed in Section 1.03.6.4, such fluids are also used as a means of accelerating slow crack growth under both static and
dynamic loading. Many glassy polymers are also sensitive to solvents, which may promote craze formation over other deformation
modes, which leads to embrittlement and hazing of transparent plastics (this is often cited as a reason for not using adhesive stickers
on plastic crash helmets). In polyamides, a significant humidity uptake is observed under ambient conditions, resulting in
significant plasticization, which is generally beneficial for toughness, so that in this case, low temperatures associated with low
ambient humidity are often of most concern. Finally, in composite materials, the matrix–filler interface is often sensitive to the
environment, resulting in phenomena such as ‘chalking’ (the formation of a powdery, dry, chalklike appearance or deposit on the
surface of a component) as well as degradation in mechanical properties. These effects imply that it is important to ensure adequate
specimen conditioning and control of the test environment in standard tests. Thus, the equilibration of moisture-sensitive speci-
mens, such as polyamides, in a controlled-humidity oven is recommended prior to any type of mechanical or physical test.
The broader implications of environmental exposure for plastics properties, including their end-of-life behavior (combustion
and compositing), has given rise to a range of test methods that are specific to different types of exposure, as will be discussed briefly
in the remainder of this section.
1.03.8.1 Thermal Aging

Thermal aging refers to long-term, irreversible changes in the structure, composition, and morphology of materials exposed to
temperatures that they are typically likely to encounter in service. It may result from a combination of mechanical loading and
chemical changes, among which oxidation through contact with atmospheric oxygen is usually the most important. In practice,
the lifetime of a plastic or FRP subjected to physical aging is defined in terms of a critical threshold for an easily measured
physical property, such as the strain to break, which is referred to as an ‘end-of-life’ criterion. Depending on the choice of
criterion, it is often possible to link the lifetime to the aging temperature via an Arrhenius-type relationship, with the aim of
providing long-term predictions. However, as with extrapolation of creep lifetimes (Section 1.03.5.4), the possibility of tran-
sitions in mechanisms within the range of temperatures of interest may render this approach unreliable. The technique used to
monitor thermal aging usually depends on the property of interest, but spectroscopic methods such as FTIR (Section 1.03.3.4)
are often used to interpret the observed physical property changes in terms of changes in chemical structure, such as the
appearance of –OH and C] O groups, characteristic of the thermooxydative degradation of aliphatic polymers. DSC may also
be used to investigate annealing and aging effects, while the evolution of the molar mass distribution may be followed by GPC
or viscosimetry (Section 1.03.3.1).
1.03.8.2 Weathering
Weathering tests are designed to determine the aging behavior of materials during outdoor climate exposure. They involve effects
that are due not only to heat and humidity variations, but also to factors such as erosion (via, e.g., wind or rainfall), pollution,
microbial attack, and, most importantly, exposure to ultraviolet radiation, which constitutes some 2–7% of the solar spectrum. As
with thermal aging, UV degradation is typically dominated by oxidation reactions due to the presence of atmospheric oxygen, which
is initiated by the absorption of high-energy UV photons. Depending on the polymer, these may lead to either chain scission or
cross-linking, with immediate consequences for the mechanical properties. UV degradation also results in pronounced yellowing in
many transparent polymers, such as PS or PC, which limit service lifetimes in certain applications, even in the absence of significant
deterioration in the material’s bulk strength and stiffness. The effects of UV degradation on materials destined for long-term outdoor
applications are generally assessed using accelerated exposure tests in which color changes, surface appearance, oxygen uptake, and
chemical changes are continuously monitored. Such tests may be carried out under laboratory conditions using high-intensity UV
sources such as carbon or xenon arc lamps or fluorescent UV lamps. Xenon arc lamps are often preferred because they produce
a spectral output that is similar to the sun. However, it is generally difficult to establish quantitative correlations between the results
of indoor accelerated aging tests and outdoor exposure, owing to additional factors, such as migration and leaching of additives,
which may act in synergy with microbial attack, erosion, or other factors, resulting in substantial decreases in product lifetimes. As
a result, laboratory weathering tests are increasingly combining UV testing with environmental simulations and taking into account
one or more of these factors. An alternative is to use accelerated outdoor testing based on solar concentrator and tracking tech-
nologies. By using these tests, it is in principle possible to simulate decades of natural UV radiation exposure in less than a year.
However, while such tests incorporate all the factors that contribute to weathering in service, these are difficult to control, and the
results will clearly depend on the local geographical conditions, which should ideally be matched to those under which the material
will be used.
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1.03.8.3 Thermal Degradation and Fire Resistance

Thermal degradation, as opposed to thermal aging, refers to the short-term effects of heating and is critical for processing, during
which the plastic is exposed to temperatures well above the intended final use temperature. TGA (Section 1.03.3.2) is widely used to
provide a rapid determination of the associated limits on processing windows. These correspond to the onset of pyrolysis, which is
generally the first step in combustion, given an oxidizing atmosphere.
Fire hazard requirements vary widely depending on the application, and are particularly important in the aeronautics industry,
for example. These requirements also involve a variety of criteria related to phenomena such as the ignition of combustion, the
sustainability of combustion at a given oxygen level, heat generation during combustion, and mechanical integrity (e.g., resistance
to dripping), and specific tests have been developed to cover all of these scenarios (74). In ignitability tests, a specimen is exposed to
flowing air and the temperature increased until the specimen ignites (from either self-ignition or flash ignition, depending on
whether a pilot light is used). The limiting oxygen index test (Figure 38(a)) provides a measure of extinguishability. It is used to
determine the minimum oxygen concentration in the oxygen–nitrogen mixture that is required to ignite a polymer and maintain its
combustion. Fire performance in the developing regimes that follow ignition is also widely characterized by the cone calorimeter
test (Figure 38(b)), in which a fixed heat flux is applied to the specimen and the gases resulting from pyrolysis are ignited in the
presence of atmospheric oxygen. Such tests enable one to measure heat release (e.g., by monitoring oxygen consumption), release of
gases (CO, CO2, etc.), mass loss, and smoke scattering simultaneously. The exact conditions may be varied in standard tests in order
to simulate different scenarios (e.g., small or large fires, or different specimen geometries). Finally, there are a wide variety of tests
aimed at specific applications and specific aspects of combustion, such as flame spread and penetration resistance (75).
1.03.8.4 Biodegradation
Biodegradable plastics undergo biological degradation by microorganisms to give lower molecular weight molecules that may be
dispersed in the environment without adverse consequences. In general, biodegradable plastics are required to be insoluble in water
so that degradation is heterogeneous, involving sufficient reduction of the molar mass at the polymer surface by extracellular
enzymes to permit uptake by living cells and incorporation into metabolic pathways. Nonbiological processes such as hydrolysis
may also play an important role; however, it is often more correct to refer to environmental degradation in this context. Various
definitions of biodegradation have been proposed by the different standards organizations. Compostability is of particular
importance for the packaging industry, where the term is generally considered to describe the ability of a plastic to biodegrade in
a composting system (76,77).
A large number of standards and accompanying analytical methods have been developed in recent years to address the problem
of biodegradation and often concern unwanted biodegradation, as in microbial attack on structural elements during weathering
(see Section 1.03.8.2). These fall into three main categories: laboratory tests, simulations, and field tests. While field tests appear to
be most appropriate to real conditions, as with weathering tests, it is difficult to control environmental conditions such as
temperature and pH and to analytically monitor the degradation process (in this case, analysis may be limited to looking for visible
traces of the test specimen in certain tests). Therefore, simulated environmental conditions may be preferable in many cases, and
a number of tests have been introduced to simulate specific environments such as landfills and composting (76). Laboratory tests
under well-defined conditions (e.g., microbial strains and synthetic media) may give more reproducible results, and are often used
in fundamental studies and for initial screening. However, such tests are difficult to quantitatively link to conditions that are likely
to be encountered in practice.
Figure 38 (a) Apparatus for measuring the limiting oxygen index; and (b) cone calorimeter test.
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1.03.9 Conclusions
It has been necessary to limit or omit discussion of many important topics in this chapter, and, within the broader context of plastics
testing, it may be questioned whether the traditional emphasis on mechanical plastics testing remains a reasonable choice in all
scenarios. Certainly, as the focus in the polymer industry shifts toward bioplastics, there will be increasing concern with issues that
have only been treated superficially here, such as biodegradation and environmental impact. However, bioplastics must continue to
fulfill basic design criteria with regard to both processing and final properties, and mechanical and rheological testing will remain
fundamental to plastics engineering in the foreseeable future. One might also argue that because specialty polymers are increasingly
required to show multiple functionality, the corresponding properties (electrical properties, biological properties, or optical
properties) should be considered alongside mechanical properties. On the other hand, the vast array of test techniques associated
with these additional functions is not always specifically aimed at polymer testing, and in many cases, the response of a given plastic
to physical stimuli owes more to local chemical structure or the presence of additives than to its polymeric character. Of course, such
considerations do not apply to many of the standard test methods used for textiles, coatings, and adhesives, whose omission can be
justified only in terms of lack of space.
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1.04 Stress-Based Forming Limit Curves
TB Stoughton, General Motors Global Research and Development Center, Warren, MI, USA
JW Yoon, Deakin University, Geelong Waurn Ponds, VIC, Australia
Published by Elsevier Ltd.
1.04.2 Strain-Based Forming Limit Criteria 72
1.04.3 Stress-Based Forming Limit Criteria 76
1.04.4 Summary and Conclusions 83
References 83
1.04.1 Introduction
The metal-forming industry routinely uses forming limit criteria in the analysis of stamped sheet metal and tube
hydroformed components to obtain more robust manufacturing processes and improved product performance charac-
teristics. These criteria are essential to computer-aided engineering during product design and manufacturing process
development for analysis of predicted stress and strain histories of the deformation process. Forming limit criteria are also
helpful later during physical validation of the sheet-forming process, and during die tryout for analysis of measurements
of actual forming strains and strain histories, to help ensure robust manufacturing in production. Finally, forming limit
criteria are an essential element of computer-aided engineering of product design to help optimize performance
requirements early in the product development cycle and reduce the dependence on physical testing to achieve optimal
product performance.
The most important deformation limit for sheet forming concerns avoidance of the onset of a surface defect known as
a localized neck (also called a through-thickness neck), which appears as a grove across the surface of the sheet with a width
dimension that is approximately equal to the sheet thickness. Localized necking is often immediately followed by fracture at the
thinnest point within the developing neck. As the product or manufacturing process is improved, fractures are naturally elim-
inated first, followed by elimination of the necks that precipitated the fracture through further modification of the product or
manufacturing process. Although fracture is a much more serious defect, localized necking is also unacceptable from the aspect
of product quality. Since localized necking is the most frequent cause of fracture in manufacturing, the metal-forming industry
has focused a great deal of attention in the last 50 years on developing criteria to predict and avoid the onset of necking that is
reliable under the varied forming conditions that occur in manufacturing processes. Since necks most often precede fracture
under tensile loading, the metal-forming industry has until recently considered it sufficient to utilize only a necking limit
criterion for analysis of manufacturing processes, or otherwise treat necking and fracture as indistinguishable with a single
forming limit criterion.
It is important to recognize that for the purpose of forming limits in manufacturing, there is no particular concern with
another type of strain localization known as diffuse necking, such as that seen in a uniaxial tension test after maximum load is
achieved. The condition of maximum load, also known as the Considere Condition, causes the uniaxial tension specimen to
elastically unload along most of its length, while a small section of the length, the region of diffuse necking, continues to stretch
in a nonuniform manner under plastic deformation. The length of this plastically deforming region is approximately equal to the
width of the tensile specimen, and it continues to strain harden with increasing stress, but at a slower rate than the reduction of
the cross-sectional area, so that the load decreases at a rate equal to the elastically unloading sections in the specimen. The
nonuniformity of strain within the diffuse neck arises because the edge along the length of the specimen is free to distort and
contract nonuniformly. In contrast to the uniaxial tension test, if a uniaxial stress condition existed within the body of
a deforming sheet, isolated from the edges due to the complexity of the geometry, then there would be no edge and no length
scale that would allow a localization corresponding to a diffuse neck to occur. As a result, the deformation would proceed as
a stable plastic flow under decreasing load without any surface or other visible defect. Consequently, in the body of the deforming
sheet, the only neck that is a forming limit to manufacturability of a product is one that develops through the thickness. This type
of bifurcation is always possible, due to the intrinsic proximity of the sheet surfaces that allow the grove through the sheet
thickness to form.
This chapter will primarily focus on models for predicting when localized necking will occur in complex stamping processes. We
begin with a review and history of the strain-based forming limit diagram in Section 1.04.2, which is widely used by the metal-
forming industry to characterize the necking limits of a given metal. This section will also emphasize the limitations of this method
with respect to the handling of nonlinear strain paths. Section 1.04.3 introduces the stress-based forming limit diagram, including
its history and a critical discussion of its experimental and theoretical basis, followed by a summary and conclusion in
Section 1.04.4 and the list of references.

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72 Stress-Based Forming Limit Curves
1.04.2 Strain-Based Forming Limit Criteria
The Forming Limit Diagram (FLD) was proposed by Keeler and Backhofen (1) as an analysis tool for use in die tryout of sheet metal
stamping processes to determine how close the process is to cause necks to form during stretching of the metal. The FLD is
composed of a plot of the major principal strain versus minor principal strain and contains an empirically determined forming limit
curve (FLC) to define the strain limit at the onset of necking for a given metal. The diagram was further improved for characterizing
limit strains on the left-hand side of the FLD (negative minor strain) and validated through industrial trials by Goodwin (2), and
was widely adopted by industry in the early 1970s. Due to their contributions, it is sometimes referred to as the Keeler–Goodwin
diagram, but more often it is simply called the FLD. For the purposes of this chapter and to clarify the distinction with other types of
diagrams, we will refer to this diagram as the Strain FLD. An example of the Strain FLD for an aluminum alloy 2008-T4 reported by
Graf and Hosford (3) is shown in Figure 1, which shows the shape of the Strain FLC that is common to aluminum and steel alloys in
the as-received condition, which are characterized by a minimum in the plane strain condition (minor strain equal to zero) and
where the major strain at this point is referred to as FLD-zero and denoted as FLDo.
One of the most attractive features of the Strain FLD is that it helps to identify opportunities for eliminating necking in the
manufacturing process that may not be obvious without the aid of a diagram. For example, due to the lowest point on the Strain FLC
at FLDo, any necking condition slightly above the Strain FLC may be remedied by increasing the magnitude of the minor strain
without decreasing the major strain. This solution is beneficial because higher strains are intrinsic to forming complex geometries,
so use of the Strain FLD may help find solutions to formability problems through process modification without significant product
concessions. Another attractive feature of the Strain FLD is that by modifying the manufacturing process such that the strains are
a specified distance from the Strain FLC, engineers ostensibly ensure robustness of the manufacturing process to handle the material
and process variations that are expected during the mass production of up to a 100 000 stampings with the tooling.
While the Strain FLD was originally introduced as a tryout tool, its greatest impact was realized decades later in virtual tryout that
uses finite element simulation of the sheet-forming process, since the opportunities for process modification are much larger, and
the cost and consequences of product concessions are much smaller at this early stage of the product development cycle. It is also
easier and more comprehensive to implement forming limit analysis in virtual tryout, since the predicted strains across the entire
formed panel can be instantly shown in a single Strain FLD at the conclusion of the finite element simulation, such as is reproduced
in Figure 2 for the stamping of a structural steel panel that involves more than 300 000 elements. This distribution of strains is well
below the Strain FLC and reflects a great deal of engineering work that was required to optimize manufacturing conditions and
obtain necessary product concessions to realize what appears to be a robust manufacturing process.
Despite the popularity of the Strain FLD, it is widely misinterpreted and misused in industry. In this chapter, we will demonstrate
that the Strain FLD as it is commonly used is not effective for reliably realizing its supposed benefits. However, with a better
understanding of the causes of these limitations, we will propose solutions equivalent in function to the Strain FLD that meet or at
least come much closer to realizing the benefits that are commonly attributed to the Strain FLD.
The root of the misunderstanding about the Strain FLD is that the Strain FLC is interpreted as a static limit. This interpretation is
implicit in its use to analyze strains from finite element simulation and to optimize strain conditions from a stamping to produce
Strain FLD
0.4
0.3
Major Strain
0.2
0.1
0.0
–0.2 –0.1 0.0 0.1 0.2 0.3
Minor Strain
Figure 1 Keeler–Goodwin FLD with the Strain FLC of 2008-T4 aluminum in the as-received state as reported by Graf and Hosford. Reproduced from
Graf, A. F.; Hosford, W. F. Metall. Trans. A 1993, 24, 2503–2512.
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Stress-Based Forming Limit Curves 73
Strain FLC
Strain Analysis
+8.7% Margin of Safety
Figure 2 Example of how the FLD is used to optimize a stamping process through simulation to achieve apparently robust processes.
ostensibly robust manufacturing processes, such as in the example shown in Figure 2. The dynamic nature of the Strain FLC was first
documented by Nakazima et al. (4) in 1968, but continues to be recognized in academic studies of the effect of nonlinear strain
paths, such as the previously referenced study of AA 2008-T4 alloy reported by Graf and Hosford. In addition to measuring the
Strain FLC for a linear strain path from the as-received condition of the sheet as shown in Figure 1, Graf and Hosford also measured
and reported the net strain at the onset of necking after first straining the as-received metal to a set of two different strain levels in
plane strain conditions along the rolling and transverse directions, three strain levels in uniaxial tension along the rolling and
transverse directions, and four strain levels in equal-biaxial tension. The results of these 14 tests are shown in Figure 3 and clearly
demonstrate that the Strain FLC is not static, but is a dynamic limit. The dynamic nature is perhaps more clearly understood with the
set of four snapshots of the dynamic limit for uniaxial tension along the rolling direction, as shown in Figure 4. Here we can see that
the only point on the original Strain FLC for the as-received condition that remains static is the point in the direction of the linear
strain path. In all other directions, the Strain FLC has changed such that in some directions the limit is lower, while in other
directions, the limit is higher than the limit in the as-received condition.
Strain FLD
0.4
P1 P2 P3 P4 U1
U2 U3 U4 U5 U6
E1 E2 E3 E4 AR
0.3
Principal Strain Along R
0.2
0.1
0.0
–0.2 –0.1 0.0 0.1 0.2 0.3 0.4
–0.1
Principal Strain Along T
Figure 3 Forming limit of 2008-T4 aluminum alloy after various modes and levels of prestrain, as reported by Graf and Hosford. Reproduced from Graf,
A. F.; Hosford, W. F. Metall. Trans. A 1993, 24, 2503–2512.
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Strain FLD
0.4
U1 U2 U3 AR
0.3
Principal Strain Along R

0.2
0.1
0.0
–0.2 –0.1 0.0 0.1 0.2 0.3
Principal Strain Along T
Figure 4 Dynamic nature of the strain-forming limit of 2008-T4 AA for a linear strain path in uniaxial tension along the rolling direction.
Ignoring the dynamic nature of the Strain FLC has consequences, as was the case for the die tryout of the manufacturing process
simulated, and resulting in the net strains shown in Figure 2. Rather than passing through tryout without any problems, as one
might expect if the Strain FLC were static and the strains were as shown in Figure 2, necking and tearing was observed in two of the
four corners of the panel. It was later realized that the strain paths in these two areas were highly nonlinear, which meant that the
starting position of the Strain FLC was an invalid gauge for assessing the formability of the strain history of the area that became
critical. As a result, it took an additional six months before a formable condition was obtained through the trial-and-error die tryout
process, requiring product concessions to be made at great cost much later in the development process.
While these costly negative consequences result from ignoring the dynamic nature of the Strain FLC, there is a significant positive
benefit from accounting for the dynamic effects in addition to simply avoiding the costly negative consequences. Nakazima was one
of the first to recognize the positive benefits of accounting for the dynamic effect by identifying surprisingly high levels of strain that
are formable for certain nonlinear strain paths, particularly those with final strain increments driven by conditions close to uniaxial
or equal-biaxial tension. Evidence of these unusually high strains is shown in Figures 3 and 4, where the net strain-forming limit
after the first stage of forming is found in some directions of the secondary increment to be higher than the Strain FLC for linear
strain path in the as-received condition, which is shown as the heavy black line in Figures 3 and 4. This data literally means that one
can achieve strains up to these dynamic limits by following the bilinear strain paths that were followed in these experiments.
The first and perhaps only example of successful application of this understanding in die tryout was reported by Ishigaki (5) in
1978. He reported that during die tryout of a rear quarter panel of a Toyota product stamped from a deep drawing quality steel,
tearing was observed in the rear light area during the final cam die restrike operation, resulting in a strain level that is indicated by
the red point in Figure 5. This strain is seen to be below the measured static Strain FLC for this steel, which is shown in the figure as
a heavy black line. Analysis of the strain path during forming not only confirmed that the strain path is nonlinear, but showed that
the level of strain after the first draw operation, which is shown as the black point in the figure, was achieved by an approximately
linear strain path at a strain condition of ('0.26, þ0.37). This strain state happened to be close to the strain condition for uniaxial
tension for this metal. This observation justified an effort to prestrain large amounts of the metal in uniaxial tension to a major
strain of 0.37 in order to measure the change in the Strain FLC, which is shown in Figure 6 as the heavy red line. Since the strain path
of two cam restrike operations was also approximately linear, the engineers argued that because the measured FLC after prestrain
explains why the metal necked and tore during the restrike, the same FLC depicts the forming limit for other approximately linear
strain paths that can be achieved by modification of the two restrike operations. Ishigaki reported that the engineers then modified
the cam-form process to drive the final strain along the path indicated in Figure 6 by the dashed green line that ends at the green
point. Ishigaki also reported that this solved the necking and tearing problems and so Toyota went into production with this
modified process, confident in the safety margin between the final strain shown as the green point and the dynamic forming limit as
it was at the end of the first draw, shown at the red curve. What is particularly exciting about this result is how far this strain
condition is above the static Strain FLC for this steel, which is shown by the solid black curve. The reason this is so important is that
by allowing higher strains, not only were the engineers able to achieve the original product design shape without concessions, but
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Figure 5 Strain path ending in a tear below the Strain FLC in early die tryout of the forming of a rear quarter panel as reported by Ishigaki.
Figure 6 Neck/tear-free strain path at the end of tryout that was motivated and justified after determination of the dynamic strain limit.
the higher tensions enabled greater use of the metal strain hardening characteristics to produce a stiffer higher quality panel. In
addition, the higher local and overall stretch translates to less volume of metal within the product, and therefore, a lighter weight
product.
While the achievement reported by Ishigaki is inspiring, it all came about because of several unlikely and fortuitous circum-
stances that allowed the engineers to empirically determine what the dynamic strain limit was at a critical juncture in the forming
process. In most applications, strain paths are too complicated or inherently beyond the scope of what can be reproduced in the lab.
Without an understanding of the cause of why the strain-forming limit is dynamic, it is impossible to determine what the strain
limits are for an arbitrary nonlinear strain path. In other words, in general, there was no obvious empirical way to determine the
location of the red curve shown in Figure 6, except for the unusual circumstance of this particular strain path. For this reason, in the
last 35 years, no one has claimed to have been able to apply the methods described by Ishigaki in die tryout for other applications.
However, as will be demonstrated in the next section, with an understanding of what is causing the dynamics of the strain path
effect, and to the extent known today, it is possible to apply these techniques not only to physical die tryouts, but also in the analysis
of finite element simulation results for any application, regardless of the complexity of the strain path.
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1.04.3 Stress-Based Forming Limit Criteria
A reasonable interpretation of the experimental data shown in Figure 3 is that the forming limit of the metal is not a function of the
strain, or if it is, it is also a function of something else. An obvious answer to what that something else could be is the stress condition.
In 1977, Kleemola and Pelkkikangas (6) were perhaps the first to propose using a forming limit diagram based on stress variables for
analysis of secondary forming processes, but one of the reasons this idea went largely unnoticed was that they did not publish
experimental evidence to show the merits of using stress analysis. Later, in 1982, Arrieux, Bedrin, and Boivin (7) published the results
of Arrieux’s thesis, including experimental evidence showing that the stress-forming limit of several steel alloys were insensitive to
nonlinearity in the strain path. But even then, the metal-forming industry remained largely unaware of these solutions, possibly
because Kleemola et al. and Arrieux et al. emphasized the application of stress-forming limits for the analysis of secondary forming
processes, which at the time was receiving little attention with respect to formability, as industry was largely focused on formability in
the first draw die. With the exception of a few studies, such as the one reported by Ishigaki in the previous section, little effort was
made to address and resolve the formability issues of secondary forming processes using the forming limit diagram.
The motivation changed sometime in the mid-1990s when industrial scientists came to the realization that the dynamic nature of
the Strain FLC was not a problem that was limited to secondary forming operations, but would apply equally well to the first forming
operation. While metal tends to deform under a linear strain path, a fact that explains why the Strain FLD was successfully adopted by
industry in the 1970s, nonlinear strain paths commonly occur in specific areas of the die, such as in corners of deeply drawn
stampings, where the strain path changes from drawing conditions to near plane-strain stress conditions as the metal pulls from the
binder into the nearly vertical wall of a die cavity. Strain path changes are also driven by contact between the sheet and tooling
surfaces to form complex geometry. The effects are especially noticeable in late contact areas, such as window and fuel filler door
openings, door handle areas, some stylistic features, and engineering surfaces that are required for fixtures or other purposes. In all of
these areas of the first draw die, analysis of the forming severity based on a static Strain FLC will give an erroneous picture of the local
formability, which doesn’t become apparent until die tryout results in ‘unexpected’ necking and splitting. This problem occurs in an
estimated 10% of the first draw dies that have been approved for die build based on a static Strain FLC. Even that estimate is
conservative because it assumes that additional limits on maximum thinning are also used, which are effective at avoiding some of
the expected failures that occur due to nonlinear strain paths in the equal-biaxial stretch conditions shown in Figure 3.
After realizing the importance of nonlinear strain paths in the first draw die and the cost of treating strain limits as though they
were static, Stoughton (8) rediscovered the value of formability assessments based on the stress condition and published an analysis
of the Strain FLCs for a number of materials reported in the literature in 2000, including the equal-biaxial prestrain of steel,
published by Ghosh and Laukonis (9), and the multiple prestrain conditions for AA 2008-T4 published in the previously referenced
work of Graf and Hosford. Figure 7 shows six Strain FLCs reported by Graf and Hosford, including the FLCs after 0.12 major true
strain in uniaxial tension along the rolling and transverse directions, the FC after 0.08 major true strain under near-plane-strain
conditions along the rolling and transverse directions, and the FC after 0.07 major true strain in equal-biaxial strain conditions,
along with the FLC for the as-received condition. Using the material properties of AA 2008-T4 reported in Graf and Hosford’s
publications of Graf ’s thesis work, combined with isotropic power law hardening and Hill’s 1948 yield function (10), Stoughton
calculated the stress conditions for each of these FLCs and showed that the limiting conditions collapse to what appears to be
a single curve in the Stress FLD, as shown in Figure 8. One of the remarkable facts of this analysis is that the measurement of the
FLCs and the material properties were reported several years before the analysis of the stress conditions. This is important because
definition of the shape of the FLC is subject to human interpretation. The flexibility in drawing the strain limit curves could
Figure 7 Strain path ending in a tear below the Strain FLC in early die tryout of the forming of a rear quarter panel as reported by Ishigaki.
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Figure 8 Neck/tear-free strain path at the end of tryout that was motivated and justified by measurement of the dynamic strain limit.
unintentionally influence their shape if the goal was to seek a pattern in the behavior, such as degeneracy to a single stress limit.
However, because the experiments were recorded years before the stress analysis was attempted, there is no possibility of unin-
tentional bias in defining where to draw the strain limit curves in Figure 7 to improve the results seen in Figure 8. As a result and
after other observations, Stoughton concluded that the dynamic nature of the Strain FLC is an artifact of a static Stress FLC and the
nonunique relationship between the net plastic strain and the stress conditions that control the plastic strain rate.
The conclusion drawn from Figure 8 is that the Stress FLC is static and can be productively used in analysis of complex stamping
processes that is still not universally accepted, and other interpretations of the evidence shown in this figure have been offered. The
reasons for the reluctance to accept a stress-based forming limit criteria suggested by Figure 8 undoubtedly may also help explain
the lack of acceptance of the independent works published by Kleemola and Arrieux more than 30 years ago. In the remainder of
this section, we will address common objections to using stress metrics to assess formability, and we will provide additional analysis
and theoretical arguments to resolve these concerns.
One argument for the nonacceptance of stress-forming limits is the level of theoretical understanding and work that has been
done to explain the strain-forming limit. The theoretical foundation of the Strain FLD includes bifurcation models of Hill (11) in
which a neck forms at an angle to the major tension axis due to a load bifurcation that allows a solution with zero extension of the
material along the axis of the neck. The model only applies under conditions of negative minor strain rates and successfully
describes the orientation of the neck for uniaxial and biaxial tension conditions and the shape of the FLC on the left-hand side of the
Strain FLD where the minor strain rate is negative. Another bifurcation model in support of the Strain FLD is based on deformation
theory, as described by Storen and Rice (12), and applies to both sides of the Strain FLD. Later, Zhu et al. (13) introduced the
consideration of moment balance between the neck and outlying region, resulting in a generalized bifurcation condition that
included Hill’s and Storen and Rice’s models as solutions. The Storen and Rice approach was also generalized to apply to incre-
mental theory by Hutchinson and Neale (14,15) for both rate-independent and rate-sensitive materials. Finally, one of the most
widely used theoretical models of the Strain FLD is the Marciniak–Kuczynski (M-K) (16) defect model, which defines necking to
occur when the plastic strain rates within a preexisting defect diverge from the plastic strain rates in the matrix by a prescribed
condition. In addition to providing a theoretical basis for the Strain FLD, these models may also contribute to the level of skepticism
regarding claims that the Strain FLD is wrong or that forming limits are actually caused by a completely different set of variables that
cannot be uniquely represented in the strain diagram.
A turning point in this perspective originated from Zhu, who understood that the derivation of forming limits in all the models
described above requires the introduction of an assumed linear strain path. While the M–K model has also been used with mixed
success to predict FLCs for nonlinear strain paths, it seems that no one had purposefully asked what the assumption of strain path
on these models means with regard to what is actually causing the neck to form. Zhu understood that prior to imposing any
assumption about strain path in the bifurcation models, the bifurcation conditions under plastic deformation describe a unique set
of stress conditions that did not depend on any history variables other than those defined uniquely by the current stress conditions.
This led Stoughton and Zhu (17) to review the derivation of these bifurcation models, introducing the form of the constitutive
model under isotropic hardening, but omitting the step of imposing a strain path to derive an explicit equation for the stress limit
for an otherwise arbitrary history of plastic deformation. Although they did not provide numerical analysis, they also pointed out
that the strain rates and strain paths that occur in the defect and matrix of the M–K model are driven solely by the imposed stress
conditions. Since the necking is defined by the divergence of the strain rates in the matrix and defect, they argued without proof that
the M–K model will also predict a single-stress FLC. This was later confirmed through numerical analysis by Zeng et al. (18).
Ironically, while the well-established theoretical basis of the Strain FLD has perhaps contributed to the reluctance to accept a new
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approach based on a stress FLD, these same models actually validate the concept of characterizing history-independent forming
limits in terms of stress variables, at least for conditions under which isotropic hardening prevails.
Another cause for nonacceptance of stress-forming limits is the misinterpretation of the data in Figure 8 that the close proximity
of the curves is only an artifact of the saturation of the stress due to the nature of the hardening law, and that the data does not
provide evidence that stress limits are independent of the path taken to get to these limit stresses. However, the original analysis
published by Stoughton noted that the stress curves are not simply squeezed together, but are overlapped, crossing each other
between areas of stress space where the curves are slightly above or slightly below each other. On the other hand, a few of the 14
prestrain conditions shown in Figure 3 result in portions of the stress curves that show significant deviation from the Stress FLC for
the as-received condition. Most of the latter outlying portions of these deviating curves were found to cover portions of the Strain
FLC that had too little or no experimental data to justify drawing the strain curve where it was drawn. In contrast to areas of the curve
that are supported by too little data, it was also noted that the cusp of each Strain FLC is remarkably close to the same stress
condition for all tests, which is argued to reflect the fact that most of the experimental measurements were made near the plane-
strain stress condition to determine this critical limit condition associated with FLDo as accurately as possible.
In contrast to the predominant evidence for a static stress limit, the highest level of prestrain for a given mode of prestrain does
show some indication of a path dependency. However, this may be explained as an artifact of the assumption of isotropic hardening
and the neglect of kinematic effects that result in a small amount of plastic deformation after early yielding and transient hardening
prior to recovery of the isotropic hardening behavior, which are not considered under isotropic hardening models. A likely remedy
for those cases would be the use of a more realistic hardening law that included kinematic or distortional hardening effects. Finally,
among the majority of the prestrain conditions, it was noted that no pattern was detected in the changes of the FLC with the
magnitude of prestrain for a given mode of prestrain. These observations are not consistent with the interpretation that Figure 8
reflects the effect of a saturated stress condition, but they are consistent with the interpretation that the scatter is due to the
experimental uncertainty in the measurement of the Strain FLCs.
In order to explicitly demonstrate that the scatter is consistent with experimental uncertainty, we can take the single-stress limit
curve calculated from the Strain FLC for the as-received condition, as shown in Figure 1, to obtain the Stress FLC shown in Figure 9.
Then we can use this single curve to predict the net strain at the onset of necking for different loading conditions after each condition
of prestrain, based on the assumption that the Stress FLC is static. The predicted net Strain FLCs are shown as the dashed lines in
Figure 10, along with the experimental FLCs for each of these prestrain conditions. We assert that experimentalists tasked with
measuring Strain FLCs would be delighted to be able to reproduce the same FLC from another set of tests on the same batch of
material to the level of the differences seen between the pairs of dashed and solid curves in Figure 10. It is especially important to
note that a single Stress FLC is able to predict not only the translation of the cusp of the Strain FLC with prestrain, but also the
sharpening of the cusp, as seen in Figure 10, by comparing the wider V-shape of the Strain FLC in the as-received condition to the
narrower V-shapes of any one of the Strain FLCs after prestrain. The small strain differences of a few percent between these dashed
limit curves and the corresponding experimental forming limits shown as solid lines is remarkably strong evidence in support of the
conclusion that these sets of predicted and experimental curves are within experimental uncertainty the same curves. Consequently,
it is reasonable to conclude that the degeneracy of the stress limit conditions seen in Figure 8 is due to the fact that the forming
limits depend only on the state of stress, and not on the path taken to reach the critical stress levels.
Figure 9 Stress FLC corresponding to the Strain FLC shown in Figure 2 is shown here as the solid line. Dashed lines indicate the stress history
corresponding to selected prestrain conditions.
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Figure 10 Comparison of predicted (dashed line) and experimental (solid line) Strain FLC. Predictions are based on the assumed static Stress FLC
shown in Figure 9.
Another argument against acceptance of the Stress FLD is that calculation of the stress-forming limit curves shown in Figure 8
would be completely different if one used a different model. This argument is ostensibly made to suggest that these stress limits are
artificial and therefore not real in the same sense as the strain limits. A counterargument is that one should always use the material
model that produces the most accurate stress and strain predictions. Consequently, there is in fact no ambiguity about what material
model should be used to calculate the stress limit. Despite the fact that the stress limit depends on the material model, once the
appropriate model is selected and calibrated, the stress limit is a unique curve.
Nevertheless, the concern about selection of the material model does raise an interesting question about the degeneracy of the
stress-forming limit. That question is, ‘Does the model that gives the most accurate stress and strain predictions also lead to
a degeneracy of the stress forming limit, such as seen in Figure 8?’ This question is particularly troubling because Hill’s (10) model
used in the calculations shown in Figure 8 is known to not be the best model for aluminum alloys. In a 2003 paper, Stoughton (19)
analyzed the Graf and Hosford data using several yield functions, including von Mises, Hill (10), a nonassociated flow model
proposed by Stoughton (20), and the Barlat (21) model, which is particularly popular in the description of the deformation
behavior of aluminum alloys. While these different yield functions were shown to result in very different stress-forming limit curves,
the degeneracy of the forming limits to a single stress limit curve was evident in all cases. This latter observation is very interesting
because it means that even though the so-called stresses may not represent the actual physical stresses, they are nevertheless reliable
metrics to differentiate safe from nonsafe conditions with respect to necking. The paper also considered the effect of various
hardening models, including Voce hardening with an artificially high exponent, demonstrating the practical use of stress limits even
in the case of asymptotic saturation, emphasizing the point that differentiation of safe and unsafe conditions is practical as long as
the hardening is monotonic for finite strain.
A more effective way to address the criticism with respect to saturation of the hardening law is to use alternate forms
of stress diagrams, which eliminates the hardening law from consideration. Among the first to propose this were Yoshida,
Kuwabara, and Kuroda (22) who noted that for isotropic monotonic hardening of a material with in-plane isotropy, the stress state
maps one-to-one to the value of the effective plastic strain (EPS) and the ratio of the principal stresses. They proposed to use an
equivalent stress-based diagram by plotting the EPS as a function of the stress ratio. Translating the data shown in Figure 7 into this
space leads to the FLCs shown in Figure 11, where it is seen that the prestrain conditions are shown as vertical dashed lines. The
prestrains are seen to consume 25–50% of the limit value of the EPS in the prestrain condition, with no significant change (within
experimental uncertainty) to the net limit on the EPS.
In addition to avoiding the use of the hardening law and the issue of stress saturation, the approach recommended by Yoshida
et al. describes the limits in the more familiar terms of strain. However, like stress, the value of EPS cannot be easily measured, since it
does not have a one-to-one correspondence to the net plastic strain, so for practical application, the EPS diagram is no less difficult to
use than the Stress FLD. Zeng et al. (18) have also recommended a similar solution of using a limit on the EPS value, but using the
ratio of the plastic strain rates as the ordinate, instead of the ratio of stresses. Finally, Stoughton and Yoon (23,24) proposed a polar
diagram of the effective plastic strain, which they referred to as the PEPS diagram. The EPS is the radial variable in this polar diagram,
and the angle with respect to the vertical direction is the arc tangent of the ratio of the minor and major plastic strain rates. Translating
the strain limits to this polar diagram leads to the set of FLCs shown in Figure 12, which, as expected, are within experimental
uncertainty of the FLC for the as-received condition of this aluminum alloy and is shown as the heavy black line. The particularly
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Figure 11 Translation of the FLCs shown in Figure 7 in terms of the variables recommended by Yoshida et al. Reproduced from Yoshida, K.; Kuwabara,
T.; Kuroda, M. Int. J. Plast. 2007, 23, 361–384.
Figure 12 PEPS diagram: Polar diagram of EPS values as recommended by Stoughton and Yoon. Reproduced from Stoughton, T. B.; Yoon, J. W.
Numisheet. In Conference Proceedings; Chung, K., et al., Eds.; AIP, 2011; pp 15–34 and Stoughton, T. B.; Yoon, J. W. Int. J. Solids Struct. 2012, 49,
3616–3625.
attractive characteristics of the PEPS diagram over the other EPS diagrams is (1) the shape of the PEPS FLC is similar to the shape of
the Strain FLC in the as-received condition in the conventional Strain FLD, and (2) due to the definition of the angle in PEPS Diagram,
the direction of the strain increments, or path, in the strain diagram, is locally parallel to the direction of the corresponding path in the
polar diagram. Consequently, the way die engineers would use the PEPS FLD to drive strain paths under nonlinear conditions is
identical to the way in which methods engineers use the Strain FLD to drive strain paths under linear conditions.
Any pair of variables that map one to one to the major and minor stress conditions will provide a suitable diagram for char-
acterized forming limits under nonlinear strain conditions. For example, instead of the EPS value in Figures 11 and 12, one can
replace the abscissa or radial variable in the two figures by the current yield stress, which for isotropic hardening is a monotonic
function of the EPS value defined by a hardening law. While the diagrams based on EPS are attractive because the units are in terms
of the familiar strain scale, the stress limit diagram is attractive because stress is arguably the driving mechanism of plastic strain and
localization, and would be a better metric for areas that have undergone unloading. While stress may be regarded as the causal
variable, the EPS is properly regarded as a symptom of the deformation, and while either can be used as one of the two metrics of the
necking limit, we will end this section with a demonstration of the application of the Stress FLC using two examples of how effective
the Stress FLD can be in practice.
In the first example, the tooling and stamping process for an automotive structural panel shown in Figure 13 was approved
based on simulations of the forming process that resulted in the strains previously discussed and shown in Figure 2. The net plastic
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Figure 13 Part geometry of an automotive stamping corresponding to the Figure 2 strain distribution and Figure 13 stress distribution.
Stress FLC
Stress Analysis
-20.1% Margin of Safety
Figure 14 Stress distribution responsible for the distribution of the net plastic strains seen in Figure 2 for the stamping of the part shown in Figure 13.
strains throughout the stamping were predicted to be 9% or more strain below the static Strain FLC. Physical tryout of the process
resulted in tearing in the two upper corners of the stamping shown in Figure 13, even though the measured thinning strains in these
critical areas were at the levels predicted in the simulation. The original analyses were rerun to reproduce the predicted strain
distribution shown in Figure 2 and to extract the forming stresses that developed in this process and were responsible for the strains.
These stress predictions are displayed in Figure 14, along with the calculated stress FLC, based on the same material model used in
the simulation and the Strain FLC shown in Figure 2. The fact that many elements are found to have stress conditions above the
stress limit while the net plastic strain on these same elements are more than 8% strain below the strain limit is attributed to the role
that a nonlinear strain path plays in this stamping process. In fact, the most critical elements were found to have stress conditions
with an EPS value more than 20% above the limit for that stress condition. The elements above the forming limit in Figure 14 are
plotted in red in Figure 13, showing the location of the predicted tears. All the other elements with more than 5% strain below the
stress FLC are shown in green, except for the few elements in the binder that are under compressive means stress, and are shown in
blue color. The predicted tears from the Stress FLD exactly match the location and orientation of the tear observed in tryout. This
kind of correlation is not uncommon, with additional examples of this type from other die tryout applications reported in
Stoughton and Yoon (24).
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The second example of application of the Stress FLD has two important distinctions from the previous one. In the previous
example, we show how the Stress FLD can help identify and avoid problems in physical tryout. This has the benefit of reducing the
cost of physical testing and correcting for any necessary product changes earlier in the product design process, which is always less
costly. In this example, we are going to demonstrate that we can utilize the Stress FLD not only in the early design stages of FEM
simulation, but also during physical tryout. More importantly, this example will demonstrate how we can use the Stress FLD to
achieve robust manufacturing of more complex designs. We will do this by applying stress analysis to the Toyota rear quarter panel
problem discussed by Ishigaki and described in Figures 5 and 6.
As explained in the previous section of this chapter, Ishigaki was faced with a torn panel during early tryout of the stamping
process at a strain below the forming limit of the metal, as illustrated in Figure 5. By measuring the strain path, he was certain that
the failure was caused by the strain crossing a dynamic Strain FLC, but he would not have been able to confirm this conjecture except
for the fortuitous conditions of the strain path, which allowed his engineers to measure a snapshot of the dynamic strain limit, as
illustrated in Figure 6. This measurement not only confirmed why the failure was occurring in early tryout, but also helped the
engineers see an opportunity to stretch the metal in the critical area along a path that could safely reach a strain much higher even
than the Strain FLC for the as-received condition. It was also pointed out in the previous section that this high stretch is highly
desirable for purposes of product quality. The problem is, however, that the method used in Ishigaki’s study is dependent on the
fortuitous conditions of the strain path involved in this particular case study, and apparently was too rare to be repeated in the last
35 years.
As described in Stoughton and Yoon (24), we can calculate the stress conditions for the two strain paths shown in Figure 6 and
compare them to the Stress FLC calculated from the Strain FLC for the as-received condition to obtain the results illustrated in
Figure 15. In this figure, the black curve is the Stress FLC. The blue line ending at the black point shows the calculated loading path
during the first draw die. The black dashed line shows the expanded yield surface at the end of the first draw. In early tryout, the
continuation of the strain path shown by the red line in Figure 6 is calculated to be the result of the stress path shown by the red line
in Figure 15. This path starts plastic deformation when the stress rises to the point on the expanded yield surface at the start of the
red line, and ends at the red point above the Stress FLC, explaining the observed failure. At the conclusion of tryout, the contin-
uation of the strain path shown by the green dashed line in Figure 6 is calculated to be the result of the stress path shown by the
green line in Figure 15. This path also starts plastic deformation when the stress rises to the point on the expanded yield surface at
the start of the green line, and ends at the green point below the Stress FLC, explaining why this remarkably high level of net strain
showed no sign of necking and the Toyota engineers decided to proceed to production.
This example shows that we can explain both the failure below the ‘static’ Strain FLC and the safe strain condition above the
‘static’ Strain FLC based solely on the Stress FLC calculated from the single ‘static’ Strain FLC. Unlike the method used by
Ishigaki 35 years ago, there is no need to measure any snapshots of the dynamic Strain FLC, or to wait for special circumstances
where one might be able to do this, which apparently happens too infrequently to be useful. But now, using the single Stress
FLD as the only forming-limit criterion, we can safely stretch metal to levels of strain that would once have been considered
impossible and, at the same time, avoid necking conditions that are not predicted by the old method of treating the Strain FLC
as a static limit.
Figure 15 Calculated stress conditions corresponding to the two strain paths and Strain FLC shown in Figure 6. The dashed line shows the location of
the yield surface at the end of the first draw at the start of the first cam restrike operation.
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1.04.4 Summary and Conclusions
In this chapter, we have described and compared two approaches to describe the necking limit for sheet metal deformation. The
traditional approach is to describe this forming limit in terms of the net plastic strain. While this approach is only valid for linear
strain paths, or more specifically, only for the strain paths involved in the measurement of the strain limit, the approach has been
widely adopted by industry with considerable success. However, this success is largely due to the dominance of linear or nearly
linear strain paths within a single stamping process.
It is well known that the traditional approach using the Strain FLD does not apply to the analysis of secondary forming processes.
This failure is due to the intrinsic nonlinearity of multistage forming operations. However, the Strain FLD also does not apply in
certain regions of the stamping within a single stamping process. While the majority of the forming panel usually follows a linear
strain path, corner areas of deeply drawn panels experience significant change in strain path as the metal flows from the binder into
the die wall area. In addition, the sequence of tool contact during the stamping of a panel with geometric features also continuously
or abruptly drives changes in strain path. Consequently, the Strain FLD does not apply to these affected areas.
This chapter also described a new approach for predicting necking in sheet metal deformation, based on stress metrics. The
utility of these diagrams is demonstrated in lab tests and measurements of the dynamic nature of the Strain FLC under nonlinear
loading conditions, where it is shown that the forming limit in terms of stress appears to be static. This interpretation is also
supported by all the theoretical models traditionally used to describe Strain FLC. In addition to a static Stress FLC defined in
terms of principal stresses in a Stress FLD, this chapter also discusses other forms of equivalent stress diagrams, based on the EPS
or the yield stress, with an appropriate ordinate variable, such as the ratio of principal stresses, or the ratio of the principal plastic
strain rates. A particularly interesting Stress FLD is constructed as a polar diagram with EPS as the radius variable and the arc
tangent of the ratio of the principal plastic strain rates as the angle. This so-called PEPS FLD has similarities to the traditional
Strain FLD, but unlike the latter, has a static FLC. The chapter includes two examples of applications of the Stress FLD and
limitations of the Strain FLD that demonstrate the practical advantages of the Stress FLD to avoid necking in complex metal
stamping processes, as well as the ability to safely stretch metal beyond the limits suggested by the traditional view of a static
Strain FLC.
We conclude this section with a list of other factors that affect necking and tearing during metal deformation that in general
should be accounted for to improve the reliability of the determination of formability limits. One of these factors, which is a caveat
of the dynamic nature of the Strain FLC, is that the measured Strain FLC is strictly limited to the strain path involved in the
experiments used to determine it. The two most commonly used methods for measuring the Strain FLC are the Nakajima Test,
which involves stretching specimen strips of various widths over a 100-mm hemispherical punch, and the Marciniak Test, which
involves stretching similar strips by a 100-mm cylindrical punch. In the latter test, a metal carrier blank with a hole cutout centered
on the cylindrical punch is placed between the sheet strip and punch to facilitate stretch of the specimen on the punch face through
the lightly constrained expansion of the hole in the carrier blank. Not surprisingly, these two tests involve different strain paths,
resulting in systematic differences in the measurement of the Strain FLC by the two methods. Leppin, Li, and Daniel (25) describe
a stress-based method to account for the nonlinearity in the strain paths in these two tests and obtain a corrected Strain FLC that
applies to linear strain paths. This FLC can then be used to determine the Stress FLC for nonlinear strain paths.
Other factors affecting or confusing the prediction of necking is the influence of curvature (26), cyclic bending and unbending
(27), fracture (28,29), and material anisotropy (30). The sited references provide a detailed discussion of these issues and methods
to incorporate their effects in the forming limit criteria.
References
1. Keeler, S. P.; Backhofen, W. A. ASM Trans. Q. 1964, 56, 25–48.

2. Goodwin, G. M. SAE paper 680093, 1968.
3. Graf, A. F.; Hosford, W. F. Metall. Trans. A 1993, 24, 2503–2512.
4. Nakazima, K.; Kikuma, T.; Hasuka, K. Yawata Tech. Rep. 1968, 264, 8517–8530.
5. Ishigaki, H. Mechanics of Sheet Metal Forming. In Koistinen, D. P.; Wang, N. M., Eds., 1977; pp 315–333.
6. Kleemola, H. J.; Pelkkikangas, M. T. Sheet Met. Ind. 1977, 63, 591–599.
7. Arrieux, R.; Bedrin, C.; Boivin, M. In Proceedings of the 12th Biennial Congress of the IDDRG, 1982; pp 61–71.
8. Stoughton, T. B. Int. J. Mech. Sci. 2000, 42, 1–27.
9. Ghosh, A. K.; Laukonis, J. V. In Proceedings of the 9th Biennial Congress of the IDDRG, 1976.
10. Hill, R. Proc. Roy. Soc. London A 1948, 193, 281–297.
11. Hill, R. J. Mech. Phys. Solids 1952, 1, 19–30.
12. Storen, S.; Rice, J. R. J. Mech. Phys. Solids 1975, 23, 421.
13. Zhu, X.; Weinmann, K.; Chandra, A. J. Eng. Mater. Tech. 2001, 3, 329–333.
14. Hutchinson, J.; Neale, K. Mechanics of Sheet Metal Forming. In Koistinen, D. P.; Wang, N. M., Eds., 1977; pp 127–153.
15. Hutchinson, J.; Neale, K. Mechanics of Sheet Metal Forming. In Koistinen, D. P.; Wang, N. M., Eds., 1977; pp 269–285.
16. Marciniak, Z.; Kuczynski, K. JMPS 1967, 9, 609–620.
17. Stoughton, T. B.; Zhu, X. Int. J. Plast. 2004, 20, 1463–1486.
18. Zeng, D.; Chappuis, L.; Xia, Z. C.; Zhu, X. SAE paper, 2008-01-1445, 2008.
19. Stoughton, T. SAE paper, 2002-01-0157, 2002.
20. Stoughton Int. J. Plast. 2002, 18, 687–714.
21. Barlat, F.; Brem, J.; Yoon, J. W.; Chung, K.; Dick, R.; Lege, D.; Pourboghrat, F.; Choi, S.; Chu, E. IJP 2003, 9, 1297–1319.
www.iran- mavad.com
22. Yoshida, K.; Kuwabara, T.; Kuroda, M. Int. J. Plast. 2007, 23, 361–384.
23. Stoughton, T. B.; Yoon, J. W. Numisheet. In Conference Proceedings; Chung, K., et al., Eds.; AIP, 2011; pp 15–34.
24. Stoughton, T. B.; Yoon, J. W. Int. J. Solids Struct. 2012, 49, 3616–3625.
25. Leppin, C.; Li, J.; Daniel, D. Numisheet. In Conference Proceedings; Hora, P., Ed.; AIP, 2008; pp 217–221.
26. Tharrett, M.; Stoughton, T. SAE 2003-01-1157, 2003.
27. Auto-Steel Partnership. Enhanced Formability Project Report, 2003. www.a-sp.org.
28. Wierzbicki, T.; Bao, Y.; Lee, Y. W.; Bai, Y. Int. J. Mech. Sci. 2005, 47, 719–743.
29. Stoughton, T. B.; Yoon, J. W. Int. J. Plast. 2011, 27, 440–459.
30. Stoughton, T. B.; Yoon, J. W. Int. J. Mech. Sci. 2005, 47, 1972–2002.
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1.05 Sheet Bulge Testing
T Hallfeldt, Ford Werke GmbH, Köln, Germany
W Hotz, Novelis Innovation Centre, Sierre, Switzerland
C Leppin, Suisse Technology Partners Ltd., Neuhausen am Rheinfall, Switzerland
S Keller, Hydro Aluminium Research & Development, Bonn, Germany
H Friebe, GOM mbH, Braunschweig, Germany
ET Till, voestalpine Stahl GmbH, Linz, Austria
R Müller, Fraunhofer-Institut für Werkzeugmaschinen und Umformtechnik IWU, Chemnitz, Germany
M Vu!ceti"c, Leibniz Universität Hannover, Garbsen, Germany
H Vegter, Tata Steel Research, Development & Technology, CA Ijmuiden, The Netherlands
1.05.2 Bulge Test Equipment and Specimens 85
1.05.2.1 Bulge Test Principle 86
1.05.2.2 Bulge Test Equipment 86
1.05.2.3 Test Specimen 87
1.05.2.4 Strain Rate Effects in Bulge Test 88
1.05.3 Measurement Equipment 89
1.05.3.1 Pressure Measurement 89
1.05.3.2 Deformation Measurement 89
1.05.4 Stress–Strain Curve Calculation 89
1.05.4.1 True Stress–True Strain Calculation 89
1.05.4.2 A Simple Approach to Determine Uniaxial Stress–Strain Curve from a Bulge Test 91
1.05.5 Summary 92
1.05.6 Acknowledgments 93
References 93
1.05.1 Introduction
Numerical forming simulations require accurate material parameter models, including true stress–true strain curves for the
reliable prediction of sheet metal–forming behavior. Uniaxial tension tests are usually accepted as a standardized testing
procedure to determine the required material parameters. However, due to the uniaxial loading condition that is present
during a tension test, only a limited strain range is considered when determining the true stress–true strain curve. To extend
the curves to cover higher true strains in actual forming operations, several empirical functions are available and are used to
extrapolate the measured and calculated data, as shown in Figure 1. The tensile test data are valid up to uniform elon-
gation, which typically corresponds to a true strain value of 0.2, depending on the material grade. It is obvious that the
extrapolation formulas currently in use lead to a spread of the possible hardening curves beyond the measured tensile
test data.
The bulge test can be used to extend the validity of the hardening curve. It enables the use of a much larger strain range
under biaxial loading conditions. In comparison to extrapolations from uniaxial tensile test data, smaller variations in
extrapolated stress values at a strain equal to 1 are found while using different extrapolation methods, as shown in Figures 1
and 2 (1,2).
Although the bulge test has been a recognized testing method for several years (1–7), experts are still considering the test
conditions and the evaluation of material parameters from the measurement results. Thus, application of the test has not been
widespread in the past. It was essential to standardize the test conditions, the measuring procedures, and the test evaluation
algorithms (1,2).
1.05.2 Bulge Test Equipment and Specimens
The advantage of the bulge test is that it is a nearly frictionless and biaxial testing procedure. In this test sheet material, behavior will
be characterized in terms of formability (in pure stretching). Furthermore, it is possible to determine both a yield locus point as well
as the material’s strain-hardening behavior. By knowing the actual thickness in the bulge dome, the curvature of the actual bulge,
and the pressure of the fluid, the true stress–true strain curve can be calculated. Tactile measurement systems can be used to
determine the curvature, although using optical measurement systems provides more accurate results (1).

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86 Sheet Bulge Testing
Figure 1 True stress–true strain curves based on tensile test data, with several extrapolations.
Figure 2 True stress–true strain curves based on bulge test data, with several extrapolations.
1.05.2.1 Bulge Test Principle

A circular blank is clamped at its flange in a suitable tool between the die and the blank holder. A bulge is formed by building up
pressure with a fluid, usually oil, until tearing of the specimen occurs (Figure 3).
The pressure of the fluid is constantly measured during the test, while the specimen’s deformation is recorded by an optical
measuring system. By monitoring and measuring the recorded deformations, the local curvature and the true principal strains at the
apex of the dome are realized.
1.05.2.2 Bulge Test Equipment

The principles of the test equipment, including the optical measurement system, the location of lock beads, and the pressure
measurement system, are shown in Figures 3 and 4.
During the test, the optical system measures (without contact) the X, Y, and Z coordinates of the grid points on the bulging
surface of the specimen. Based on these coordinates, the principal true strains of ε1 and ε2 for each point of the selected area and the
curvature radius r for the apex of the dome are calculated. Note that any movement of the test piece between blank holder and die
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Sheet Bulge Testing 87
Figure 3 The principle of the bulge test.
Deformation
measurement
system
ddie
R1
t0 p
Lock
Fluid bead
Pressure
measurement Piston
Sealer
system
d BH
Figure 4 Principle drawing of a test rig.
should be prevented. During the test, the bulge pressure is typically acting on parts of the blank holder to reduce the effective blank
holder force. This must be considered when defining the necessary blank holder force. Furthermore, the fluid should be in contact
with the blank surface without any air remaining to prevent energy storage by compressed air during the test, which leads to higher
energy release and greater oil splashing at failure. A lock bead is located between the blank holder and the die. The lock bead
geometry should be designed in a manner that prevents wrinkling or premature bulging of the blank while closing the tool, and also
prevents the blank from sliding during the test.
With the assumption of incompressibility of the material during plastic deformation, the thickness strain ε3 and the actual
thickness of the blank can be calculated from the measured principal strains. Furthermore, assuming the stress state of a thin-walled
spherical pressure vessel at the apex of the dome, the true stress is calculated from measurements of the fluid pressure, current
thickness, and curvature radius.
Glass plates in front of the lenses and the illumination unit are recommended to protect the optical measuring system from
splashing fluid due to blank failure at the end of the test.
1.05.2.3 Test Specimen

The circular flat test piece is clamped between the blank holder and the die to prevent material flow. The preparation of the blank
does not influence the results as long as the surface of the test piece is not damaged by scratches or polishing. For optical full-field
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Figure 5 Typical measurement images: Left side: full image size; right side: enlarged local area with mathematical subsets (facets) for the calculation of
surface point. Reproduced from Keller, S.; Hotz, W.; Friebe, F. Yield Curve Determination Using the Bulge Test Combined with Optical Measurements;
IDDRG, 2009; pp 319–330.
measurement devices, the grid must fulfill two objectives – determination of the specimen’s surface curvature radius as well as the
strain calculation of the material deformation. Deterministic grids (such as squares, circles, or dots) should have a strong contrast
and must be applied without any notch effect and/or change in microstructure. Some common application techniques include
electrochemical etching, photochemical etching, offset printing, and grid transfer. Stochastic (speckled) patterns can be applied by
spraying paint on the test piece surface (Figure 5).
1.05.2.4 Strain Rate Effects in Bulge Test

Almost all bulge test equipment contain constant fluid volume rates during the test. This typically leads to an increase in the strain
rate at the center of the test specimen and can influence the results, especially when strain-rate–sensitive material grades are tested.
Figure 6 shows an example of this condition, where high strain rates lead to increased stress and different slopes of the stress–
strain curve, especially in the range between ε ¼ 0.1 and ε ¼ 0.5. As long as the test cannot be conducted with the recom-
mended constant strain rate of 0.05 s'1, a constant forming velocity of the punch or fluid should be guaranteed. In order to avoid
significant influence on the biaxial stress–strain curve of temperature-sensitive or strain rate–sensitive materials, the bulge test
should be conducted in 2–4 min. This time frame guarantees slow and acceptable strain rates, as well as a cost-effective testing
duration (8).
700 0.8
Material: mild steel DX54,1.5 mm
600 r 1 = 30 mm 0.7
r 2 = 10 mm
0.6
500
Strain rate dε /dt [1/s]
True stress (MPa)
0.5
400
10s (test duration)
0.4
300
0.3
200
0.2
100 0.1
150s (test duration)
0 0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
True strain ε (–)
Figure 6 Bulge test curves, calculated at different strain rates.
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1.05.3 Measurement Equipment

1.05.3.1 Pressure Measurement
The pressure of the fluid in the chamber may be measured indirectly or directly. For indirect pressure measurement, a load cell
located at the punch will detect the force of the punch during the movement. The pressure can be calculated by dividing the punch
force by the punch area.
Direct pressure measurement in the bulge chamber is recommended, but consider that the load range of the pressure sensor is
aligned with the pressure to be measured in order to reduce the error of measurement.
1.05.3.2 Deformation Measurement

To determine the radius of curvature r and the true principal strains ε1 and ε2, an optical deformation field measurement system
with two or more cameras should be used, and the measurement area should be half the size of the die radius or larger. The optical
measurement system will provide certain images at a given time interval. In the last image before failure, the area of the dome with
the highest deformation is selected and defined as the position at which to determine the true biaxial stress and the true thickness
strain ε3. To obtain a stable radius of curvature of the dome, a best-fit sphere can be calculated based on a selected area of points. For
this selection, a radius r1 is defined around the apex of the dome in the last image before bursting, and the fit is performed for all
forming stages with the same selection of points (Figure 7). For robust values of the true strain and thinning in the apex, the average
value of a number of selected points is taken. A second evaluation area is defined by a radius r2 in a similar manner (Figure 7). Based
on this procedure, for every forming stage (image) the radius of curvature, the average thickness strains, as well as the corresponding
thickness and stress values at the dome apex are calculated. This evaluation can be carried out for different r1 and r2 values. For
a good convergence and robust values, the following ranges of r1 and r2 are recommended:
r1 ¼ ð0:125 ) 0:025Þddie
r2 ¼ ð0:05 ) 0:01Þddie
1.05.4 Stress–Strain Curve Calculation

1.05.4.1 True Stress–True Strain Calculation
For the calculation of the biaxial stress–strain curves, a simple membrane stress state of a thin-walled spherical pressure vessel is
assumed at the center of the blank. This implies the following simplifications:
1. An equi-biaxial stress state:
s1 ¼ s2 ¼ sB
2. The representation of the curvature by the mean curvature radius:

" #'1
1
r¼ ð1=r1 þ 1=r2 Þ
2
As a result, the biaxial true stress can be calculated according to the following equation:
rp
sB ¼
2t
Figure 7 Choices of r1 and r2 for calculation of true stress and true strain for each forming stage. Reproduced from Keller, S.; Hotz, W.; Friebe, F.
Yield Curve Determination Using the Bulge Test Combined with Optical Measurements; IDDRG, 2009; pp 319–330.
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using the fluid pressure p, the curvature radius r, and the current thickness t, with
t ¼ t0 expðε3 Þ
Assuming a plastic incompressible deformation of the material and neglecting elastic strains, the total thickness strain for the
calculation of the actual thickness can be approximated by the total major and minor true strain with the following equation:
ε3 z ' ε1 ' ε2
Based on the plastic work principle, the biaxial stress–strain curve is a function of the plastic thickness strain:
& '
pl
sB 'ε3
Assuming an isotropic linear elastic material behavior and plastic incompressibility, the plastic thickness strain is then given by:
pl 1'n
ε3 ¼ 'ε1 ' ε2 þ 2 sB
E
For the elasticity modulus E and the Poisson ratio n, literature values are generally sufficient to subtract the elastic contribution;
for example, E ¼ 210 GPa and n ¼ 0.3 for steel, and E ¼ 70 GPa and n ¼ 0.33 for aluminum alloys.
The ratio of die diameter to thickness should be reasonably high to ensure a near-membrane stress state in the test piece, as well
as a negligible bending influence (9). For die diameter to thickness ratios lower than 100, it is recommended to check that the
bending strains are relatively small, as compared to the actual thickness strain result ε3, by using the following estimate for the
bending strains:
" #
t0
εbending z 'ln 1 ' expðε3 Þ
2r
If these bending strains are significant, an integrated correction of the corresponding error can considerably improve the results
(8,9), as demonstrated in the comparison of test results with two different bulge test diameters of the same material, as shown in
Figure 8.
Figure 8 True stress–true strain curves from bulge testing, with two different setups for die diameter and corresponding r1 and r2 values. Curves
are calculated without bending and elastic strain correction (above) and with bending and elastic strain correction (below).
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1.05.4.2 A Simple Approach to Determine Uniaxial Stress–Strain Curve from a Bulge Test
From the bulge test, equi-biaxial stress–strain curves are obtained where the average of the major and minor stress from the bulge
tests is plotted against the absolute value of the plastic true thickness strain. Usually, the true stress–true strain curve, determined
from uniaxial tensile test data in the rolling direction (RD), is used as a reference for the calculation of the stress points of the yield
locus. By comparing the curves of the stress–strain data of the equi-biaxial stress state with the uniaxial reference curve, the equi-
biaxial stress point can be calculated. A convenient way to characterize the yield locus is the calculation of stress ratios that is relative
to the uniaxial stress at the RD. The equi-biaxial stress ratio enables us to transform the equi-biaxial stress–strain curve to an
equivalent stress–strain curve. This last curve provides work-hardening data at strains higher than the uniform strain of the tensile
test. In order to use this approach, some assumptions have been made: the calculation is based on isotropic hardening, the yield
locus shape does not change with the strain, and the work hardening is independent from the strain path (loading path).
Furthermore, the loading path and strain path of the test scenario are constant, and the strain rate and temperature of the bulge test
are close to the strain rate and temperature of the tensile test. The equivalent strain definition is based on the plastic work principle:
sf $vεE ¼ s1 $vε1 þ s2 $vε2 þ s3 $vε3
where vεE means the equivalent plastic strain increment; sf is the plastic flow stress; s1, s2, and s3 are the principal stresses in the
principal directions 1, 2, 3; and vε1, vε2, and vε3 are the corresponding plastic strain increments. With s2 ¼ s3 ¼ 0 for uniaxial tensile
tests, the following equation can be used:
sf $vεE ¼ s1 $vε1
For the bulge test, we assume that the two in-plane stresses are equal to s1 ¼ s2 ¼ sB and s3 ¼ 0. By using the plastic incom-
pressibility condition, the following equation can be used:
sf $vεE ¼ sB $vε1 þ sB $vε2 ¼ 'sB $vε3 ¼ sB $jvε3 j
Assuming isotropic hardening means that a fixed ratio exists between uniaxial stress and the plastic flow stress fun ¼ s1/sf, and
a fixed ratio also exists between the biaxial stress and the plastic flow stress fbi ¼ sB/sf. The uniaxial stress–strain curve in the RD is
the reference for the equivalent stress–strain curve, so by definition, fun ¼ s1/sf ¼ 1. A combination of the equations leads to the
following definition for the equivalent strain increment:
s1 s3
vεE ¼ $vε1 ¼ $jvε3 j5vεE ¼ 1$vε1 ¼ fbi $jvε3 j
sf sf
Hence, by the definition of fun ¼ 1 for the uniaxial tensile test in the RD, the equivalent strain is equal to the axial strain. The
equivalent strain for the bulge tests is obtained through integration of the equation. The assumption of isotropy (i.e., a constant fbi)
leads to the following equation for bulge tests:
Z εE Z jε3 j
vεE ¼ fbi $jvε3 j5εE ¼ fbi jε3 j
0 0
The biaxial stress–strain curve from bulging can be transformed into an equivalent stress–strain curve for bulging. As the
calculation of fbi is the fixed ratio between the equi-biaxial stress and the uniaxial stress in the RD, it is assumed that the yield surface
is defined by stress points at constant equivalent strains. Here, the true plastic strain at uniform elongation of the tensile tests in the
RD is a possible choice for a reference value for the equivalent strain:
εE'ref ¼ ε1'UE
This is considered to be the last valid point of the true stress–true strain curve of the tensile test. Accordingly, the stress at the
uniform strain of the tensile tests is used as the reference flow stress sf-ref ; namely, the ultimate tensile strength has been transformed
to a true stress. Finding the pairs of stresses and strains in the bulge test curve that satisfy the following conditions derived from the
" Z εE #
above equation vεE leads to the corresponding reference values of the bulge test:
0
( (
sB'ref $(ε3'ref ( ¼ sf 'ref $εE'ref
Since the bulge test curve is given in discrete values, there will not be a pair of stresses and strains that perfectly satisfy the
condition above. Therefore, the point m in the bulge test data matches the following condition:
( (
sB;m $(ε3;m ( + sf 'ref $εE'ref
and
( (
sB;mþ1 $(ε3;mþ1 ( , sf 'ref $εE'ref
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Figure 9 Example of the uniaxial stress strain and the equi-biaxial stress–strain curve of a material, including the biaxial stress calculation of the
reference point and the hardening curve, based on scaled bulge test results.
where m is the index of the stress and strain data of the bulge test curve. The requested reference stress of the bulge test can now be
computed by simple linear interpolation:
s 's $ %
sB'ref ¼ sB;m þ ( B;mþ1 ( B;m ( ($ sf 'ref $εE'ref ' sB;m $ε3;m
sB;mþ1 $(ε3;mþ1 ( ' sB;m $(ε3;m (
The value of the biaxial stress ratio is obtained by

sB'ref
fbi ¼
sf 'ref
with
Z εE Z jε3 j
vεE ¼ fbi $jvε3 j5εE ¼ fbi jε3 j
0 0
and, with the definition of the biaxial stress factor, the bulge test curve can be transformed into an equivalent strain–stress curve
(Figure 9). When combined with uniaxial stress–strain curves from tensile tests, the transformed curve can be used to generate
a hardening curve with data extrapolated beyond strains at a uniform elongation.
The described method is a single proposal for handling the stress–strain data from a bulge test under the assumption of isotropic
hardening. There are more general methods available, such as those proposed by Kuwabara et al. (10), Barlat et al. (11), Yoon (12), and
Sigvant et al. (5), which are based on total plastic work and are not restricted to purely isotropic hardening. With the present method,
the assumption of isotropic hardening can be tested by comparing the equivalent stress–strain curve derived from the bulge test and
the uniaxial stress–strain curve. When these two curves deviate, then the isotropic hardening assumption is not valid.
1.05.5 Summary
In order to test sheet metals under biaxial loading conditions, the bulge test was chosen for the following reasons:
l The test conditions are nearly frictionless.
l The strain range for the determination of stress–strain curves is much larger in comparison to the uniaxial tensile test.
l Depending on the material grade used, the maximum strain is three to six times higher.
Therefore, the bulge test, combined with an online strain measurement system, is an excellent method for reliable testing of
a material’s work hardening, as well as the determination and provision of significantly improved yield curves for finite-element
(FE)-forming simulations.
Moreover, test facilities and test equipment are commercially available. The bulge test has been known for many years, but a first
standardization (ISO-standard) will be finalized soon. To improve the accuracy of the test, an optical measurements system is
recommended. This optical system will record the evolution of the deformation on the surface during the test, which can then be
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used to calculate the thickness and curvature of the dome over time. When combined with the measured pressure in the chamber, it
is possible to determine a true stress–true strain curve. The usage of the hydraulic bulge test is recommended for use with a die-to-
thickness ratio of ddie/t0 , 33. The testing velocity should be limited to reduce deviations for strain rate–sensitive materials. The test
velocity should ideally lead to strain rates that are close to the standard tensile test. To calculate the curvature and the thickness of the
dome, a simple best-fit sphere approach is suggested. An alternative approach that leads to good results is a biquadratic paraboloid
surface approximation (13), which will also be described in the ISO standard, which is currently being prepared (14). Finally, an
approach to investigate and calculate true stress–true strain curves is discussed, making the biaxial stress–strain curves comparable
to the uniaxial tensile test curves. By using this method, improved hardening curves will be obtained as input for the finite-element
method (FEM) simulations.
1.05.6 Acknowledgments
The harmonization and standardization work of the bulge test with optical measurement systems described in this chapter was
worked out at the German IDDRG working group ‘bulge test.’ The authors are members of this group and would like to thank all
group members for their contributions.
References
1. Keller, S.; Hotz, W.; Friebe, F. Yield Curve Determination Using the Bulge Test Combined with Optical Measurements; IDDRG, 2009; pp 319–330.
2. Hallfeldt, T.; Keller, S.; Staud, D.; Merklein, M.; Güner, A.; Brosius, A.; Geisler, S. Vereinheitlichung der Versuchsbedigungen für die Fließkurvenermittlung in der hydraulischen
Tiefung. Fortschritte der Kennwerteermittlung für Forschung und Praxis, 2009, ISBN: 978-3-517-00769-7, pp 129–136.
3. Ranta-Eskola, A. J. Use of the Hydraulic Bulge Test in Biaxial Tensile Testing. Pergamon Press Ltd. Int. J. Mech. Sci. 1979, 21, 457–465.
4. Dziallach, S.; Bleck, W.; Hallfeldt, T. Sheet Metal Testing and Flow Curve Determination under Multiaxial Condition. Adv. Eng. Mater. 2007, 9 (11), 987–994.
5. Sigvant, M.; Mattiasson, K.; Vegter, H.; Thilderkvist, P. A Viscous Pressure Bulge Test for the Determination of a Plastic Hardening Curve and Equibiaxial Material Data.
Int. J. Mater. Form. 2009, 2, 235–242.
6. Nasser, A.; Yadav, A.; Pathak, P.; Altan, T. Determination of the Flow Stress of Five AHSS Sheet Materials (DP600, DP780, DP780-CR, DP780-HY and TRIP780) using the
Uniaxial Tensile Test and Viscous Pressured Bulge (VBP) Tests. J. Mater. Process. Technol. 2010, 210, 429–436.
7. Koc, M.; Billur, E.; Cora, ÖN. An Experimental Study on the Comparative Assessment of Hydraulic Bulge Test Analysis Methods. Mater. Des. 2011, 32, 272–281.
8. Leppin, C.; Lange, C.; Till, E.; Daniel, D. Evaluation of the Hydraulic Bulge Test for Improved Material Hardening Modeling, Submitted for Publication at 5th Forming
Technology Forum, June 5th – 6th 2012, Zurich, Switzerland.
9. Behrens, B. -A.; Bouguecha, A.; Peshekodov, I.; Götze, T.; Huinink, T.; Vucetic, M.; Friebe, H.; Möller, T. Numerical Validation of Analytical Biaxial True Stress – True Strain
Curves from Bulge Test. 8th International Conference and Workshop on Numerical Simulation of 3D Sheet Metal Forming Processes, Seoul, South Korea, 2011, ISBN: 978-0-
7354-0944-6, pp 107–114.
10. Kuwabara, T.; Van Bael, B.; Iizuka, E. Measurement and Analysis of Yield Locus and Work Hardening Characteristics of Steel Sheets with Different r-Values. Act. Mat. 2002, 20,
3717–3729.
11. Barlat, F.; Aretz, H.; Yoon, J. W.; Karabin, M. E.; Brem, J. C.; Dick, R. E. Linear Transformation-Based Anisotropic Yield Functions. Int. J. Plasticity 2005, 21, 1009–1103.
12. Yoon, J. H.; Cazacu, O.; Yoon, J. W.; Dick, R. E. Earing Predictions for Strongly Textured Aluminium Sheets. Int. J. Mech. Sciences 2010, 52, 1563–1578.
13. Volk, W.; Heinle, I.; Grass, H. Accurate Determination of Plastic Yield Curves and an Approximation Point for the Plastic Yield Locus with the Bulge Test. In Proceedings of the
10th International Conference on Technology of Plasticity; ICTP, 2011; pp 799–804.
14. ISO/CD 16808. Metallic Materials d Sheet and Strip d Determination of Biaxial Stress-Strain Curve by Means of Bulge Test with Optical Measuring Systems, in press.
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1.06 Biaxial Stress Testing Methods for Sheet Metals
T Kuwabara, Tokyo University of Agriculture and Technology, Koganei-shi, Tokyo, Japan
1.06.2 Biaxial Compression Test 96
1.06.3 Biaxial Tensile Testing Method Using a Cruciform Specimen 96
1.06.3.1 Introduction 96
1.06.3.2 Geometry of the Cruciform Specimen 96
1.06.3.3 Method of Strain Measurement 97
1.06.3.4 Method of Measurement of Biaxial Stress–Strain Curves 98
1.06.3.5 Testing Machine 98
1.06.3.6 Methods of the Measurement of a Yield Locus and Examples of Test Results 99
1.06.3.6.1 Linear Stress Path Method – Method for Measuring a Contour of Plastic Work 99
1.06.3.6.2 Use of an Abrupt Strain Path Change for Detecting a Yield Vertex and Subsequent Yield Surface 99
1.06.3.7 Factors Affecting the Maximum Equivalent Plastic Strain Applicable to the Gauge
Area of a Cruciform Specimen 100
1.06.4 Combined Tension–Compression Testing Method 103
1.06.4.2 Testing Jigs and Specimen 103
1.06.4.3 Finite Element Analysis 103
1.06.4.4 Examples of Test Results 104
1.06.5 In-plane Stress Reversal Testing Method 104
1.06.5.2 Testing Jigs and Specimen 105
1.06.5.3 Examples of Test Results 105
1.06.6 Multiaxial Tube Expansion Testing Method 107
1.06.6.2 Tubular Specimen and Testing Machine 107
1.06.6.3 Stress and Strain Measurement 108
1.06.6.4 Determination of Biaxial Stress–Strain Curves 109
1.06.6.5 Material Modeling 109
1.06.6.6 Measurement of Forming Limit Curve 110
1.06.7 Combined Tension-Shear Testing Method 110
References 110
1.06.1 Introduction
Accurate prediction of the material behavior in sheet metal forming operations using numerical simulations, such as finite element
analysis (FEA), is strongly desirable, in order to minimize the time and cost required to design tool geometry and optimize forming
conditions. To improve the predictive accuracy of forming simulations, it is necessary to use a material model capable of accurately
reproducing the material’s deformation behavior (1,2).
Figure 1 shows a schematic illustration of the typical deformation modes found in sheet metal forming and their corresponding
stress states. Assuming that there is no normal stress applied to the sheet surface (plane-stress state), these are summarized as follows:
1. Stretching: stress state changes along the radial direction, from equibiaxial tension at the center to plane-strain tension at the die
profile.
2. Stretch flanging: stress state changes along the radial direction, from uniaxial tension at the hole edge to biaxial tension.
3. Drawing: a combination of tension in the radial direction and compression in the circumferential direction.
4. Bending: plane-strain tension (wide sheet) to uniaxial tension (narrow sheet) in the convex side, and plane-strain compression
(wide sheet) to uniaxial compression (narrow sheet) in the concave side.
Uniaxial tensile tests have been conventionally used to determine the mechanical properties of sheet metals. However, sheet
metals are generally subjected to combined stress states in press-forming operations, as Figure 1 demonstrates. Therefore, there seems
to be no rational reason to consider that the uniaxial tensile test is sufficient to determine a material model for sheet metals to perform
accurate sheet-metal-forming simulations. Biaxial stress tests are essential to determine an accurate material model for use in the FEA.
This chapter describes the material testing methods for measuring and quantifying the deformation behavior of sheet materials
under the biaxial stress states, which are shown in Figure 1. Examples of material test results and modeling results are also presented.

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96 Biaxial Stress Testing Methods for Sheet Metals
I. Stretching II. Stretch flanging
III. Drawing IV. Bending
Figure 1 Typical stress states in sheet metal forming. The markers B on the yield locus indicate the stress states that give plane-strain tension or plane-
strain compression.
The rolling (RD), transverse (TD), and thickness directions of an original flat sheet sample are defined as the x-, y-, and z-axes,
respectively, throughout this chapter.
1.06.2 Biaxial Compression Test
The biaxial compression test for sheet materials was performed by several researchers (3,4). Tozawa (4) performed the biaxial
compression tests using adhesively bonded sheet laminate specimens, and investigated the work-hardening behavior of both
annealed and prestrained sheet metals in the p-plane.
A disadvantage of the biaxial compression test is the difficulty of obtaining accurate stress–strain relations due to friction
between the specimen and compression platens. Moreover, when the plastic deformation mechanism of the material is influenced
by the hydrostatic component of stress (5), the yield locus shapes obtained from the biaxial compression test may differ from those
obtained from the biaxial tension test (6).
1.06.3 Biaxial Tensile Testing Method Using a Cruciform Specimen

1.06.3.1 Introduction
This section describes the testing method for measuring the biaxial stress–strain curves of sheet metals subject to biaxial tension at
an arbitrary stress ratio using a cruciform specimen made of flat sheet metals. The cruciform specimen introduced in this section has
the following features:
1. The slits provided in the arms of the specimen ensure superior homogeneity of stress at the gauge area, enabling the accurate
measurement of biaxial stress.
2. The specimen allows the measurement of elastoplastic deformation behavior of sheet metals at arbitrary stress or strain ratios.
3. The specimen is free from out-of-plane deformation, as encountered in the hydrostatic bulge testing method.
4. The specimen is easy to fabricate from a flat metal sheet using laser or water jet machining.
According to the FEA of the cruciform specimen (as introduced in Section 1.06.3.2), the error of stress measurement is estimated
to be less than 2% when using isotropic (von Mises) (7) and anisotropic yield functions (8) for material models, when the strain
measurement position is chosen as described in Section 1.06.3.3.
For other types of cruciform specimens and biaxial tensile testing methods proposed by other researchers, see (1) and (9).
1.06.3.2 Geometry of the Cruciform Specimen

Figure 2 shows the shape and dimensions of the cruciform specimen introduced in this section. The specimen shall be fabricated as
described below:
1. The specimen shall be cut from as-received flat-rolled sheet samples so that the arms are parallel to the RD and TD of the sheet
sample, except that the specimen sampling direction may be determined according to the agreement between the parties
involved.
2. For the fabrication of the specimen (including the machining of any slits), laser or water jet machining is recommended,
although any method demonstrated to work satisfactorily may be used.
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Biaxial Stress Testing Methods for Sheet Metals 97
3. The arm width B should be 30 mm or more with an accuracy of ) 0.1 mm, except when B may be determined according to the
agreement between the parties involved in transaction.
4. In principle, the thickness of a specimen shall be the same as that of the original sample, without any work done in the thickness
direction. When the material thickness a exceeds 8% of the arm width B, either the arm width B shall be increased in such
a manner that satisfies a+ 0.08B or the specimen’s thickness shall be reduced.
5. Seven slits per one arm shall be made. Specifically, one slit shall be made on the centerline (x- or y- axis) of the specimen with
positional accuracy of ) 0.1 mm, and three slits shall be made at an interval of B/8 with a positional accuracy of ) 0.1 mm on
each side of the centerline. The opposing slit ends shall be made at an equal distance from the centerline with a positional
accuracy of ) 0.1 mm. The distances BSx and BSy between the slit ends shall be made equal with a positional accuracy of
B ) 0.1 mm. All slits shall have the same length L ) 0.1 mm, and the relationship of B + L + 2B must be established. The slit
width wS should be worked as small as possible. See Figure 9.
6. The grip length C is considered to be sufficient if it can secure the specimen to the chuck of the biaxial tensile testing machine and
transmit the necessary tensile force to the specimen. The testing method length would be C ¼ B/2 to B.
1.06.3.3 Method of Strain Measurement

For the measurement of the nominal strain components, ex and ey, in the gauge area of the cruciform specimen, strain gauges, or
other methods that are equal in accuracy to the strain gauge shall be used.
Figure 3 shows the positions of strain gauges for measuring ex and ey. The strain gauges shall be mounted on the centerlines of the
specimens at (x, y) ¼ () (0.3–0.4)B, 0) for the tests with Fx , Fy, and at (x, y) ¼ (0, ) (0.3–0.4)B) for the tests of Fx + Fy.
4-R(0.004–0.1) B
a BSx
b wS
C
B x
L BSy
c
d
B /8
B
Figure 2 Shape and dimensions of a cruciform specimen. a: Gauge area; b: arm; c: grip; d: slit; BSx and BSy: distance between opposing slit ends; B: arm
width; C: grip length; L: slit length; wS: slit width.
Fy Fy
(0.6–0.8)(B/2) (0.6–0.8)(B/2)
Fx Fx Fx Fx
Fy Fy
B B
(a) (b)
Figure 3 Optimum position for the measurement of nominal strain components ex and ey: (a) A case of using one biaxial foil strain gauge and (b) a case
of using two uniaxial foil strain gauges. Note: These figures show the strain measurement position when Fx is equal to or larger than Fy. In case (b),
one of the strain gauges measures ex and the other measures ey.
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1.06.3.4 Method of Measurement of Biaxial Stress–Strain Curves

Using the measured values of tensile forces (Fx, Fy) and nominal strain components (ex, ey) in the x- and y-directions of the cruciform
specimen, respectively, the stress–strain curves in the x- and y-directions are determined. These curves are used to determine
contours of plastic work for the test material. See Section 1.06.3.6.1.
1. Calculate the original cross-sectional areas of a cruciform specimen perpendicular to the x- and y-axes, ASx and ASy, from
eqn [1]:
ASx ¼ a " BSy ; ASy ¼ a " BSx [1]
where BSx and BSy are the distance between the slit ends on the x- and y-axes, respectively.
2. Calculate the true stress components in the x- and y-directions, sx and sy, from eqn [2]:
Fx Fy $ %
sx ¼ ð1 þ ex Þ; sy ¼ 1 þ ey [2]
ASx ASy
3. Calculate the true strain components in the x- and y-directions, 3x and 3y, from eqn [3]:
$ %
3x ¼ lnð1 þ ex Þ; 3y ¼ ln 1 þ ey [3]
Figure 4 shows examples of the measured sx'3x and sy'3y curves for an aluminum alloy sheet.
4. Calculate the true plastic strain components in the x- and y-directions, 3px and 3py , from eqn [4]:
sx sy
3px ¼ 3x ' ; 3px ¼ 3y ' [4]
Ebx Eby
1.06.3.5 Testing Machine

Figure 5 shows the structural example of a servo-controlled biaxial tensile testing machine (10). The main body consists of the
frame, four actuators (hydraulic cylinders or servo motors) arranged in two orthogonal directions, a chuck connected to each
actuator, and one load cell installed in each axis. Opposing hydraulic cylinders are connected to common hydraulic lines so that
they are subjected to the same hydraulic pressure. The hydraulic pressure of each pair of opposing hydraulic cylinders is servo-
controlled independently. The displacements of opposing hydraulic cylinders are equalized using the pantograph-type link
mechanism proposed by Shiratori and Ikegami (11), so that the center of the cruciform specimen is always kept at the center of the
testing machine during biaxial tensile tests. This testing machine can control the stress ratio (10) or strain rate ratio (12) by means of
the actuators.
300 300
– – –
Eb y y y x x
Eb y x x
Eb x Eb x
/ MPa
/ MPa
200 200
x
– x –
x x
y
y
(uniaxial) (uniaxial)
100 100
,
, x
–
x
y y
0 0
0.00 0.01 0.02 0.03 0.00 0.01 0.02 0.03
x
, y x, y
(a) Nx : Ny 1:1 (b) Nx : Ny 2:1
Figure 4 Examples of sx'3x and sy'3y curves measured for the stress ratios, (a) sNx:sNy ¼ 1:1 and (b) sNx:sNy ¼ 2:1, in the biaxial tensile tests of
6000-series aluminum alloy sheet. The uniaxial tensile stress–strain curve in the RD of the same material is also shown for comparison. Ebx and Eby
are the slopes of the elastic part of the sx'3x and sy'3y curves, respectively.
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3 4 6
Figure 5 Example of a servo-controlled biaxial tensile testing machine. 1: Actuator; 2: center of the testing machine; 3: chuck; 4: load meter; 5:
link mechanism; 6: loading axis; 7: frame. Reproduced from Kuwabara, T.; Ikeda, S.; Kuroda, T. Measurement and Analysis of Differential Work Hardening
in Cold-Rolled Steel Sheet under Biaxial Tension. J. Mater. Process. Technol. 1998, 80/81, 517–523.
1.06.3.6 Methods of the Measurement of a Yield Locus and Examples of Test Results
1.06.3.6.1 Linear Stress Path Method – Method for Measuring a Contour of Plastic Work
The concept of the contour of plastic work in the stress space (13,14) is effective to evaluate the work-hardening behavior of the test
materials under biaxial tension. This concept was tested because, especially in the simulations of sheet metal forming, modeling the
work-hardening behavior of sheet metals as an average behavior over a certain amount of deformation range is more important
than determining an initial yield locus of the material.
Figure 6 shows a method for measuring a contour of plastic work of sheet metals. The stress–strain curve obtained from
a uniaxial tensile test along the RD of the material is selected as a reference datum for work hardening; the uniaxial true stress
s0 and the plastic work per unit volume W0 that corresponds to particular values of offset logarithmic plastic strains 3P0 are
determined. The uniaxial true stress s90 obtained from a uniaxial tensile test along the TD and the biaxial true stress
components (sx, sy) obtained from biaxial tensile tests are then determined at the same plastic work as W0. The stress points
(s0, 0), (0, s90), and (sx, sy) plotted in the principal stress space, form a contour of plastic work that corresponds to
a particular value of 3P0 . For a sufficiently small value of 3P0 , the corresponding work contour can be practically viewed as
a yield locus.
Figure 7 (15–18) shows examples of the contours of plastic work measured for different sheet metals, using the cruciform
specimens shown in Figure 2.
1.06.3.6.2 Use of an Abrupt Strain Path Change for Detecting a Yield Vertex and Subsequent Yield Surface
Yield surfaces are usually determined by probing in many different stress directions from the elastic region into the plastic
range (unloading–reloading method). By considering the possibility that a corner exists on the subsequent yield surface
at the point of loading, as predicted by crystal plasticity (19), Hecker (20) has argued that any such corner will be erased by
the unloading needed to probe the yield surface. The question of whether a vertex has formed on the yield surface is
important to the prediction of plastic instabilities (21–24). To avoid this effect of unloading, some authors have
used a zigzag loading path to study corners; such work has indicated the development of a yield surface vertex in some
materials (25).
Kuroda and Tvergaard (26) have proposed a new method for determining the shape of the subsequent yield surface in the
vicinity of a current loading point. They prescribe a proportional strain path until the loading point of interest has been reached,
and then prescribe an abrupt strain path that will cause the stress point to move quickly along the yield surface. This
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σ σ
σy σy
σx
σ σx
Wy
σ 90
Wx ε
p
p
ε
Wy σy
ε
p σx
σy
Wx
Wy p
ε
σ
σ0
σx
W0
W0 = Wx + Wy p
ε
p
ε0
Figure 6 Method for the measurement of a contour of plastic work.
determination can be performed without any unloading, which would be required if the subsequent yield surface was to be
determined by probing from the elastic region. As a result, this method is capable of detecting a yield vertex that is formed at the
point of loading.
Figure 8 shows the stress paths (thick lines) measured for abrupt strain path change that follows equibiaxial tension for (a)
a 6000-series aluminum alloy and (b) an SPCE (IF steel), using the cruciform specimen shown in Figure 2, in a closed-loop,
servo-controlled biaxial tensile testing machine (12). In the first step of straining, equibiaxial tension, D11 ¼ D22 ¼ a_ > 0, was
prescribed. At a nominal strain, e11 ¼ e22 ¼ 0.01, the prescribed strain rates were abruptly changed to the strain rate ratio, D22/
D11, as shown in the figure. The > markers indicate the accumulated equivalent (von Mises) plastic strain of D3p, which is
measured from the strain path change point; D3p increases as the stress point moves away from the strain path change point. It is
apparent that the stress paths for the abrupt strain path changes with the given D22/D11 cannot be nonyielding stress paths in the
elastic region. Therefore, we infer that a yield surface vertex is successfully detected in the figure, as clearly observed at the point of
loading. This idea is also supported by the fact that the value of D3p on the stress path is 0.002 at most. Note that the directions of
plastic strain rates, Dp, the short lines attached to the stress paths, are inclined to the forward direction of stress path, and deviates
a great deal from the normal to the stress path, which is regarded as a part of the subsequent yield surface in this testing method.
This tendency of the apparent nonnormality is very similar to the Taylor model prediction for a face-centered cubic poly-
crystalline material (Figure 5 in (26)).
Figure 8 also depicts a contour of plastic work determined for linear stress paths, indicated by the C markers, and the
subsequent yield loci determined by the unloading-reloading method, indicated by the markers, ,, B, and 6. The latter was
determined by probing in different stress directions from the elastic region. The first step of straining was prescribed by
D11 ¼ D22 ¼ a_ > 0. At nominal strains of e11 ¼ e22 ¼ 0.01, the specimen was unloaded with D11 ¼ D22 ¼ 'a_ until both loads in
the 1- and 2-directions became zero. The second step of straining was prescribed by constant nominal tensile stress ratios of
sNx:sNy ¼ 1:0, 4:1, 2:1, 3:2, 6:5, 12:11, 1:1, 11:12, 5:6, 2:3, 1:2, 1:4, and 0:1. Subsequent yield surfaces were determined as a group of
stress points, giving the same amount of plastic work for all the stress ratios; the levels of plastic work are indicated by
p
30 ¼ 0:0001ð,Þ; 0:001ð-Þ; and 0:005ðO Þ, which is the true plastic strain attained in the uniaxial tension test in the RD of the
p
material. As long as we look only at the subsequent yield surfaces determined by the unloading-reloading method with 30 ranging
from 0.0001 to 0.005, we have no apparent basis for choosing a particular one of them as the current yield surface that corresponds
to the strain path change point.
1.06.3.7 Factors Affecting the Maximum Equivalent Plastic Strain Applicable to the Gauge Area of a Cruciform Specimen
For the cruciform specimen shown in Figure 2, the arms are subjected to uniaxial tension, so that the test is finished at a time when
the nominal stress of the arm reaches the material tensile strength of the material. Accordingly, the maximum equivalent plastic
p
strain 3max applicable to the gauge area of the cruciform specimen can be estimated using the Considère condition for maximum
p
load in a strip in tension (27). 3max depends mainly on the stress ratio, the work-hardening exponent (n-value) of the test material,
the slit width of the cruciform specimen, and the anisotropy of the test material.
p
Figure 9(a) shows the effects of n-value on 3max for sx:sy ¼ 2:1 and 1:1 when wS/B ¼ 0.01. For materials having larger n-values,
p
3max becomes larger. This is because the material with larger n-value has a higher stress increase rate with the increase of the arm’s
plastic deformation, which in turn causes the increase in the normal stress acting on the gauge area.
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1.4 750
TS590 steel
1.2
600 pp
00
1.0
0.001
450 0.002
0.8 0.005
MPa
0
0.01
/
0.02
y
0.6
y/
Experimental ( 0 =0.04)
p 300 0.03
von Mises 0.04
0.4 0.05
Hill '48
150 0.06
Yld2000-2d (M=4)
0.2 0.07
Yld2000-2d (M=6)
0.08
Yld2000-2d (M=8) 0.09
0.0 0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 0 150 300 450 600 750
x / 0 x / MPa
(a) (b)
p
0 (Sheet): 0.001 0.002
p
0 (Tube) : 0.002 0.005 0.02 0.04 0.085
1.2
1.0 1.5
0.8
High cube
Experimental 1.0
0
0.6 Yld2000-2d
/
/
y
(M=12)
y
0.4 Low cube

0.5
Experimental
0.2 Yld2000-2d
(M=6)
0.0 0.0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 0.0 0.5 1.0 1.5
x
/ 0 x/ 0
(c) (d)
Figure 7 Examples of contours of plastic work measured for linear stress paths: (a) High-strength steel sheet with a tensile strength of
590 MPa. Reproduced from Hashimoto, K.; Kuwabara, T.; Iizuka, E.; Yoon, J. W. Effect of Anisotropic Yield Functions on the Accuracy
of Hole Expansion Simulations for 590MPa Grade Steel Sheet. Tetsuto-Hagene´ 2010, 96 (9), 557–563 (in Japanese); (b) SUS304 stainless
steel sheet. Reproduced from Murakoso, S.; Kuwabara, T. Measurement and Analysis of Ultra-Thin Austenitic Stainless Steel Sheet
Under Biaxial Tensile Loading and In-Plane Reverse Loading. J. Solid Mech. Mater. Eng. 2009, 3, 1330–1339; (c) 6000 series
aluminum alloy sheet with high- and low-density cube textures. Reproduced from Yanaga, D.; Kuwabara, T.; Uema, N.; Asano, M. Material
Modeling of 6000 Series Aluminum Alloy Sheets with Different Density Cube Textures and Effect on the Accuracy of Finite Element
Simulation. Int. J. Solids Structures 2012, 49, 3488–3495; and (d) pure titanium sheet. Reproduced from Ishiki, M.; Kuwabara, T.;
Hayashida, Y. Measurement and Analysis of Differential Work Hardening Behavior of Pure Titanium Sheet Using Spline Function. Int. J.
Mater. Form. 2011, 4 (2), 193–204. In (d) the work contours for 3p0 , 0:002 were measured using the multiaxial tube expansion
testing method as described in Section 1.06.6.
p
Figures 9(b) and (c) show the effects of wS on 3max for sx:sy ¼ 2:1 and 1:1 (7). As the effective sectional area of the
arms decreases with the increase of wS, the load transmitted to the gauge area decreases; therefore, this results in the
p
decrease of 3max .
Note that the results shown in Figure 9 should be viewed only as reference data, because these are numerical analysis results
based on the simple mechanics of plasticity and the maximum load condition for the arm (27), by assuming that the material is
isotropic.
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250
A6XXX-T4 350 SPCE
D22= –D11 (D22 >0)
200 300
250
p
=0.001 D22 = –D11 (D22 >0)
150
D22 = –0.833D11(D >0)
/ MPa
/ MPa
22 200 p
=0.001
p
=0.002 Dp p=0.0019
22
22
100 D11=D22 = 1 150

p =0.001
D11=D22 =1
100 Dp
D22 = –D11 (D11>0)
50 D22 = –1.2D11 (D11>0)
D22 = –D11 (D11>0)
50 p =0.001
p
p
=0.002 =0.0017
0 0
0 50 100 150 200 250 0 50 100 150 200 250 300 350
/ MPa 11
/ MPa
11
(a) (b)
Figure 8 Stress paths observed for abrupt strain path change following equibiaxial stretching for (a) 6000-series aluminum alloy and (b) SPCE (IF steel),
compared with the subsequent yield surfaces, ,, B, and 6, measured by unloading-reloading method and the work contour, C, measured for
the as-received materials subjected to linear stress paths. Reproduced from Kuwabara, T.; Kuroda, M.; Tvergaard, V.; Nomura, K. Use of Abrupt Strain
Path Change for Determining Subsequent Yield Surface: Experimental Study with Metal Sheets. Acta Mater. 2000, 48, 2071–2079.
p
ε max
0.15
w s /B=0.01
σx : σy =1:1
0.10 σx : σy =2:1
0.05
0.00
0.1 0.2 0.3 0.4 n
(a)
p
ε max ε max
p
0.12 0.12
σx : σy =2:1 σx : σ y =1:1
0.10 0.10 n=0.30
0.08 0.08 n=0.25
0.06 n=0.30
0.06 n=0.20
n=0.25
0.04 0.04
n=0.20
0.02 0.02 n=0.1
n=0.10
0.00 0.00
0.005 0.010 0.015 0.020 0.005 0.010 0.015 0.020
ws / B ws / B
(b) (c)
p
Figure 9 Effect of n-value (a) and the slit width (b and c) on the maximum equivalent plastic strain 3max , applicable to the gauge area of the cruciform
specimen shown in Figure 2. Material model: von Mises yield function. The number of slits: 7. Reproduced from Hanabusa, Y.; Takizawa, H.;
Kuwabara, T. Numerical Verification of a Biaxial Tensile Test Method Using a Cruciform Specimen. J. Mater. Processing Technol. 2013, 213 (6), 961–970.
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1.06.4 Combined Tension–Compression Testing Method

In the cylindrical cup drawing process, a material element in the flange area is subjected to tension in the radial direction and
compression in the circumferential direction. Since the flow stresses in the flange area are one of the main factors that affect the
formability of sheet metals in cup drawing, the combined tension–compression test is useful to evaluate the cup drawability of sheet
metals.
1.06.4.2 Testing Jigs and Specimen

Figure 10(a) shows a schematic diagram for the setting of the dies that are designed and fabricated for the combined tension–
compression test (28). The lower dies 1 and 2 are fixed to the chucks of a biaxial tensile testing machine, so that the teeth of
each of the lower dies are dovetailed with each other. A specimen is set on the lower dies as shown in the figure. A pair of
compression platens is fixed to the lower dies to apply compressive force to the sides of the gauge area of the specimen. The upper
dies were placed over the specimen and fixed to the lower dies using bolts with a gap of 101% of the sheet thickness between the
upper and lower dies. Teflon sheets are inserted between the specimen and the dies to reduce the amount of friction between the
dies and the specimen. In addition, the edges of the Teflon sheet are bent, so that it may be inserted between the compression
platens and the sides of the specimen to enhance the reduction of friction.
Figure 10(b) shows a picture with a specimen sandwiched between the upper and lower dies. Both ends of the specimen are
clamped by the chucks of the testing machine. The strain components of the specimen are measured using a biaxial strain gauge
mounted on the center of the gauge area; the lead wires of the strain gauge are fed through the gaps between the teeth of the dies.
Figure 10(c) shows the geometry of the specimen used for the combined tension–compression test.
1.06.4.3 Finite Element Analysis

In order to estimate the accuracy of stress measurement using the specimen shown in Figure 10(c), the stress distribution in the
gauge area of the specimen was analyzed using FEA with four-node shell elements. The ratio of the applied forces was taken to be
Fx:Fy ¼ 1:'1. The coefficient of friction between the side of the gauge section of the specimen and the compression platen was 0.05.
Upper die 1
Lower die 1 Upper die 2
Chuck 1
Specimen
Teflon sheet Lower die 2
Chuck 2
Compression platens
(a) (b)
Slit width: 0.8 y(x ) Strain gauge
(c)
Figure 10 Testing jigs and specimen for the combined tension–compression test. Reproduced from Kuwabara, T.; Horiuchi, Y.; Uema, N.;
Ziegelheimova, J. Material Testing Method of Applying In-Plane Combined Tension-Compression Stresses to Sheet Specimen. Proc. IDDRG 2008, 2008,
163–171. (a) Overview. (b) Specimen sandwiched between the lower and upper dies with both ends clamped by the chucks of a biaxial tensile
testing machine. (c) Geometry of the specimen used for the combined tension–compression test (dimensions given in millimeters).
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1 3
(MPa) y (MPa)
x
1: 144.1–141.8 5
1: 136.4–138.6 1
2: 141.8–139.2 4 2: 138.6–140.9 3
1
3: 139.5–137.3 3
3: 140.9–143.2 2 1
3
4: 137.3–135.0 1 3
2 3 3 1
1
(a) (b)
xy (MPa)
1: 2.2–0.0 3 2 y
Fy
2: 0.0 –2.2
1
3: –2.2 –4.4
3
2 1 Fx
3
1
x
0
(c)
Figure 11 Contours of (a) sx, (b) sy, and (c) sxy calculated using FEA in the gauge area of the specimen shown in Figure 10. The average true
stresses were sx ¼ 'sy ¼ 142.7 MPa; the equivalent plastic strain in the gauge area is approximately 0.002. The increment of contour is
approximately 2 MPa. Reproduced from Kuwabara, T.; Horiuchi, Y.; Uema, N.; Ziegelheimova, J. Material Testing Method of Applying In-Plane
Combined Tension-Compression Stresses to Sheet Specimen. Proc. IDDRG 2008, 2008, 163–171.
The material was assumed to follow the von Mises yield criterion with the work-hardening characteristics of
s ¼ 808(0.009 þ 3p)0.245 (MPa) (28).
Figure 11 shows the calculated results of sx, sy, and sxy when the equivalent plastic strain in the gauge section reached 0.002. The
calculated forces were Fx ¼ 'Fy ¼ 4280 N and the thickness strain was almost zero; therefore, the average true stresses, sx ¼ 'sy, were
4280 (N)/30 (mm2) ¼ 142.7 MPa. On the other hand, the values of the normal stress components sx and sy were within
139.2 < sx < 141.8 MPa, 140.9 < 'sy < 143.2 MPa at the central region of the gauge section. Accordingly, the error of stress
measurements that use the specimen is estimated to be less than 3% in sx and less than 2% in sy. The shear stress component, sxy, is
'2.2 < sxy < 0 MPa for the 70% area of the gauge section, which means that sxy is less than 1.5% of the maximum principal stress.
These results confirm that the gauge section of the specimen is nearly in the pure-shear stress state. We carried out the same analysis
for the case when the equivalent plastic strain in the gauge area of the specimen reached 0.04 and found that the error of stress
measurement is less than 1% in sx and less than 4% in sy, and that the shear stress component sxy is less than 4% of the maximum
principal stress. As a result, it was again confirmed that the gauge section of the specimen is nearly in the pure-shear stress state.
1.06.4.4 Examples of Test Results

Figure 12 shows the measured work contours for a steel sheet with a tensile strength of 440 MPa, superimposing the theoretical
yield loci calculated using the Yld2000-2d yield function (29) with an exponent of 6. The short lines attached to the data points
represent the directions of the current plastic strain rates measured at different levels of 3P0 . The yield loci based on the Yld2000-2d
yield function are generally in good agreement with the measured work contours.
1.06.5 In-plane Stress Reversal Testing Method

In the bending of a sheet material, part of the material fibers layered in the thickness direction of the sheet are subjected to in-plane
compression. The flow stress of some metals is often observed to be higher in compression than in tension, and vice versa, even if
the metal is fully annealed; this phenomenon is referred to as the strength-differential effect (SDE). The SDE is significant especially
in hexagonal closed packed materials (30,31).
During the processes of sheet metal part production, the sheet metal undergoes several strain path changes. The raw material is
successively cold rolled into a flat sheet until the desired thickness is obtained. Blanks are then cut off from the rolled sheet and
formed into final part shapes by drawing and bending. Furthermore, the formed parts are often subjected to repeated loading in
service. Therefore, in order to obtain in-depth knowledge of the mechanical properties of the parts, it is vital to observe the stress–
strain response of the sheet metal when it is subjected to strain path changes, monotonic tensile loading, and compressive loading.
Note that the strain path changes during forming processes affect the dislocation substructure of the material and the stress–strain
curve is dependent on it (32). Moreover, the directionality of dislocation structures in severely deformed metals and their rear-
rangement during reloading can result in tension–compression asymmetry (TCA) of the flow stress in the material (33).
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500
400
300
200
100
/MPa
y
0
–100
–200
–300
–400
–500
–500 –400 –300 –200 –100 0 100 200 300 400 500
x /MPa
Figure 12 Comparison of work contours with the yield loci calculated using the Yld2000-2d yield function with an exponent of 6. 3P0 ¼: C0.0005,
B0.005, :0.02, 60.03, and ;0.04. Reproduced from Kuwabara, T.; Horiuchi, Y.; Uema, N.; Ziegelheimova, J. Material Testing Method of Applying
In-Plane Combined Tension-Compression Stresses to Sheet Specimen. Proc. IDDRG 2008, 2008, 163–171.
Consequently, in order to perform accurate forming simulations for sheet metals, it is vital to develop a testing device that
enables the correct measurement of the stress–strain responses of the sample subjected to in-plane compression and/or in-plane
stress reversal, and to establish more sophisticated material models that enable the reproduction of the observed SDE and/or TCA.
1.06.5.2 Testing Jigs and Specimen

Figure 13 shows an example of the testing apparatus for in-plane stress reversal test (34). Figure 13(a) shows the comb-type dies
developed for application of continuous in-plane stress reversal to sheet specimens. Lower and upper comb-type dies are installed in
the testing apparatus, as shown in Figure 13(b). Lower die 1 is fixed to the lower plate of the die set, and lower die 2 is fixed to a slide
rail that enables the die to move smoothly in the horizontal direction. A sheet specimen is set on lower dies 1 and 2 and both ends of
the specimen are attached to the dies by chucking plates. The upper dies are placed on the specimen so that the four positioning pins
that are fixed on the lower dies align with the holes of the upper dies. The movement of the upper dies is synchronized with that of
the lower dies. Lower die 2 is actuated in the horizontal direction by the servo-controlled hydraulic cylinder A, so that continuous in-
plane stress reversals are applied to the specimen. Hydraulic cylinder B exerts a constant blank-holding force on the specimen
through the upper dies and the cylindrical rollers lying between the upper dies and the blank-holding platen. The specimen can thus
be compressed in the longitudinal direction without buckling. It is recommended that the specimen be lubricated on both sides
with Vaseline and Teflon sheets to prevent the specimen from galling the dies.
A strain gauge measures the amount of longitudinal strain. An amount of blank-holding pressure is applied to the specimen and
is approximately 1% of the tensile strength of the material, which prevents buckling of the specimen during in-plane compression.
According to the FEA of the specimen deformation and the strain measurement position shown in Figure 13(c), the stress
measurement error is estimated to be less than 1% (35). For other types of stress-reversal testing methods, see (1).
1.06.5.3 Examples of Test Results

Figure 14 shows the true stress–true strain curves of dual-phase steel sheet with a tensile strength of 980 MPa for a tension followed
by compression test (TC test) and for a compression followed by tension test (CT test) (36). The amounts of prestrain were
3u ¼ 0.025, 0.05, and 0.10 for the TC test and '0.025, '0.05, and '0.08 for the CT test. Figure 14(a) shows an overall view of the
true stress–true strain curves. The nonlinearity of these stress–strain curves during unloading is clearly observed. Figure 14(b)
compares the stress–strain curves measured in the monotonic tension and compression tests. The stresses are slightly higher in
compression than in tension. The physical causes of the TCA in metals have been, and remain, an issue of considerable interest.
Considering that the test material used in this study is a high-strength steel alloy, the possible cause of the TCA is the pressure
dependence of plastic flow, as was observed for high-strength steel alloys, and is concluded to be the case by (5,37–39).
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Upper die 2
Hydraulic cylinder B
Upper die 1
Specimen Blank holding platen

Teflon sheets
Upper die 1 Upper die 2
Load cell
Specimen
Lower die 2
Lower plate Slide rail Hydraulic cylinder A
Lower die 1 Lower die 1 Lower die 2
(a) (b)
Strain gauge
y
(c)
Figure 13 Experimental apparatus for application of in-plane compression to a sheet specimen; (a) Configuration of the dies and (b) an overview of
the testing apparatus. Reproduced from Kuwabara, T.; Kumano, Y.; Ziegelheim, J.; Kurosaki, I. Tension-Compression Asymmetry of Phosphor Bronze
for Electronic Parts and Its Effect on Bending Behavior. Int. J. Plast. 2009, 25, 1759–1776. (c) Geometry of the specimen. Reproduced from Noma,
N.; Kuwabara, T. Specimen Geometry Optimization for In-Plane Reverse Loading Test of sheet Metal and Experimental Validation. Steel Research
International, Special Edition: 14th Metal Forming, 2012, pp 1283–1286.
Figure 15 shows another example for demonstrating the usefulness of the stress reversal test. In a basic study on the V-bending of
cold-rolled SUS304 sheets of 16 different lots, we found an interesting phenomenon when examining the springback that follows
the V-bending (40). Figure 15(a) shows the relationship between the measured springback angles after V-bending, Dq, and the flow
stresses of the samples, s0.029, at a tensile strain of 0.029. The difference of springback angles between RD bending and TD bending
was checked for all lots, where RD and TD bendings refer to the direction of V-bending in which the direction of the bending stresses
is parallel to the RD and TD of the sheet, respectively. The sheet thickness of all lots was 0.3 mm. The flow stresses of the alloys at
a 2.9% tensile strain were in a range of 880–1050 MPa. It was found that the springback angles were approximately 20% larger in TD
bending than in RD bending irrespective of lots. This result is surprising, because the tensile flow stresses of the samples in the RD
and TD were almost the same in all lots.
This phenomenon can be explained by Figure 15(b), which compares the stress–strain curves obtained from the in-plane
tension and compression tests for the RD and TD conditions. The tensile flow stresses almost coincide with each other in the RD and
Figure 14 True stress–true strain curves of dual-phase steel sheet with a tensile strength of 980 MPa. Testing direction:Rolling direction. (a) Tension
followed by compression and compression followed by tension. (b) Comparison of the uniaxial true stress–true strain curves between tension and
compression. Reproduced from Saito, R.; Kuwabara, T.; Iizuka, E. Material Modeling of 980 MPa Dual Phase Steel Sheet Based on Biaxial Tensile Test and
In-Plane Stress Reversal Test. In Proc. IDDRG 2010, Graz, Austria, 2010, pp 669–678.
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32 1500
SUS304-3/4H (0.3 mm thick)
SUS304
30
/° 1000
28
/ MPa
500
Springback angle
26
0
True stress
24
–500
22
RD –1000 RD
20
TD TD
18 –1500
850 900 950 1000 1050 1100 –0.012 –0.008 –0.004 0.000 0.004 0.008 0.012
/MPa True strain
0.029
(a) (b)
Figure 15 (a) Difference in springback angles, Dq, between RD and TD bending in V-bending cold-rolled SUS304 sheets from 16 different lots. s0.029:
Tensile stress at a tensile strain of 3 ¼ 0.029. (b) Comparison of the true stress–true strain curves measured in the tension and compression tests
for the RD and TD. Reproduced from Kuwabara, T.; Saito, R.; Hirano, T.; Oohashi, N. Tension-Compression Asymmetry in Austenitic Stainless Steel Alloys
for Electronic Parts and Its Effect on Springback Behavior. Tetsu-to-Hagene´2009, 95 (11), 732–739 (in Japanese).
TD conditions. On the other hand, the compressive flow stresses are significantly higher in the TD condition than in the RD
condition. This TCA caused higher bending moment in TD bending than in RD bending; in contrast, the springback became larger
in TD bending than in RD bending.
1.06.6 Multiaxial Tube Expansion Testing Method

p
The maximum plastic strain 3max applicable to the cruciform specimen shown in Figure 2 depends primarily on the work-hardening
p
rate (n-value) of the test material, as shown in Figure 9: 3max + 0:1 in most cases for 0 + n + 0.3.
p
The author investigated the work-hardening behavior of a pure titanium sheet under biaxial tension (18). The level of 3max for
p
which a contour of plastic work could be determined was 0.002. In order to increase the level of 3max , tubular specimens were
fabricated from a flat sheet sample, and combined internal pressure and axial force were applied to the tubular specimens using
p
a servo-controlled tube bulge testing machine (41–43). As a result, 3max increased up to 0.085 (18) and 0.225 (44). Furthermore, the
same testing method was applied to an ultralow carbon steel sheet; the work-hardening behavior of the sample was successfully
p
measured for many linear stress paths up to a level of 3max ¼ 0:19 (45), see Figure 19. Therefore, this testing method, referred to here
as the multiaxial tube expansion testing method, is a useful material testing method to measure the biaxial deformation behavior of
sheet metals for a large plastic strain range.
This section introduces the multiaxial tube expansion testing method and shows examples of testing results. The reader is also
referred to excellent reviews of earlier work on multiaxial tube expansion/torsion tests (20,46–48), although most of the studies
were concerned with the initial yielding behavior of tubular specimens machined from bulk metals.
1.06.6.2 Tubular Specimen and Testing Machine

Figure 16 shows a tubular specimen with an outer diameter of D, a thickness of t, and a length of L. It is fabricated by bending a piece
of sheet sample into a cylindrical shape with a constant curvature and welding the sheet edges together. The bending strain should
be as uniform as possible in the circumferential direction during tube fabrication; otherwise, uniform, axisymmetric bulge
deformation is prohibited in the following tube bulge test and early failure is prone to occur at a position with excessive plastic
strain.
C C
t
I II
D L
Figure 16 Geometry of a tubular specimen for the multiaxial tube expansion testing method. 4 indicates the RD of the original sheet sample.
The RD is taken in the axial direction for type I specimen and in the circumferential direction for type II specimen. The length C is the area for clamping
the specimen to a testing machine.
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Pantograph-type
link mechanism Strain gauges
(a) (b)
Figure 17 Experimental apparatus for the multiaxial tube expansion testing method. (a) Electrically servo-controlled tension-internal pressure testing
machine. (b) Arrangement of strain gauges and a spherometer. Reproduced from Kuwabara, T.; Yoshida, K.; Narihara, K.; Takahashi, S. Anisotropic
Plastic Deformation of Extruded Aluminum Alloy Tube Under Axial Forces and Internal Pressure. Int. J. Plast. 2005, 21, 101–117.
The width of the weld line should be as narrow as possible to minimize the effect of the weld line on the test results. Two types of
tubular specimens, type I and II, may be fabricated; type I and II specimens have the RD of the original sheet sample in the axial and
circumferential directions, respectively.
1.06.6.3 Stress and Strain Measurement

Figure 17(a) shows a schematic of the combined tension-internal pressure testing machine used for the biaxial bulge test. Axial
loads were applied to the specimen by opposing hydraulic cylinders and internal pressure by an intensifier; both were servo-
controlled using an electrical, closed-loop control system. A pantograph-type link mechanism is used so that the center of the
specimen is always positioned at the center of the testing apparatus, where the spherometer shown in Figure 17(b) is located. For
the details of the testing machine, see (41).
The deformation behavior of the specimen is measured using a spherometer and two strain gauges. The spherometer consists of
a displacement meter and two wedges. The spherometer has the freedom to rotate around an axis vertical to the central axis of the
specimen, so that the pointed ends of the displacement meter and the two wedges are always in contact with the bulged surface of
the specimen.
The axial and circumferential membrane strains, 3f and 3q, are measured using strain gauges mounted on the center of the
specimen as shown in Figure 17(b) 3f and 3q are assumed to be uniform in the circumferential direction of the specimen, and are
evaluated at the middle thickness using the following equations:
Rf
3f ¼ 3fS ' ln ;
Rf ' ðt=2Þ
[5]
D't D0 expð3qS Þ ' t
3q ¼ ln ¼ ln ;
D0 ' t0 D0 ' t0
where 3f and 3q are the axial and circumferential true strains measured on the outer surface of the specimen, D0 and t0 are the initial
outer diameter and wall thickness of the specimen, and D and t are the deformed outer diameter and thickness measured at the
center of the specimen. The current thickness, t, is determined under the assumption of constant volume and neglecting elastic
strains as
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
" #2 " #ffi
D D ðD0 ' t0 Þt0
t¼ ' ' $ % [6]
2 2 exp 3f
The strain gauges are replaced when the strain value reaches a predetermined limit value.
The axial and circumferential stress components, sf and sq, are calculated as the values at the middle thickness by using the
following equations, which are based on the equilibrium requirements at the center of the specimen:
PpðD=2 ' tÞ2 þ T

sf ¼ ;
pðD ' tÞt
$ % [7]
Rf ' t ðD ' 2tÞ D't
sq ¼ $ % P' sf ;
2Rf ' t t 2Rf ' t
where T and P are measured values of the axial load and internal pressure, respectively.
The measured values of T, P, 3f, 3q, and Rf are input to a personal computer, and sf and sq are calculated from eqn [7]. These
values of sf and sq are compared with the command values of sf and sq. According to the discrepancy between the measured and
command stress values, two PI-controllers then output command signals for controlling T and P. The command signals for T and P
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Figure 18 Comparison of the true stress–true plastic strain curves in the rolling direction of the test material for sx:sy ¼ 2:1, measured using a cruciform
specimen and tubular specimen. Material: A cold-rolled, ultralow carbon steel sheet. Reproduced from Kuwabara, T.; Enatsu, R. Measurement and
Material Modeling of Work Hardening Behavior of Cold Rolled IF Steel Sheet Using Multiaxial Tube Expansion Testing Method. Tetsuto-Hagane´2012, 98
(6), 275–282 (in Japanese).
are then compared with the measured values, and the servo-valves are controlled according to the difference between the measured
and command values of T and P. These valves activate the hydraulic cylinders and intensifier so that the desired values of sf and sq
are applied to the specimen.
1.06.6.4 Determination of Biaxial Stress–Strain Curves

Figure 18 shows an example of the stress–strain curve in the maximum principal stress direction for a 0.8-mm-thick cold-rolled
interstitial free (IF) steel sheet (49). The inner diameter of the tubular specimen is 44.6 mm. First, the biaxial true stress–true plastic
strain curves that were measured using a cruciform specimen are superimposed on those measured using a tubular specimen.
Second, the latter are shifted along the strain axis so that both SS curves are smoothly connected to each other at a star marker q; this
shifting procedure is necessary to account for the work hardening caused by the prestrain applied to the tubular specimen during
bending (tube forming) process.
1.06.6.5 Material Modeling

Figure 19 shows the measured stress points that form the contours of plastic work for the same material shown in Figure 18. In
Figure 19(b), all stress values (sx,sy) that form a work contour are normalized by s0 corresponding to a specific value of 3P0 . The
figures also depict the theoretical yield loci based on the von Mises (50), Hill’s quadratic (Hill ‘48) (51), and the Yld2000-2d yield
functions (29) with an exponent of M. The work contours are generally in good agreement with the Yld2000-2d yield function with
Yld2000-2d M=5
500 1.5
ε0p= ε0p =
0.002 0.002
400 0.01 1.2 0.01
0.02 0.08
0.03
0.131
300 0.04 0.9 0.19
σy /MPa
0.06
σy / σ0
0.08
0.10
200 0.6
0.131 von Mises
0.16 HIll'48
0.19 Yld2000-2d
100 Yld2000-2d 0.3
M=6 M=5 (ε 0p= 0.131)
M =6 (ε 0p= 0.002)
0 0.0
0 100 200 300 400 500 0.0 0.3 0.6 0.9 1.2 1.5
σx / σ0
σx /MPa
(a) (b)
Figure 19 Measured stress points comprising contours of plastic work compared with the theoretical yield loci. Material: Cold-rolled, ultralow carbon
steel sheet. Each symbol corresponds to a contour of plastic work for a particular value of 3p0 . In (a), the exponent M selected for the Yld2000-2d
yield function was 5 for 0:002 + 3p0 + 0:19 and was 6 only for 3p0 ¼ 0:002. In (b), the stress values were normalized by s0 corresponding to the 3p0 for
each work contour. Reproduced from Kuwabara, T.; Enatsu, R. Measurement and Material Modeling of Work Hardening Behavior of Cold Rolled IF
Steel Sheet Using Multiaxial Tube Expansion Testing Method. Tetsuto-Hagane´2012, 98 (6), 275–282 (in Japanese).
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0.6
1:4 Fractured
Fracturing
at basewelded
beside material
zone
: 4:1 2:1 4:3 1:1 3:4 1:2 1:4
at weld zone
in welded x y
0.4
p
y
1:2 3:4
True plastic strain

x: y = 1:1
0.2
4:3
0.0
2:1
4:1
–0.2
–0.2 0.0 0.2 0.4 0.6
p Fracture at weld
True plastic strain x
(a) (b)
Figure 20 (a) Measured strain paths and forming limit strains of the tubular specimens subjected to linear stress paths, and (b) the specimens that
fractured under the linear stress paths shown in (a). The material is the same as that used in Figure 19.
p
an exponent M of 5 for 0:002 + 30 < 0:19, although M ¼ 6 appears to have slightly closer agreement with the work contour only for
p
30 ¼ 0:002.
1.06.6.6 Measurement of Forming Limit Curve

Figure 20 shows the measured strain paths and forming limit strains of the test specimens deformed under linear stress paths, as
shown in Figure 19, and the pictures after they fractured. All specimens other than that for sx:sy ¼ 1:1 fractured at a position away
from the weld line. As a result, we confirm that this testing method is effective at determining forming limit strains and stresses of
sheet metals under multiaxial stress states in the first quadrant of stress space.
It is noted that type I and II specimens were used for the tests with sx < sy and sx , sy, respectively; the maximum principal stress
direction was always taken in the circumferential direction of the specimen. This is because the weld of the IF steel has a higher flow
stress than that of the base material.
Forming limit stress curves have been measured for aluminum alloy tubes (42,52), steel tube (43), and ultra-low carbon steel
sheet (53) using the multiaxial tube expansion testing method and its path dependency has been discussed.
1.06.7 Combined Tension-Shear Testing Method
Multiaxial stress test can be performed by applying normal and tangential loads to a rectangular sheet specimen, see (54–56).
References
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13. Hill, R.; Hutchinson, J. W. Differential Hardening in Sheet Metal Under Biaxial Loading: A Theoretical Framework. J. Appl. Mech. 1992, 59, S1–S9.
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Struct. 1994, 31, 2999–3021.
15. Hashimoto, K.; Kuwabara, T.; Iizuka, E.; Yoon, J. W. Effect of Anisotropic Yield Functions on the Accuracy of Hole Expansion Simulations for 590MPa Grade Steel Sheet. Tetsu-
to-Hagene´ 2010, 96 (9), 557–563 (in Japanese).
16. Murakoso, S.; Kuwabara, T. Measurement and Analysis of Ultra-Thin Austenitic Stainless Steel Sheet Under Biaxial Tensile Loading and In-Plane Reverse Loading. J. Solid
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Finite Element Simulation. Int. J. Solids Struct. 2012, 49, 3488–3495.
18. Ishiki, M.; Kuwabara, T.; Hayashida, Y. Measurement and Analysis of Differential Work Hardening Behavior of Pure Titanium Sheet Using Spline Function. Int. J. Mater. Form.
2011, 4 (2), 193–204.
19. Hutchinson, J. W. Elastic-Plastic Behaviour of Polycrystalline Metals and Composites. Proc. R. Soc. London A 1970, 319, 247–272.
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Stricklin, J. A., Saczalski, K. H., Eds.; ASME: New York, 1976; pp 1–33.
21. Støren, S.; Rice, J. R. Localized Necking in Thin Sheet. J. Mech. Phys. Solids 1975, 23, 421–441.
22. Hutchinson, J. W.; Tvergaard, V. Shear Band Formation in Plane Strain. Int. J. Solids Struct. 1981, 17 (5), 451–470.
23. Larsson, M.; Needleman, A.; Tvergaard, V.; Storåkers, B. Instability and Failure of Internally Pressurized Ductile Metal Cylinders. J. Mech. Phys. Solids 1982, 30 (3), 121–154.
24. Needleman, A.; Tvergaard, V. Analyses of Plastic Flow Localization in Metals. ASME Appl. Mech. Rev. 1992, 45, S3–S18.
25. Hecker, S. S. Experimental Investigation of Corners in the Yield Surface. Acta Mech. 1972, 13, 69–86.
26. Kuroda, M.; Tvergaard, V. Use of Abrupt Strain Path Change for Determining Subsequent Yield Surface: Illustrations of Basic Idea. Acta Mater. 1999, 47, 3879–3890.
27. Marciniak, Z.; Duncan, J. L.; Hu, S. J. Mechanics of Sheet Metal Forming; Butterworth-Heinemann: Oxford, 2002, p 63.
28. Kuwabara, T.; Horiuchi, Y.; Uema, N.; Ziegelheimova, J. Material Testing Method of Applying In-Plane Combined Tension-Compression Stresses to Sheet Specimen. In Proc.
IDDRG ’08; Olofstrom: Sweden, 2008. June 16-18; pp 163–171.
29. Barlat, F.; Brem, J. C.; Yoon, J. W.; Chung, K.; Dick, R. E.; Lege, D. J.; Pourboghrat, F.; Choi, S. H.; Chu, E. Plane Stress Yield Function for Aluminum Alloy Sheets – Part 1:
Theory. Int. J. Plast. 2003, 19, 1297–1319.
30. Plunkett, B.; Lebensohn, R. A.; Cazacu, O.; Barlat, F. Anisotropic Yield Function of Hexagonal Materials Taking into Account Texture Development and Anisotropic Hardening.
Acta Mater. 2006, 54, 4159–4169.
31. Lou, X. Y.; Li, M.; Boger, R. K.; Agnew, S. R.; Wagoner, R. H. Hardening Evolution of AZ31B Mg Sheet. Int. J. Plast. 2007, 23, 44–86.
32. Barlat, F.; Ferreira Duarte, J. M.; Gracio, J. J.; Lopes, A. B.; Rauch, E. F. Plastic Flow for Non-Monotonic Loading Conditions of an Aluminum Alloy Sheet Sample. Int. J. Plast.
2003, 19 (8), 1215–1244.
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2009, 25, 1759–1776.
35. Noma, N.; Kuwabara, T. Specimen Geometry Optimization for In-Plane Reverse Loading Test of Sheet Metal and Experimental Validation. Steel Res Int, Special Edition: 14th
Metal Forming, 2012, 1283–1286.
36. Saito, R.; Kuwabara, T.; Iizuka, E. Material Modeling of 980 MPa Dual Phase Steel Sheet Based on Biaxial Tensile Test and In-Plane Stress Reversal Test. Proc. IDDRG 2010,
Graz, Austria, 2010, pp 669–678.
37. Spitzig, W. A.; Sober, R. J.; Richmond, O. Pressure Dependence of Yielding and Associated Volume Expansion in Tempered Martensite. Acta Metall. 1975, 23, 885–893.
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40. Kuwabara, T.; Saito, R.; Hirano, T.; Oohashi, N. Tension-Compression Asymmetry in Austenitic Stainless Steel Alloys for Electronic Parts and Its Effect on Springback Behavior.
Tetsu-to-Hagene´ 2009, 95 (11), 732–739 (in Japanese).
41. Kuwabara, T.; Yoshida, K.; Narihara, K.; Takahashi, S. Anisotropic Plastic Deformation of Extruded Aluminum Alloy Tube Under Axial Forces and Internal Pressure. Int. J. Plast.
2005, 21, 101–117.
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43. Yoshida, K.; Kuwabara, T. Effect of Strain Hardening Behavior on Forming Limit Stresses of Steel Tube Subjected to Nonproportional Loading Paths. Int. J. Plast. 2007, 23 (7),
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44. Sumita, T.; Kuwabara, T.; Hayashida, Y. Measurement of Work Hardening Behavior of Pure Titanium Sheet Using a Servo-Controlled Tube Bulge Testing Apparatus. In The 14th
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45. Enatsu, R.; Kuwabara, T. Biaxial Tensile Test of Cold Rolled IF Steel Sheet for Large Plastic Strain Range. In Proc. NUMISHEET 2011; AIP Conference Proceedings, 2011,
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1.07 Residual Stress Measurements
TR Watkins, Oak Ridge National Laboratory, Oak Ridge, TN, USA
GS Schajer, The University of British Columbia, Vancouver, BC, Canada
MJ Lance, Oak Ridge National Laboratory, Oak Ridge, TN, USA
Portions of the contribution have been prepared by UT-Battelle, LLC, Operator of Oak Ridge National Laboratory under Contract No. DE-AC05-00OR22725,
with the U.S. Department of Energy.

1.07.2 Powder Diffraction 113
1.07.2.1 Bragg’s Law, Residual Strain, and Stress 114
1.07.2.2 Sources and Goniometers 114
1.07.2.3 Safety and Alignment 116
1.07.2.4 Experimental Considerations 117
1.07.2.5 Measurement and Analyses 119
1.07.2.6 Example: Residual Stresses Developed in Micro Drills 121
1.07.2.7 Concluding Remarks about Powder Diffraction Residual Stress Measurements 121
1.07.3 Introduction to Hole-Drilling 122
1.07.3.1 Features of Hole-Drilling 123
1.07.3.2 History 123
1.07.3.3 Drilling Technique 124
1.07.3.4 Deformation Measurements – Strain Gauges 124
1.07.3.5 Deformation Measurements – Full-Field Optical Techniques 125
1.07.3.6 Uniform Residual Stress Calculation 126
1.07.3.7 Residual Stress Profile Calculation 126
1.07.3.8 Stress Computation from Optical Data 127
1.07.3.9 Concluding Remarks about Hole-Drilling 128
1.07.4 Introduction to Piezospectroscopy 128
1.07.4.1 Piezoluminescence 128
1.07.4.2 Piezo-Raman 130
1.07.4.3 Emerging Techniques 131
1.07.4.4 Concluding Remarks about Piezospectroscopy 132
References 132
1.07.1 Introduction
Residual stresses are self-equilibrating stresses that exist in a material, sample, or component in the absence of externally applied
forces. They are created during most manufacturing processes, most notably during welding and casting processes. Since residual
stresses often play a part in material behavior, knowing their state is essential in predicting the performance of many engineering
components.
As is true of other forms of stress ‘measurement,’ in actuality, the strain, displacement, or length change is what is actually
measured. The methods of measurement can be coarsely divided into two categories. Measurement methods such as diffraction and
spectroscopy require a reference sample or state for comparison, calibration, and/or normalization. Measurement methods such as
hole-drilling measure the samples’ relaxation response after a portion of the sample has been removed or sectioned. In either
category, a length change or difference is measured and normalized to strain. The residual stress is then determined or calculated
from that strain. As we will discuss, the success of any chosen residual stress measurement method depends on the sample’s
composition, size, bonding/crystallinity, and/or its ability to be altered (i.e., cut, sectioned, polished, downsized, etc.).
1.07.2 Powder Diffraction
Diffraction, particularly X-ray diffraction, is a common characterization technique that can readily yield a wealth of information
from crystalline materials, such as most metals and ceramics (1). Diffraction may be of limited utility when working with polymers
and amorphous materials, which are often better characterized by other scattering techniques (2). While single crystals readily
diffract, most engineering materials are polycrystalline. Polycrystalline materials contain many grains or crystallites and may be in
solid or powder form; in a randomly oriented sample, the diffraction pattern and properties of the material will reflect this assembly
of grain and vice versa. Polycrystalline diffraction is frequently called powder diffraction, even though the sample may not

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114 Residual Stress Measurements
necessarily be a powder. Solid samples can sustain long-range applied or residual stresses, while powders cannot – though powders
can be useful as a strain-free reference. This chapter will only discuss the determination of residual stresses within solid poly-
crystalline samples.
Briefly, the X-ray powder diffraction method is widely used to characterize polycrystalline samples (1). It is used most frequently
to provide phase identification and phase fraction, which may be obtained from a diffraction pattern. This pattern typically covers
a sizable range of diffraction angle, 2q, which contains multiple peaks, in order to make a conclusive determination. The intensity
(counts) or height of a peak is proportional to the number of diffracting grains. Thus, the degree of nonrandomness of the grains of
a sample or its crystallographic orientation or texture may be determined from a comparison of the intensities from a solid sample
to those of a random one, such as a carefully prepared powder. These data are typically presented in a pole figure. Similarly, the
mosaicity of a crystal or sample is determined from a rocking curve. The width of a diffraction peak is related, in part, to the sample’s
crystallite size or dislocation density and/or gradients (e.g., strain, chemistry). Further detailed discussion of these applications of
powder diffraction is beyond the scope of this work; the reader should refer to (1) for more information on this topic. Powder
diffraction is also one method for ‘measuring’ or, more correctly, determining the residual (or applied) stress.
1.07.2.1 Bragg’s Law, Residual Strain, and Stress

When Bragg’s law is satisfied, diffraction occurs, and a diffraction peak, also called a reflection, is observed. Using Bragg’s law (1,2),
we can calculate the spacing between planes of atoms (i.e., the interplanar spacing), d:
l ¼ 2d sin qB ; [1]
where l and qB are the radiation wavelength and half the Bragg angle, 2qB, respectively (1). Here, the wavelength will be considered
to be a constant, and the Bragg angle will be scanned and measured. If the interplanar spacing of a stressed sample, d1, and another
unstressed sample, d0, are measured, a strain, ε, can be calculated:
ε ¼ ðd1 ' d0 Þ=d0 [2]
If the appropriate Young’s modulus, E, is known, the stress (applied or residual), s, can be determined. Illustratively, the
following equation may be used:
s¼Eε [3]
More exact equations will be introduced later. Stress/strain measurements can also be considered as measuring peak shift, as shown
schematically in Figure 1.
In the diffraction literature, residual stresses may be classified according to the length scale over which they act (3,4), and as such,
the terms macrostress and microstress are frequently used in the diffraction residual stress literature. Unfortunately, they are often not
well defined. Macrostresses or type I stresses are typically regarded to occur over the mm and longer length scales, resulting in
diffraction peak shift or change in 2qB. Microstresses or type II stresses occur over mm length scales and also result in a peak shift (5).
Root-mean-square (RMS) stresses or type III stresses, which have also been referred to as microstresses (6), occur over the nm length
scale and result in peak broadening. (RMS stresses will not be discussed further here.) Since diffraction measures the total strain, any
combination of these residual stress types may be present. As such, careful analysis is often required to obtain a correct under-
standing of the residual stresses present in a given sample.
1.07.2.2 Sources and Goniometers

X-ray and neutron diffraction measurement methods are complementary. Simplistically, X-rays scatter off of the electron clouds of
atoms, and neutrons scatter off of the nuclei. X-rays, generally speaking, provide information from the surface (<0.1 mm) while
neutrons provide information from the bulk (1 < depth < 25 mm). There are three main types of X-ray generators or sources, listed
here in order of increasing relative intensity, cost, and maintenance: sealed tube, rotating anode, and synchrotron (3). X-rays from
most laboratory sources are equipped with an X-ray tube, typically with a Cu target, generating radiation which penetrates + 25 mm
over a w1 to 100 mm2 area. High-energy synchrotron X-rays penetrate deeper (>1 mm), sometimes to depths comparable to
Figure 1 Left, a strain-free crystal structure. Center, a tensile strain/stress is applied horizontally. Right, if diffraction occurs off of the horizontal
planes, and the Bragg peak shifts to a higher angle as the interplanar spacing decreases.
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Residual Stress Measurements 115
(a) (b)
Figure 2 (a) A PANalytical 2-axis q–q goniometer and (b) a Seifert 4-axis goniometer (base q–2q goniometer) with an open Eulerian cradle. Both
in parallel beam configuration with an incident multilayer parabolic mirror and Soller slits attached to the X-ray housing and radial divergence limiting slits
in front of a point detector (note: the Seifert unit has a rotating anode generator with both an electronic shutter and a manual shutter).
neutrons, depending on the atomic number of the material interrogated (7). While not a solution to all problems, synchrotrons can
provide intense, highly collimated, and truly monochromatic radiation to readily see minute quantities of phases present with the
highest resolution. In contrast to X-rays, neutrons can penetrate deeper (tens of mm in most materials) since most of the volume of
an atom is not made up of nuclei. This also indicates that neutron scattering is not very efficient, such that typical scattering or gauge
volumes are , 1 mm3. Neutrons for diffraction are produced either in a nuclear reactor or a pulsed source (8,9). In the nuclear
reactor and with regards to Bragg’s law, 2qB is scanned, l is constant, and d is calculated. In the pulsed source, 2qB is held constant, l
varies, and d is calculated.
X-ray diffractometers consist of an X-ray source and a goniometer, or angle-measuring device. The goniometers have two
common designs or geometries: theta–theta and theta–2theta (see Figure 2). The theta–theta geometry has the distinct
advantage that the sample rests in the horizontal plane and does not tilt during measurement. Since the sample is much less
likely to fall off its mount, this goniometer is the most popular choice and easily lends itself to in-situ stages (such as high-
temperature chambers). A theta–theta goniometer typically has two axes: U/incident-tube side and 2q/diffracted-detector
side. The diffraction plane is vertical for the theta–theta geometry, but is horizontal for the theta–2theta geometry. The theta–
2theta geometry also has two axes: U/sample and 2q/diffracted-detector side. This has the advantage of being able to attach and
support additional axes or ‘circles,’ which are often heavy. Commonly, an Eulerian cradle (full, half, or open) is added to make
a four-circle goniometer, which lends itself to residual stress determinations and crystallographic texture work. Although
a great deal of residual stress work is done with a two-axis goniometer, it is more advantageous to do this work with the
additional axes to orient the sample with respect to the incident beam. Portable X-ray units are also available, some of which
can perform X-ray residual stress analyses (see Figure 3). These units can be used for scientific studies, but they are really
engineering tools capable of examining samples that are very large (e.g., a submarine (10)) and/or possess a complicated shape
(e.g., engine blocks (11)).
Figure 3 The goniometer portion of a portable X-ray residual stress measurement system wherein the X-ray collimator and PSDs are located on
the far left tip. Courtesy Robert Drake, Proto Manufacturing Inc.
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(a)
(b)
Figure 4 (a) The HB-2B/NRSF2 beamline at the high flux isotope reactor. Incident snout is just visible above the detector (black, contains 7 PSDs), left.
The sample is mounted to the U-X-Y-Z stage, center. (b) The Vulcan beamline at the spallation Neutron source. Incident snout is not visible. One detector
(black, trapezoid-shaped), is on the left, another is opposite, on the right, but not visible. Cone tube, right, is the beam stop. The empty load frame is
mounted to the rotation-X-Y-Z stage, center. Note crane hook above. Both facilities are located at ORNL.
Similarly, neutron beamlines consist of a neutron source and a goniometer/sample stage. The goniometer will be in the theta-
2theta geometry often with a line, 1-D, or position sensitive detector (PSD) on the 2theta arm (see Figure 4(a)). Alternately, at
pulsed sources, the line detector(s) may be fixed at 90* 2q. In either case, the sample stage possesses X, Y, Z translation functionality
coupled with a rotation axis (see Figure 4). The translation stages should have a precision of at least 0.1 mm and a generous range of
travel (>300 mm). Since neutron samples tend to be large, the sample stage should have a >90 kg (w200 lb) load capacity, with
hoist and rigging access conveniently situated. In-situ testing, particularly mechanical loading, will require even more load capacity
(see Figure 4(b)).
1.07.2.3 Safety and Alignment

Radiation safety is paramount when working with X-rays and neutrons and is maintained through both engineering/physical and
administrative/procedural controls. Radiation exposure should be ALARA (as low as reasonably achievable). Laboratory X-ray
diffractometers typically come with fail-safe warning lights and an interlock circuit (12). Both light(s) and circuit should be
regularly tested for functionality. A Geiger counter should be obtained and regularly used to check for radiation ‘leaks,’ nontypical
X-ray bounces, and unshielded regions. The radiation generating device (RGD) custodian should ascertain the composition of the
shutter material. X-rays create ozone, which rapidly corrodes many materials, particularly in humid atmospheres (13,14). Shutter
materials, such as lead and nickel-coated brass, also corrode readily. This corrosion will typically be the root cause of the shutter
‘sticking’ open, sooner or later. Lead is also quite malleable and wears poorly. These materials should be replaced with tantalum
and 304L stainless steel, respectively, by either the manufacturer or the RGD custodian (12). If possible, a second, independent
safety circuit is recommended for laboratory X-rays. Such a circuit could check for the presence of X-rays and the status of the
enclosure door. If X-rays were present and the door open, an alarm, at a minimum, would sound a warning to the operator.
Dosimetry should be worn as required and is used to monitor individual doses. At large facilities like neutron sources and
synchrotrons, radiation control technicians and staffs are dedicated to the safe operation of all beamlines. Safety is maintained
through proper shielding and interlocks, as well as procedures. In addition to exposure risks, neutrons can activate some elements,
such as cobalt, in alloys to high levels such that the samples are not safe for public release for several decades (8). As a result,
allowances for subsequent sample sequestration/loss must be planned for, and certification to handle and store radioactive
materials should be obtained. Powders also pose a contamination hazard and must be examined in sealed and labeled containers,
which are often made of vanadium or aluminum. Neutron samples may be quite heavy, requiring sound lifting devices and
techniques. In short, the greatest opportunity for injury or radiation exposure is during instrument alignment and sample
mounting. Safe habits, clear communication, and regular maintenance afford the best opportunity to avoid injury or radiation
exposure.
Instrument and sample alignment are critical to obtaining high-quality, artifact-free X-ray (12) and neutron (8) data. When
performing residual stress studies with X-ray diffraction (XRD), a well-aligned goniometer means that the beam source, goniometer
center, and back slit are all coplanar when 2q ¼ 0* . It is also necessary to place the sample surface reproducibly on the goniometer
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Figure 5 Schematic of the neutron diffraction setup, viewed from above, showing the nominal gauge volume as defined by the slits.
(After Webster, P. J.; Wang, X.; Mills, G. Problems with Railway Rails, pp 517–524.) The direction of the measured strain component is given by
the scattering vector. Note that the instrumental gauge volume (IGV), though not shown, is actually larger than the nominal gauge volume (NGV) due
to angular beam divergence. Reproduced from Hutchings, M. T.; Withers, P. J.; Holden, T. M.; Lorentzen, T. Introduction to the Characterization of
Residual Stress by Neutron Diffraction; CRC Press: Boca Raton, FL, 2005.
center or the center of rotation. If either of these conditions is not met, erroneous peak shifts will be introduced into the data and
will be falsely interpreted as real strains. While these shifts can be corrected in principle, the time spent correcting the data would be
better allocated to aligning the diffractometer to collect accurate data in the first place. Acceptable goniometer alignment and sample
positioning can and should be verified by mounting a standard powder (e.g., LaB6, Fe, Si) on a zero background plate and then by
conducting a residual strain measurement (described later). Since the powder has no long-range stress/strain, the measurement
should reveal a negligible peak shift (<0.03* for angles >120* 2q). If significant peak shifting is observed, the goniometer alignment
and/or the sample positioning need improvement (12). Neutron instruments also require alignment and repeatable sample
positioning on the center of the goniometer. Since neutron scattering is so inefficient, neutron beamlines typically employ line
detectors to speed up data collection. The detectors need to be calibrated to remove nonlinearities in the intensity and background
responses, parallax errors, and conversion of channel to an angular position. The beamline custodians typically take care of the
detector calibration and provide evidence of same. Sample alignment, however, is often more involved than XRD, given the 3-D
nature of neutron residual stress work. Transits/theodolites and/or laser trackers are typically used to locate the center of rota-
tion of the goniometer or stage, as well as align the section of interest of the sample relative to same (15,16). Once mounted, edge
scans are typically performed to confirm that the neutron beam/gauge volume coincides with the optical readings. In an edge scan,
the sample is translated relative to instrumental gauge volume (IGV), and the intensity is monitored to determine where the edge of
the sample is located. For samples with a complicated shape, edge scanning may take several hours. Laser metrology tools and
tailored software (17,18) have been employed to reduce dramatically the number of edge scans needed (15). When the IGV (see
Figure 5) crosses a surface, either exterior (air to material), interior (material to air), or internal (material 1 to material 2), an
anomalous peak shift will result (8,19,20). As with XRD, these anomalous peak shifts can be corrected in principle. However, it is
generally best to simply keep the gauge volume fully buried in one material, which requires careful sample alignment to know the
measurement location within the sample.
1.07.2.4 Experimental Considerations

In general, efficient residual stress work that uses diffraction requires prior knowledge of the sample. This is particularly important for
neutron and synchrotron work where experimental access to these facilities is limited, and when collaboration is usually required with
beamline scientists who also have limited time with the instruments in question. In these cases, it is important to know the following
about the sample: its phase and number of phases, chemistry, average grain size, crystallographic texture, sample dimensions weight,
and any gradients in composition, texture, strain, or other characteristics. As will be discussed, these items will affect the experimental
setup and data collection strategy. A standard X-ray diffraction scan can provide insight into many of these factors.
One of the most important experimental choices is the wavelength of the radiation to be used, which is often dependent on the
sample. For laboratory sources of X-rays, changing the wavelength of the radiation requires changing the X-ray tube for one with
a new anode (and then realignment). Unlike X-ray tubes, the available wavelengths of synchrotron X-rays are not discrete, but are
continuous over an energy range. The wavelength is then selected with a monochromator. Unlike laboratory sources, however, it is
typically quite difficult to return to exactly the same wavelength if the work spans two time periods between which the
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monochromator has been moved. The same is true for a monochromator at a neutron source. For experiments where the wave-
length is constant, the position or Bragg angle of the selected peak or peaks is important. For X-ray work, it is desirable to have a peak
in the high 2q region (>130* ) for maximum sensitivity to strain and reduced sensitivity to misalignment (3,21). For neutron work,
it is typically desirable to have the diffraction peak near 90* 2q to keep the base of gauge volume approximately square (see
Figure 5). For high-energy synchrotron X-ray work, the peaks tend to be in the very low 2q region (<10* ). In addition to the peak
position, it is desirable to avoid superimposed peaks, as deconvoluting them can often be problematic. In this regard, synchrotron
radiation can be quite helpful, as it is monochromatic. A monochromatic X-ray beam reduces the number the peaks, as compared to
a laboratory source (viz., Ka1, Ka2, Kb peaks), which is important for low-symmetry phases and multiphase samples. Synchrotrons
also have the highest peak-to-peak resolution (i.e., the lowest instrumental broadening). The strain resolution or peak shift reso-
lution of any diffraction technique is governed by several experimental conditions, including peak width, working 2q region,
sample-to-detector distance, goniometer alignment, and sample position/placement, relative to the center of rotation. Typical strain
sensitivities range from 50 to 500 ppm strain.
In addition to peak position, the chemistry of the sample has an impact on the choice of radiation. X-Rays can cause samples to
fluoresce. For example, the energy of the X-rays from an X-ray tube with a copper anode will cause samples containing iron atoms to
absorb the incident radiation and then fluoresce. This raises the background level appreciably, often making it impossible to observe
weak peaks. This can be mitigated by using a different X-ray tube/anode (e.g., Co or Cr) or by employing a diffraction side
monochromator, at the cost of some diffracted intensity. This feature can be advantageous if one wants a very shallow X-ray
penetration depth. X-ray scattering power and penetration depth increase and decrease with Z, respectively. Neutron scattering and
penetration depth is not as easily described, and neutron scattering lengths and cross sections are tabulated (22). As a result, many
elements have isotopes that are strong neutron absorbers, including Li, B, Cd, and Gd. Moderate neutron absorbers include Mn, Cr,
Ag, and other elements used in common engineering materials. While not always practical, isotopes are sometimes swapped to
obviate this problem (e.g., replace B10 with B11). Neutron diffraction of materials containing water increases the background
significantly, which can be removed if the water is deuterated.
The grain size of the sample is another critical piece of information. As the grain size increases, the number of diffracting grains
decreases for a given irradiated volume. That is, powder diffraction transitions to single-crystal diffraction. Grain sizes between 1 and
10 mm are most desirable, as a large fraction of the grains will be available to diffract and will therefore provide a representative measure
of the average strain state. Grains larger than approximately 50 mm are typically problematic, as their contribution to any diffracted
peak(s) will unrepresentatively dominate the fitted peak position and interfere with data analysis (23). Peaks from large-grain materials
may have a jagged or ‘sawtooth’ appearance where each ‘jag’ is a signal from a particular large grain. Fitting a mathematical function to
such a peak profile is obviously an uncertain method to determine the average peak position. Useful powder diffraction data can
sometimes be obtained from large-grained materials by oscillating the sample about one or more axes and/or by oscillating the source.
The resultant signal and stresses are an average over the irradiated region. Another problem with large grains is that neutron diffraction
assumes both a random grain orientation and a random size distribution within the gauge volume. Large grains not only alter the peak
shape, but may also cause peak shifts, because the diffracting grains are not distributed evenly around the center of the volume.
A crystallographic texture or a preferred orientation often results from various material-forming processes that produce a micro-
structure in which the grains are not randomly but preferentially oriented; that is, not all the atomic planes are equally available to
diffract at all sample tilts or Euler angles. This condition is almost ubiquitous for coating and films, which most often exhibit a ‘fiber’
texture (4). In addition to the experimental problem of the absence of a peak at a particular tilt, the Young’s modulus should no
longer be considered isotropic for most textures and materials, and an (hkl)-dependent elastic constant will be needed. An X-ray
elastic constant can be measured, although this is not common, due to the effort required (3). Depending on the sample, useful data
can be obtained by selecting tilt angles commensurate with the texture, assuming that these are representative of the sample (4).
Sample thickness is another consideration. Coatings, layers, or regions of interest <1 mm are likely best examined with X-rays.
Since laboratory X-rays penetrate 5–25 mm, diffraction from the substrate or underlying material may need to be considered. As
mentioned above, the sampling or X-ray penetration depth can be controlled with radiation choice and angle of incidence (24)
Alternatively, layer removal via electropolishing also allows for depth profiling, but requires a correction for relaxation (3,4).
Coatings thinner than 200 nm typically require synchrotron radiation to obtain an appreciable signal in a reasonable length of
time. Neutron diffraction can usually provide information from depths wherein the attaining beam path length is <50 mm for
most materials. Increased depth or beam path may be obtained by judicious material removal that does not significantly alter the
stress state (such as drilling or cutting a hole in the side of a thick cylinder to diffract from the opposite side).
Broad diffraction peaks indicate small crystallite size and/or the presence of a gradient in the sample, for example, gradients in
plastic deformation, stress, and/or chemistry. If the gradient varies considerably with the depth of radiation penetration, the stress
analysis must account for it (25). In metal samples, broad peaks may indicate that the sample has been plastically deformed, which
may confound analysis, producing an oscillatory sin2j plot, particularly for X-rays (3). Generally speaking, such a plot should not
be used to determine a stress.
The last 12 years have yielded a wide variety of optics and detectors for X-ray diffraction, each with advantages and disadvan-
tages. Briefly, while point detectors are still the most common detector type in use, the performance and reduced maintenance of
line detectors have advanced significantly, making their use more common (26). Two-dimensional detectors have a distinct
advantage in residual stress work, as they are capable of capturing portions of or the entire Debye ring(s) of the phase(s) that are
present in a sample (27). This allows for a more complete description of the sample and more rapid data collection. Although these
detectors are being used at synchrotrons (7), cost and maintenance are limiting their present application in the laboratory. A review
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of X-ray optics is provided by Misture (28). If the standard incident and receiving slits are used for residual stress measurement, the
instrument will be quite sensitive to misalignment and sample surface displacement, such as sample surface positioning offsets
from the center of rotation of the goniometer. Of the optics choices, parallel beam detectors are particularly advantageous for
residual stress work with X-rays, as they eliminate the peak shift associated with sample surface displacement (29).
Generally, there are fewer ‘optics’ choices with neutrons. However, an important choice to consider is the size and shape
(matchstick or cube) of the gauge volume of measurement. This choice depends a great deal on whether one plans to map the stress
and/or the size of the region(s) of interest. While the smallest gauge volume commonly used is 1 mm3, this small size is conse-
quently coupled with long count times (e.g., >30 min per point) to obtain reasonable data. Generally, a gauge volume of
8–10 mm3 is used. If radial collimators are available for line detectors, these will improve spatial resolution, but they are costly and
are thus counterbalanced by a limited number of choices of gauge volume.
1.07.2.5 Measurement and Analyses

The full stress tensor can be determined from the strains measured in six different directions. In other words, a total of six strain
measurements are made, each one in a different direction. In practice, this is not done when using laboratory X-rays nor neutrons.
More than six strain measurements are typically made at various angles inclined to the sample surface in three or more azimuthal
directions (see Figure 6) in order to determine the full residual stress tensor using the sin2J technique. As laboratory X-rays are
usually low energy (<25 keV) and are highly absorbed, they cannot be used to directly measure the in-plane strain, viz. the inter-
planar spacings parallel to the horizontal plane of Figure 1, unless one has a very flat sample, parallel beam optics, and a 4-axis
goniometer for chi tilting around 88* . Figure 6(b) illustrates that diffraction occurs when the normal to the plane bisects the inci-
dent and diffracted X-rays. The tilt angle, j, is the angle between the surface and the plane normals and is parallel to the diffraction
vector. The measured strain is in the direction of the diffraction vector. The fully expanded equation relating strain to stress is (3)
$ 0 % $ %)
ε33 fj ¼ dfj ' d0 d0 ¼ a3k a3l εkl
* +
¼ ð1 þ nÞ=E$ s11 cos2 f þ s12 sin 2f þ s22 sin2 f ' s33 $sin2 j þ ð1 þ nÞ=E$s33 ' n=E$ðs11 þ s22 þ s33 Þ
þ ð1 þ nÞ=E$fs13 cos f þ s23 sin fg$sin 2j; [4]
and may be reduced to

εfj ¼ ð1 þ nÞ=E$sf $sin2 j ' n=E$ðs11 þ s22 Þ [5]
assuming a biaxial stress state of s13 ¼ s23 ¼ s33 ¼ f ¼ 0. ‘a’ and n are the directional cosine and Poisson’s ratio, respectively. The
variables and subscripts f, j, and 0 refer to the azimuthal angle, tilt angle, and stress-free, respectively. Alternatively, eqn [5] may be
expressed as follows:
dfj ¼ ð1 þ nÞ=E$sf $sin2 j$d0 ' n=E$ðs11 þ s22 Þ$d0 þ d0 [6]
Equation [6] is the classic and most often used X-ray residual stress analysis equation (3). The slope of the strain as a function of
sin2j is proportional to the residual stress in a particular direction in the sample defined by f:
sf ¼ s11 cos2 f þ s22 sin2 f [7]
sf ¼ s11 cos2 f þ s12 sin 2f þ s22 sin2 f [8]
Figure 6 (a) Definition of the sample coordinate system and the azimuthal and tilt angles, f and j, respectively. (After Noyan, I. C.; Cohen, J. B. Residual
Stress, Measurement by Diffraction and Interpretation; Springer-Verlag, New York, 1987.) (b) Schematic of the sin2J technique. showing the relative
orientation of the diffracting planes to source tilt and the incident and diffracting X-rays for J = 0 and J = 45. Note that in-plane tensile force
causes the spacing of the planes parallel and perpendicular to the force contract and expand, respectively, which causes the peaks to shift (see Figure 1
showing J = 0). J is the angle between the surface normal and the diffraction vector or scattering vector, which is the bisector of the incident and
diffracted X-rays and the normal to the diffracting planes. As the source-detector assembly is tilted about the center of rotation of the goniometer (C)
relative to the sample or vice versa, some of the grains with planes inclined to the sample surface are brought into the diffracting condition. Also
note that diffraction is discontinuous with not all grains contributing for a particular set of planes (hkl). Ultimately, the average interplanar spacing is
measured for a particular direction, f , for a series of tilts, plotted as a function of sin2J (see Figure 7b) and analyzed as described.
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An example of a ‘sin2j’ plot is shown in Figure 7(b). The y-axis is most often shown with interplanar spacing and occasionally
shows the strain or Bragg angle. Assuming that the slope from the sin2j plot is linear, the residual stress is readily determined. Other
stress states can be determined, and analyses can be performed. However, these are beyond the scope of this chapter, and the reader
should refer to (3) and (4) for more information.
Stress-free interplanar spacing is common to both the X-ray and neutron analyses. For X-ray work, the importance of this value
varies. When using the biaxial analysis (eqn [5] or [6]), the stress-free interplanar spacing has + 0.1% effect of the residual stress
values for most materials (3). In such cases, practitioners often take the value of df¼0;j¼0 as the stress-free interplanar spacing, d0. As
a result, this analysis has the distinct advantage of facilitating comparisons of one condition to another. However, if more than one
component of the stress tensor is desired, stress-free interplanar spacing has a huge impact on the final calculated stresses.
Depending on the magnitude of Young’s modulus, variations of 0.0002 Å in d0 can substantially shift the magnitude of the residual
stresses. If possible, the interplanar spacing from the same reflection is obtained from a powder of the same composition as the
solid. Sometimes a ‘sister’ sample can be comminuted into a powder with minimal effect on the desired interplanar spacing, as with
ceramics. However, this technique does not work well with metals or coatings. In these cases, the value may be calculated using the
analysis of Hauk et al. (3,4,30), provided that the s33 component is small. Alternately, the stress-free interplanar spacing can be
calculated from a stress-free lattice parameter. While the sin2j technique can be performed with neutrons, it is not commonly done,
as the desired strain can be measured directly. Given that three strains are needed to calculate a stress (see eqns [9]–[11] below), the
stress-free interplanar spacing is a critical value to have when performing neutron residual stress work. As before, powders are again
preferred in these situations, provided a sufficient quantity can be obtained (w1 cm3) and contained. For metals, this is prob-
lematic, as it is often difficult to obtain a powder with the same microstructure, precipitates, and other properties as the solid
sample. Typically, a sister sample is gently sectioned by electric discharge machining (EDM) the sample into small cubes
(e.g., 4 " 4 " 4 mm). The small cubes are then regarded as stress-free and may be stacked or arranged as needed, depending on the
chosen gauge volume. Saw cutting is not recommended, as it will tend to impart additional residual stresses into the reference.
Sometimes the stress-free interplanar spacing varies with depth. For example, carburized steels have a steep carbon gradient, which
must be accounted for with a depth dependent strain-free interplanar spacing. Cubes are cut from material with the same gradient to
the depths to be investigated. As sectioning proceeds, the cubes are marked such that their relative position and original registry are
preserved. During the setup of the neutron measurement, they can be stacked ‘anatomically correctly’ such that the chemistry effect
can be removed from the peak shift. Alternately, ‘combs’ are sometimes EDM cut in these cases. Although this method inherently
preserves the registry of the regions, experimental measurements are required in order for researchers to be convinced that the
residual stresses in the ‘tines’ are actually low. Similar concerns exist with matchstick stress-free parallelepipeds where the
dimension(s) exceed 6 mm.
After careful calibration of the neutron detectors and alignment of the neutron goniometer/sample stages, a sample(s) is
mounted and aligned with the help of transits/theodolites and/or laser trackers. As mentioned previously, during neutron
stress measurements, strains are typically measured at the same location(s) along three orthogonal directions relative to
sample shape. For a plate sample, the strains are measured at the same point in the length/longitudinal, width/transverse, and
thickness/normal directions. For a cylinder, the strains at the same point are measured in the axial, hoop/circumferential, and
radial directions. Usually, shear strains/stresses are not measured or determined. Two of the three measurements of strain can
Figure 7 (a) A photograph of a microdrill bit. The diameter of the fluted end is 1.15 mm. (b) The strain as a function of sin2j for the drill bit routed at 60 s
per cycle.
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be achieved in one sample mounting simply by rotating the sample 90* . The measurement of the third component requires
unmounting the sample, rotating it 90* appropriately, and remounting. Sample mounting can also be aided by the use of
transits/theodolites and/or laser trackers followed by edge scans. The stress-free reference sample should be periodically
measured throughout the run to generate replicate measurements. This also serves a general monitor of the work, such that
any significant deviations in the peak position, intensity, and/or width could alert or confirm that a collision between the
sample, fixturing, etc. and the incident snout, detector, etc. has occurred and that subsequent data and the setup are
compromised.
Once the data are collected and the peaks fit or the lattice parameter is refined, the total average strain within the gauge volume is
determined from the shift in the interplanar spacings of the planes within the diffracting grains, relative to the interplanar spacing of
a strain-free reference sample (eqn [2]). The measured strain is an average of the strains over the large number of diffracting grains
within the sampling volume. Assuming negligible plastic deformation, Hooke’s law is then used to transform the strain
measurements to residual stresses by (3):
E
s11 ¼ " ½ð1 ' yÞε11 þ yðε22 þ ε33 Þ( [9]
ð1 ' yÞð1 ' 2$yÞ
E
s22 ¼ " ½ð1 ' yÞε22 þ yðε11 þ ε33 Þ( [10]
ð1 ' yÞð1 ' 2$yÞ
E
s33 ¼ " ½ð1 ' yÞε33 þ yðε11 þ ε22 Þ( [11]
ð1 ' yÞð1 ' 2$yÞ
1.07.2.6 Example: Residual Stresses Developed in Micro Drills

Tungsten carbide micro drills are used to drill very small holes in computer boards and may fracture in use at the base of the ‘flute’ or
cutting portion of the bit. The flute is the helix portion of the bit (see Figure 7(a)). (This research through the Oak Ridge National
Laboratory’s High Temperature Materials Laboratory User Program was sponsored in part by the U. S. Department of Energy, Office
of Energy Efficiency and Renewable Energy, Vehicle Technologies Program.) The manufacturer of the drill bits was concerned that
the routing or ‘fluting’ process was introducing deleterious residual stresses into the bits. To examine this problem, the residual
stresses within the flutes of several drills were measured and correlated to the fluting speed. Since machining mostly changes the
surface, X-rays should be used in this case. Since the surfaces are curved and the area of interest is small, the X14A synchrotron
beamline at National Synchrotron Light Source at Brookhaven National Laboratory (31) was selected because of its parallel, high-
intensity beam. A six-axis Huber goniometer was employed using psi geometry for tilting and a point detector (3). Parallel beam
optics were achieved with the incident parallel X-ray beam and the receiving side Ge analyzer crystal (d ¼ 3.266 Å). The beam was
0.3 " 0.3 mm in size in order to measure ‘inside’ the flute. To get a better average in light of the small spot size, the sample was
rocked ) 5* about the U axis to improve particle statistics and averaging. The WC phase was cubic with a 6–8 wt.% Co binder phase
and possessed a grain size of 1–10 mm. The residual strains were measured using the (211) WC reflection at a nominal 2q 118.6* ; the
wavelength was 1.551 Å. The sin2j plots were found to be reasonably linear (see Figure 7(b)), and the stresses were calculated using
eqn [5]. The stress-free interplanar spacing was determined from WC powder and found to be 0.9017 Å. The Young’s modulus and
Poisson’s ratio were taken as 724 GPa and 0.19, respectively. The WC drill bits machined at low, regular, and high fluting speeds of
87, 73, and 60 s per cycle possessed average residual stresses of –210 ) 40, –340 ) 40, and '410 ) 110 MPa, respectively. The
correlation of these residual stresses with manufacturing methods and the probability of breakage assisted the manufacturer in
producing more reliable drill bits.
1.07.2.7 Concluding Remarks about Powder Diffraction Residual Stress Measurements

Neutrons and high-energy X-rays, in particular, are used for mapping (15) as well as for in-situ loading studies (8). It should be
noted that diffraction measurements are ‘discontinuous’ (see Figure 6(b)). That is, an area or a volume containing grains is
irradiated, but only a subset of those grains is oriented such that it can diffract. Bonda and Noyan (32) studied the plastic
deformation of a solder using the SEM. Their micrographs clearly show that plastic deformation is inhomogeneous on the grain
length scale. As a result, it is important to get a large number of grains to diffract so as to obtain a representative signal or measure
of the residual stress. Further, diffraction measures only elastic strains, not plastic. That is, during slip, the interplanar spacing
should not change. Figure 8 schematically shows the elastic residual strain measured in a material that has been plastically
deformed. In Figure 8, the top bar has no applied stress and no plastic deformation. When tensile loading above the yield stress
occurs, the material plastically deforms, but in this case, deformation only occurs within the dotted circle/oval region. In the third
bar down from the top, the deformed region is removed, while still under load, from the remaining elastically deformed bar. Next,
the applied tensile load is removed from both the bar and the deformed region; there is presently no residual stress. The elastic
residual stress that the diffraction measures is the one that originates from ‘putting’ the deformed oval region back into the circular
hole in the bar. Particularly with the sin2j, plastically deformed materials exhibit oscillatory sin2j plots, which cannot be
explained by eqn [5] or [6].
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Figure 8 A schematic showing a region within a bar being plastically deformed and the resultant elastic residual stress left afterward. Here, s, PD, and V
are the applied stress, plastic deformation, and void, respectively.
Residual stress measurements using diffraction can provide information from both the surface and the bulk of crystalline
materials using X-rays and neutrons, respectively. Although occasionally the samples need to be sectioned, diffraction itself is
nondestructive when using the interplanar spacings with the grains as built-in strain gauges. Stress/strain can be measured as
a function of phase and can be discerned on three microstructural scales: macro, micro, and nano. Strain anisotropy as
a function of crystallographic direction can be studied, particularly with spallation or pulsed neutron sources. Measurements
can take minutes to hours to complete with nominal spatial resolutions of 5 " 5 mm2 and 1 mm3 or greater with X-rays and
neutrons, respectively.
1.07.3 Introduction to Hole-Drilling
The hole-drilling method is one of the most commonly used methods for measuring residual stresses. It is straightforward to
implement, the equipment required is of relatively modest cost, it can be used with a wide range of materials and specimen
geometries, and it gives reliable results. The method involves drilling a small hole in the test material, typically 1–4 mm in diameter
(but could be orders of magnitude smaller or larger), and with a depth approximately equal to its diameter. The deformations in the
surrounding material surface are then measured, and the residual stresses that originally existed within the hole are calculated. The
most common way of measuring the surface deformations is by using strain gauges, such as those shown in Figure 9(a). In recent
years, the use of full-field optical techniques, such as Electronic Speckle Pattern Interferometry (ESPI), Moiré Interferometry, and
Digital Image Correlation (DIC) have also been introduced for measuring surface deformations.
The ring-core method is an ‘inside-out’ variant method, with the measurement made in the center area and the ‘hole,’ in this case
an annular groove, cut in the surrounding area. Typical inner diameters for the groove are in the range of 15–150 mm, with a depth
equal to 25–150% of that dimension. The residual stress computation method is mathematically the same for both the hole-drilling
and ring core methods, with the only difference being the numerical values of the calibration constants used.
The deep-hole method is a further variant approach that is useful for determining the residual stresses within the interior of
a given material. The method combines the hole-drilling and ring-core methods and involves drilling a deep hole into the test
material, then measuring the change in diameter as the surrounding material is overcored. An important feature of the method is
that the measurements are made in the interior of the hole rather than at the surface. Thus, the evaluated residual stresses are in the
deep interior rather than near the surface. The diameter change can be monitored along the entire length of the deep hole, creating
a detailed stress versus depth profile.
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Figure 9 Hole-drilling methods: (a) conventional hole-drilling method, (b) ring-core method, and (c) deep-hole method. Schajer, G.S. Relaxation
Methods for Measuring Residual Stresses: Techniques and Opportunities. Exp. Mech. 2010, 50(8), 1117–1127.
1.07.3.1 Features of Hole-Drilling

The hole-drilling and ring core methods are often described as semidestructive. The removal of material is limited in extent and
often it is either tolerable or can be adequately repaired. Both measurement methods also share the advantage of being relatively
rapid and convenient in practice.
The ring core method has a greater strain/stress sensitivity than the hole-drilling method because it involves almost complete
relief of the surface strains in the central core. By comparison, the hole-drilling method involves only partial strain relief in the
material around the hole, typically about the size of a US quarter coin. The ring core method is also tolerant of any minor diameter
errors or eccentricity of the annular hole, with respect to the strain gauges. In addition, it is less sensitive to stress concentration
effects than the hole-drilling method, and it can evaluate stresses near the material yield stress. However, the size of the annular ring
is relatively large, causing much more damage than the hole-drilling method. Also, the results are much less localized because the
hole/ring diameter defines the area of residual stress measurement. Another concern of the ring core method is that it is less
convenient to perform, particularly when using strain gauges, because the central wiring gets in the way of the slot cutting.
The hole-drilling method has complementary advantages and disadvantages when compared with the ring core method. It does
relatively little damage to the specimen, and it allows much more localized residual stress measurements. Also, the strain gauge
connections need not be disturbed for the drilling of the hole. However, the hole-drilling method is relatively insensitive, and any
error in diameter measurement or eccentricity of the hole with respect to the strain gauges can introduce significant errors in the
residual stress calculation.
Despite its potential disadvantages, the hole-drilling method is usually the most common choice for measuring strains. The
method is very well established, both experimentally and theoretically. The availability of specialized precision drilling equipment,
together with well-proven experimental procedures, substantially mitigates the potential disadvantages of hole-drilling. The much
lower amount of damage to the specimen, the more localized measurements, and the more convenient measurement procedure are
the key advantages.
The deep hole method differs fundamentally from the hole-drilling and ring core methods in that the deformations are
measured within the hole rather than at the surface. As a result, the deep hole method is able to identify residual stresses in the deep
interior of a specimen. This is a significant feature when working with large specimens, even those on the geological scale. However,
the method requires specialized equipment and expertise and, as a result, is much less widely applied than the standard hole-
drilling method of measurement.
1.07.3.2 History
The hole-drilling method dates from the pioneering work of Mathar in 1934 (33). He used a mechanical extensometer to measure
the displacements around a circular hole that was drilled through a stressed plate. Later, Soete and Vancrombrugge (34) greatly
improved measurement accuracy by using strain gauges instead of a mechanical extensometer. The ring core method was introduced
by Milbradt (35) in 1951 as a more sensitive alternative to the hole-drilling method. The deep hole method dates from 1958 in the
work of Hast (36) and measures stresses deep within rock formations. The method was adapted by Smith (37) to measure residual
stresses within metal castings.
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In 1956, Kelsey (38) published the first investigation into residual stress variation with depth by using the hole-drilling method.
He was also the first to use blind holes instead of through holes. The modern application of the hole-drilling method dates from the
work of Rendler and Vigness (39) in 1966. They developed the hole-drilling method into a systematic and easily reproducible
procedure, and defined the geometry of the ASTM E837 (40) standard hole-drilling strain gauge rosette.
Modern finite element numerical techniques allowed the replacement of earlier empirical calibrations, such as those of Beaney
(41). The ability to perform calculations for loading cases that would be difficult or impossible to achieve experimentally provided
the opportunities for developing advanced calculation methods, such as those described by Schajer (42,43).
In recent years, the use of optical techniques for measuring the surface deformations around the drilled hole has attracted a great
deal of interest. The advantages of such measurements are that they are ‘full-field’ and are thus data-rich. They are also noncontacting
and do not require the time-consuming attachment of strain gauges. Nelson (44) described the use of laser holography in 1985, Lu
et al. (45) described Moiré Interferometry in 1988, and McGinnis (46) described the use of digital image correlation in 2003. Further
developments in the use of optical measurements and in the hole-drilling technique in general continue apace, with several dozen
new publications on these techniques appearing annually. The original measurement concept of Mathar in 1934 has proven to be
a fertile area for research, with no sign of slowdown in further developments.
1.07.3.3 Drilling Technique

The drilling of the hole for residual stress measurements must be done with significant care to avoid introduction of errors. There are
three main error sources: the introduction of machining stresses (adding to the residual stresses to be measured), a noncylindrical
hole shape, and the eccentricity of the hole relative to the strain gauge rosette.
Early hole-drilling work was done using conventional twist drills and drilling speeds (39). To improve hole quality and reduce
machining stresses, the use of milling cutters and dental burrs was introduced to give square-bottom holes of well-defined depth,
which simplified the associated stress/strain calibrations. The air turbines commonly used to drive dental burs provided a further
advance in drilling technique. Their high rotation speeds (40 000 to 400 000 rpm) were found to significantly reduce machining
stresses (47) and thereby decrease induced artifacts in the computed residual stresses. In addition, it was found to be advantageous
to orbit the cutter in a circular path, as shown in Figure 10, which creates a hole larger than the cutter diameter. Such orbiting
motion shifts much of the cutting action from the end-surface cutting edges to the side-surface cutting edges and provides a freer exit
path for the removed material, with both features helping to reduce machining stresses. The orbiting motion can also help improve
hole circularity and concentricity. Orbiting motion with a much larger orbit radius is used with the ring core method. In modern
practice, sophisticated equipment for hole-drilling and ring-coring measurements are commercially available, and can be coupled to
computerized control and data acquisition systems.
1.07.3.4 Deformation Measurements – Strain Gauges

The modern application of the strain gauge hole-drilling method became established through the work of Rendler and Vigness (39)
in 1966. They formalized a standard strain gauge geometry for residual stress measurements and developed the hole-drilling
method into a systematic and repeatable procedure. Their work provided the basis for establishing ASTM Standard Test Method
E837 in 1981, which has been updated several times since then (40).
There are now three standardized hole-drilling rosette designs, which are illustrated in Figure 11. Type A is the Rendler and
Vigness design and is suitable for general-purpose use. Type B is conceptually similar, but has all the strain gauges arranged on one
side of the hole location. This arrangement enables the rosette to be used for measurements adjacent to an obstacle. Because of its
one-sided geometry, the Type B rosette is more sensitive to the effects of hole eccentricity errors. Thus, the more symmetrical Type A
rosette is preferred for use when there is no nearby obstacle. The Type C rosette is a six-element design consisting of three pairs of
Figure 10 Orbiting technique for hole-drilling residual stress measurements. Image courtesy of Philip Whitehead, Stresscraft Ltd.
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Figure 11 ASTM E837 standard hole-drilling strain gauge rosette designs. Determining Residual Stresses by the Hole-Drilling Strain-Gage Method.
ASTM Standard Test Method E837-08. American Society for Testing and Materials, West Conshohocken, PA..
strain gauges to be connected as half-bridges. This arrangement provides thermal compensation and increased sensitivity, making
the Type C rosette a good choice for materials with poor thermal conductivity or with low residual stresses, but at the cost of
increased wiring effort and overall expense. A large collection of literature on strain gauge hole-drilling measurements has been
developed, with descriptive information (48), a good practice guide (49), and measurement accuracy analysis (50).
1.07.3.5 Deformation Measurements – Full-Field Optical Techniques

Starting in the 1980s and 1990s, several optical techniques have been introduced for evaluating residual stresses by the hole-drilling
method. These techniques have the advantage of providing full-field data, which are useful for data averaging, error checking, and
extraction of detailed information. The optical methods generally require fairly controlled conditions, while the traditional strain
gauges are much better suited to field use. The two measurement approaches also have opposite cost characteristics, with optical
methods having high equipment cost but relatively low per-measurement cost, and strain gauges having relatively low equipment
cost but high per-measurement cost.
Three main optical techniques have been applied so far to hole-drilling residual stress measurements: Moiré interferometry,
holographic interferometry, and digital image correlation. When using Moiré interferometry (45,51), a diffraction grating consisting
of finely ruled lines, typically 600–1200 lines mm'1, is attached or made directly on the specimen surface. This area is illuminated
by two symmetric light beams derived from a single coherent laser source. Diffraction of the light beams creates a ‘virtual grating,’
giving interference fringes that consist of light and dark lines that are imaged by a video camera. The fringe lines represent contours
of in-plane surface displacement typically at intervals of about 0.5 mm.
Holographic interferometry (44) provides a further important method for measuring the surface displacements around a drilled
hole. A modern variant, ESPI (52,53), has become popular because its use of a video camera allows ‘live’ fringe patterns to be produced
by image subtraction. Figure 12 shows an example of an ESPI fringe pattern that is created by hole-drilling. In-plane, out-of-plane, or
surface slope ESPI measurements are possible but depend on the optical configuration used. A significant feature of ESPI is that it can
work with a plain specimen surface without attachment of the diffraction grating needed for Moiré measurements. This makes it
possible to perform ESPI measurements rapidly, and the potential exists to use this method as an industrial quality control tool.
DIC is another optical technique that can be used for hole-drilling residual stress measurements (46,54). The technique involves
painting a textured pattern on the specimen surface and imaging the region of interest using a high-resolution digital camera.
Figure 12 ESPI fringe image observed during a hole-drilling residual stress measurement.
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The camera, set perpendicular to the surface, records images of the textured surface both before and after deformation. The local
details within the two images are then mathematically correlated and their relative displacements are determined. The algorithms
used for performing this technique have become quite sophisticated, and with a well-calibrated optical system, displacements of
) 0.02 pixel can be resolved. When using a single camera, DIC can identify displacements in two in-plane directions.
1.07.3.6 Uniform Residual Stress Calculation

Two types of hole-drilling residual stress calculations are possible: the first in which the in-plane stresses can be assumed not to vary
with depth from the specimen surface, which are so-called uniform stresses; and the second in which they do vary with depth, which
are called stress profiling. The first case is the simpler one because there are only three unknown in-plane residual stresses to be
determined from the measured data. The simplest experimental procedure involves measuring the deformations as the hole is
directly drilled from zero to ‘full’ depth, approximately equal to the hole diameter. When making measurements in a thin-plate
specimen, the hole goes all the way through the material.
For the uniform stress case, when making strain gauge measurements, three strain measurements are taken to evaluate the three
unknown residual stresses. The relationship between the measured strain and the in-plane residual stresses is as follows:
sx þ sy að1 þ nÞ sx ' sy b b
ε¼ þ cos 2q þ sxy sin 2q [12]
2 E 2 E E
where sx, sy, and sxy are the in-plane Cartesian stresses, and q is the angle between the strain gauge axis and the x-direction. a and b
are calibration constants that define the strain/stress sensitivity of the measurement. Hole-drilling only partially relieves the strains
at the strain gauge location, which is typically just a third of the residual strain. Thus, the measured strains tend to be small, causing
the relative effect of noise to be large. Equation [12] can also be applied to the ring core method, but with different numerical values
of the two calibration constants. Because the ring coring relieves all the residual stress, the measured strains and the calibration
coefficients are significantly larger than for hole-drilling.
When making optical measurements with hole-drilling, surface displacements are measured rather than surface strains. Equation
[12] still applies, with surface displacement replacing surface strain on the left side. The numerical values of the corresponding
calibration constants are different, but the trigonometric form of the equation is preserved.
A practical way to improve residual stress evaluation accuracy when hole-drilling is to make strain measurements at a series
of small depth increments, as the hole is drilled from zero to full depth. All measured data can be considered, outliers
identified and removed, and an averaging method used to minimize the effect of measurement noise (55). The use of eight hole
depth increments is specified in ASTM E837 (40) and is an effective procedure for improving the quality of residual stress
evaluation.
In early strain gauge work, calibration constants a and b were evaluated experimentally by using measurements that were made
on specimens with known applied stresses (39). This method is practical for uniform stress measurements, although it is time
consuming. In later years, finite element calculations were introduced to provide the necessary calibrations (42). These calibrations
are much more consistent than experimental values. Detailed modeling of the strain gauges is necessary to achieve accurate results.
The notation for the calibration constants using a superscript ‘bar’ acknowledges the averaging over the strain gauge area. Previously,
point strain values were sometimes used.
An interesting example of a case where eqn [12] does not apply is for hole-drilling residual stress measurements in an orthotropic
material. The strain/stress relationship is not trigonometric, requiring the residual stresses to be evaluated in a more complex matrix
format using seven calibration constants (56).
A significant limitation of the hole-drilling method is that the hole creates a stress concentration that can cause localized
plastic deformations if the nearby residual stresses are sufficiently high. Typical residual stress computation methods, such as
those described by eqn [12], rely on material linearity. The localized yielding near the hole boundary caused by stress
concentrations starts to cause noticeable deviations from linearity for residual stresses that are greater than 60% of the material
yield stress. Fortunately, in most cases, the effect is to overestimate the size of the residual stress, often to values significantly
above the material yield stress. As a result, the existence of problematic results is readily apparent. If the stress–strain response of
the test material around the yield point is known in detail, then specialized correction procedures can be used to allow evaluation
of residual stresses up to 90% of the material yield stress by using the hole-drilling method (57). The ring core method does not
require such corrections because it is much less influenced by stress concentrations; as a result, it can directly evaluate residual
stresses that are near the yield stress.
1.07.3.7 Residual Stress Profile Calculation

The more general case of residual stress evaluation occurs when the stresses vary with depth from the specimen surface. This process
is called stress profiling. The stress calculation is completed using the deformation data measured at a sequence of hole-depth
increments. Early strain gauge methods for evaluating the stress profiles (38) relied on experimental calibrations of the strain versus
stress relationships. These methods were approximate out of necessity because the experimental calibrations could not provide all
the necessary detailed calibration data. The subsequent development of finite element calculations provided the necessary data (42).
For stress profiling calculations, the Integral method provides a direct generalization of the uniform stress calculation method, with
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Figure 13 Response components of a profile stress calculation. Determining Residual Stresses by the Hole-Drilling Strain-Gage Method. ASTM
Standard Test Method E837-08. American Society for Testing and Materials, West Conshohocken, PA.
eqn [12] rewritten in vector-matrix format. The strain ε becomes a vector of strains measured after a series of small increments in
hole depth. The various stresses s and s become vectors of the stresses contained within the hole-depth increments. The calibration
constants a and b become matrix quantities that relate the various stresses and strains.
Figure 13 shows a physical interpretation of matrix a. Coefficient a32 represents the strain caused by a unit stress within
increment 2 of a hole that is 3 increments deep. The matrix is lower-triangular because only stresses that exist within the hole
contribute to the measured strains.
Figure 13 illustrates the significance of the finite element calibrations because the various coefficients shown cannot be deter-
mined using experimental calibrations. The matrix equations to determine the residual stresses from the measured strain data are
‘inverse’ equations, whose solution is very sensitive to any modeling or data errors. Thus, the accuracy and consistency of the finite
element results are very important, and strict attention must be paid to a meticulous experimental technique. In mathematical
terms, the computational error sensitivity derives from the numerical ill-conditioning of matrices a and b. The small size of their
diagonal elements reduces the matrix determinants almost to zero. A computational technique called regularization can be used to
stabilize the matrices and reduce the sensitivity to measurement noise (58).
Although much more complex and sensitive to error than uniform stress evaluations, stress profiling hole-drilling measurements
are now widely used. The ASTM Standard Test Method E837 (40) has recently been revised to include a standardized procedure to
evaluate residual stress versus depth profiles.
1.07.3.8 Stress Computation from Optical Data

Most of the early development of residual stress computation methods from hole-drilling data related to strain gauge measure-
ments. These keep calculations to a moderate size because the typical three-element strain gauge rosettes provide the minimum data
set required to determine the three in-plane residual stresses. Optical measurements introduce both a challenge and an opportunity
through their massive quantity of full-field data from hundreds of thousands and even millions of pixels. The data quantity greatly
exceeds the number of discrete measurements available from strain gauges. Initial optical measurements for hole-drilling used
calculation methods parallel to those used for strain gauges (44). Typically, they involved visually picking a small number of
opportune points within the measured image, interpreting their fringe orders, and then performing a strain-gauge-style calculation.
More recently, full-field methods using a linear least-squares approach (54) have been applied successfully. Nonlinear procedures
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can also be used, but only when essential, because they are much more computationally intensive and potentially less stable. With
careful data management and choice of computation technique, the required handling of large quantities of data is not excessively
burdensome, especially with modern computer equipment.
1.07.3.9 Concluding Remarks about Hole-Drilling

The hole-drilling method for measuring residual stress has grown to become a well-established and widely accepted technique with
its own ASTM Standard Test Procedure (40). The method is fairly straightforward to implement; it can be used with a wide range of
materials and specimen geometries; the required equipment has a relatively modest cost; and it gives reliable results. Even though
the method is now long established, major advances in the technique continue, notably in full-field measurement techniques and in
residual stress computation procedures. The fundamental measurement principle is a wide-ranging and flexible one, and such
advances can be expected to continue well into the foreseeable future.
1.07.4 Introduction to Piezospectroscopy
A group of techniques that are collectively called piezospectroscopy can be used to measure local stresses in ceramics, glasses, and
polymers (59–62). These techniques rely on the linear peak shifts of characteristic energy levels (electron or vibrational) of cova-
lently bonded materials that correlate directly to stress in the material. Photo-stimulated luminescence spectroscopy, vacuum
ultraviolet, Fourier transform infrared (FT-IR), and Raman spectroscopy have all been used to measure stress; however, only
luminescence and Raman (which operate in the visible range) can obtain a spatial resolution of w1 mm, far exceeding the spatial
resolution of standard X-ray techniques and strain gauge measurements. One can also perform depth profiling, depending on the
transmittance of the material being examined. In addition, the time to generate data is greatly reduced as compared to neutron
diffraction methods that are currently more suited to extracting stress gradients on a macroscopic scale. Piezoluminescence measures
the shifts of electronic energy levels of impurity ions in crystals. The peaks are usually intense and exhibit large linear shifts with the
applied or residual stress level; however, piezoluminescence is only applicable to a handful of materials, most notably Al2O3, where
the so-called R-lines produced by Cr3þ impurities are used (63). Alternately, piezo-Raman spectroscopy can be performed on most
covalently bonded materials; however, it suffers from weaker peaks and smaller stress-induced peak shifts. In the case of piezo-
Raman spectroscopy, the peaks are vibrational and the shifts arise from the anharmonic nature of the crystal bonding (64).
Unfortunately, neither of these techniques works with metals, as the incident light must interact with localized electrons that are not
present in metals.
Piezo-Raman spectroscopy and piezoluminescence utilize the same equipment, which consists of a laser that is focused on the
sample through a standard optical microscope. Some of the Raman scattered or luminescent light is then collected back into the
microscope and directed into a spectrometer, where it is dispersed and detected using a charged-coupled device (CCD). The
microscope can either be used to view the sample surface or to collect spectra. Laser light may also be delivered with a fiber-optic
probe or with a long working-distance lens for measuring inside furnaces or high-pressure vessels. The strengths and weaknesses of
these two piezospectroscopic techniques will be discussed in relation to one another and in context with other stress-measurement
approaches.
1.07.4.1 Piezoluminescence
Rare-earth and transition metal ions have unpaired f-shell and d-shell electrons, respectively. These electrons can interact with
electromagnetic radiation through a radiative transition, either emission or absorption, between two energy levels. The strength and
energy of the transition are determined by the electron configuration and binding energy of the metal ion. When doped in a crystal,
the outer-shell electrons of the metal ion interact with the crystal field to shift and split the electronic energy levels. Some examples
of dopant ions in crystals that exhibit characteristic emission lines include Cr3þ in MgO (65), Nd3þ in YAG, Fe3þ in Al2O3 (66), and
Er3þ in ZrO2 (67).
Perhaps the most well-known example of metal ion luminescence is that of ruby, which has two red lines or R-lines caused by
Cr3þ dopant ions in a-Al2O3, which occur at w693 nm. Incident light is absorbed into the blue and green absorption bands,
nonradiatively de-excites down to the two energy levels corresponding to the R-lines (14 430 and 14 400 cm'1), and then de-excites
down to the ground state, which produces the ruby’s characteristic luminescence. The R-lines are very intense, and since chromium
is ubiquitous in alumina, the R-lines are always observed in alumina with no need of additional doping. A single stress
measurement can be collected in less than 1 s, which allows for mapping of stress across a surface in a reasonable amount of time.
Typical luminescence spectra of alumina are shown in Figure 14.
If the unit cell of Al2O3 is distorted, then the energy levels of Cr3þ will shift slightly in response to the change in the crystal field.
Therefore, a strain will cause the R-lines to shift. This is the source of the piezospectroscopic effect. This stress-induced peak shift has
been widely used as a stress calibration for diamond anvil cells (68–72). The potential of using the R-lines as a stress sensor was first
suggested by Wachtman in 1972 (68). Grabner first demonstrated the use of piezoluminescence for measurement of stress in dense
alumina in 1978 (73). A phenomenological description was later derived by Ma and Clarke for a generalized stress state in
polycrystalline alumina (63), and a shortened version is presented below.
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Figure 14 Example of the stress-induced peak shift of the R-lines of a-Al2O3 measured at room temperature. The alumina phase goes into tension
as the mullite content increases due to the CTE mismatch between the two phases.
The stress-induced peak shifts (Dn) of the R-lines of alumina are described by the piezospectroscopic coefficients Pij by the
equation:
Dn ¼ Pij scij [13]
c
where s ij is the stress in the crystal frame of reference which can be rotated into a general frame of reference using the direction
cosines aij by the equation:
scij ¼ aik ajl skl [14]
Pij is a second rank tensor and is limited by the symmetry of sapphire (D3d) to be:
2 3
P11 0 0
Pij ¼ 4 0 P22 0 5 [15]
0 0 P33
The three piezospectroscopic constants for both R-lines have been measured (74) and are shown in Table 1.
Combining eqns [13] and [15], we obtain the equations for peak shift in the crystal frame of reference:
DnR1 ¼ 2:56s11 þ 3:50s22 þ 1:53s33
[16]
DnR2 ¼ 2:65s11 þ 2:80s22 þ 2:16s33
where the units of Dn and sij are cm'1 and GPa, respectively. For polycrystalline alumina, the direction cosines, aij, of eqn [14] can be
integrated around all directions to obtain the isotropic stress-induced peak shift:
poly
DnR1 ¼ 7:59sh
[17]
poly
DnR2 ¼ 7:61sh
Table 1 Piezospectroscopic coefficients of ruby
P11 P22 P33 P11 þ P22 þ P33
R1 2.56 3.50 1.53 7.59

R2 2.65 2.80 2.16 7.61
All values are in cm'1/GPa.
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where sh is the trace of the stress tensor or hydrostatic stress (sh ¼ sii/3). The constants in eqn [17] are simply the trace of sij in eqn
[15]. Therefore, only the hydrostatic stress can be measured in polycrystalline alumina with piezoluminescence, assuming that
enough grains are sampled for the sake of averaging. The R1 line has been found to have a slightly nonlinear peak shift with stress, so
only the less intense R2 line should be used. Figure 14 shows an example of the stress-induced R-line shift. Stress was measured in
an alumina/mullite composite, and the tensile stress in the alumina increased with increasing mullite content, due to the coefficient
of thermal expansion (CTE) mismatch between the two phases (75).
In addition to applied and residual stress, the R-lines will also shift with changes in the chromium concentration (76). An increase
in 1 wt.% Cr will result in a peak shift of 1 cm'1, which would appear as a hydrostatic tensile stress of 130 MPa. In fact, this peak shift
is also caused by the stress generated from substituting the larger Cr atom for Al; however, in most cases, the changes in stress from
other factors and not from chromium concentration are desired. Therefore, one must take into account the possibility of varying
chromium concentration, which may occur in alumina scales that are grown on alloys containing large amounts of chromium.
Another potential source of error is the peak shift induced by temperature, which is '0.135 cm'1 per * C and would appear as an
effective stress of '17.7 MPa per * C. This is a substantial peak shift, so care must be taken to maintain a constant room temperature
during data acquisition. Also, the incident laser may generate enough heat to cause the peaks to shift. Therefore, prior to measuring
a new sample, a trend of peak shift versus laser power should be acquired, and a low enough power should be selected such that no
temperature-induced shift is generated. This large peak shift with temperature makes it difficult to measure the stress in alumina at
elevated temperatures where temperature fluctuations across the sample may occur. In addition, the R-lines become less intense as
temperature increases, and eventually disappear above 200 * C. For high-temperature stress measurement, one must use diffraction
techniques or Raman spectroscopy.
One approach to reduce sources of error is to frequently calibrate the measurement tools with a zero-stress reference. This
reference could be a measurement far away from a stress concentrator of interest in the same material, or a free-standing powder
with a low-chromium concentration. It is recommended that the NIST standard reference material 676A, which is a pure unstressed
Al2O3 powder used to calibrate X-ray diffractometers, be used as a standard. Subtracting the zero-stress reference peak position also
removes errors associated with the instrument calibration and room temperature changes that may also be affecting the spec-
trometer or gratings. Following this approach, a stress resolution below 10 MPa can be achieved.
Clarke et al. have done extensive research on the stress-induced peak shift of the alumina R-lines and have applied the technique
to a number of materials problems. The stress in polycrystalline alumina was measured as a function of grain size and was compared
to theoretical predictions of the internal stress caused by thermal expansion anisotropy (77). The residual stresses in sapphire fiber
composites were measured during fiber push-out (78), and stresses in laminate systems have been compared to theoretically
predicted stresses (79).
More recently, researchers have used piezoluminescence to measure stress in thermally grown alumina scales on metal substrates
(61,62,80). This technique is ideally suited for oxide scales, since the stresses created by the CTE mismatch between the metal and
the substrate are usually very large (>1 GPa), and the resulting R-line shifts can be easily observed. Also, the stress state is often equi-
biaxial, which simplifies the analysis. The R-lines are so intense that stresses can be measured nondestructively in an oxide scale
through a 250-mm-thick zirconia thermal barrier (81).
1.07.4.2 Piezo-Raman
The Raman effect was first predicted by Smekal in 1923 (82) and then measured with benzene in 1928 by the Indian physicist C.V.
Raman (83). The intensity of Raman-scattered light is extremely weak, with only one out of every billion or so incident photons
interacting with a typical material through the Raman effect. Consequently, the use of Raman spectroscopy has been severely limited
by deficiencies in instrumentation and not by a lack of theoretical understanding.
Early Raman spectra were obtained with mercury lamps as the excitation source, which are difficult to use and have relatively low
emission intensities. With the advent of lasers in the 1960s, Raman spectra became much easier to excite and detect. The first laser
Raman spectrum was acquired by Porto and Wood (84), which renewed interest in Raman spectroscopy as an analytical tool. In the
mid-1970s, Raman microscopy was introduced (85), which combined a spectrograph with a standard optical microscope, allowing
measurements of samples in the picogram range. Detector technology also improved during this period with the introduction of
CCD detectors (86). Using advanced coatings to increase the signal at the CCD chip, the quantum efficiency of these detectors
approaches 90%, almost allowing for the detection of individual photons. Other improvements came in monochromator design
such as holographic gratings and nondispersive techniques such as Fourier transform Raman and holographic notch filters, used to
remove stray light from the laser excitation line. The current state of the art includes the use of fiber-optic probes for remote
sampling in industrial environments, portable Raman spectrographs for on-site analysis, and near-field Raman microscopy for high-
resolution work.
Raman spectroscopy measures the characteristic vibrational frequencies of molecules and crystals. The Raman effect is initiated
by irradiating a sample with a monochromatic light source. Some of the light will scatter inelastically by creating or destroying
a vibration, thereby producing Raman peaks (87). Molecular or crystal vibrations can be estimated using a ball-and-spring model,
where the angular frequency of the vibration, u, is:
sffiffiffiffiffiffiffi
K
u¼ [18]
mm
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where K is the force constant of the spring and mm is the reduced mass of the vibrating balls. This simple model provides insight into
what may affect the Raman spectrum of a material. Nonstoichiometry, solid solutions, the presence of defects, and different isotopes
will alter the mass of the atoms (mm) in a crystal; consequently, the Raman spectrum may be affected. Similarly, any change in
a material that affects its bonding (K), such as phase transformations, amorphous phases, nonstoichiometry, crystal disorder, and
crystallite size may also alter the Raman spectrum. A third category that affects vibrational energy levels arises from considering that
eqn [18] is valid only for perfectly harmonic bonds, that is, bonds with parabolic potential energy wells. Since no bonds are perfectly
harmonic, the force constant K will become a function of strain in the bond, and since K affects the frequency of vibration, Raman
peaks will shift with strain. For polycrystalline materials, the peak shift is linearly related to the hydrostatic stress in the crystal
through a calibration constant that is similar to the result found for piezoluminescence in eqn [17] (88). Owing to the weakness of
the Raman effect, typical acquisition times for a single spectrum range from tens of seconds to minutes, depending on the material
and experimental setup.
Anastassakis and Bernstein were the first to present a calculation of the Raman frequency shift of a strained crystal (64). Since
then, piezo-Raman calculations have found broad application in silicon integrated circuits for measuring stress (89) as well as other
semiconductors such as Si1'xGex (90) and GaAs (91). Anastassakis also derived the peak shifts for polycrystalline silicon under
different stress states (92). The results of this work are similar to those of piezoluminescence insofar as only the hydrostatic stress is
measured and not the stress tensor in polycrystalline materials. The main advantage of piezo-Raman calculations over piezolu-
minescence is that almost all nonmetallic materials exhibit intrinsic Raman spectra without the need of doping.
In order to measure stress using Raman spectroscopy, one must first calibrate the Raman peak shift to stress. This can be done by
obtaining a bend bar of the material of interest, applying a flexural load, and collecting spectra along a line across the side of the bar
from compression to tension (93). One major weakness of piezo-Raman spectroscopy is that the peak shift with stress may change
significantly with minor changes in the composition or thermal history of the material being studied. For instance, Abel et al. found
that the peak shift with stress for the 521-cm'1 peak of polysilicon varied from '1.87 to '3.81 cm'1/GPa, depending on the
amount of boron or phosphorous dopant present in the sample (93). No clear trend in the peak shift with processing history stress
was observed. This means that, unlike piezoluminescence, one must not assume that the peak shift with stress remains the same
after processing of a material, and each new condition will require a new calibration. Due to this difficulty, the piezo-Raman method
lends itself more to measuring stress distributions in a homogeneous material rather measuring stress between samples that had
undergone different processing methods. Indeed, the piezo-Raman method has been successfully applied to measuring stress
distributions around crack-tips (59,94) where the calibration of peak shift to stress may be assumed to remain constant within the
mapped region.
Another weakness of the piezo-Raman method is that the Raman peaks will shift for reasons other than stress. For instance,
the amount and type of stabilizer in tetragonal zirconia will affect the Raman peak positions. Kim et al. measured the change in
the Raman spectra of tetragonal zirconia with the addition of tetravalent dopants (95). Dopants that had the largest difference in
atomic volume with zirconia caused the largest changes in the Raman spectra. This result is significant, since variation in the
stabilizer content in zirconia may result in peak shifts that are not due to stress, thereby limiting the use of the piezo-Raman
method. Similar effects may occur in other materials where local inhomogeneities produce Raman peak shifts independent of
residual stress.
In addition to microelectronics, the piezo-Raman method has been used in materials science to characterize stress in poly-
crystalline ceramics and glasses. DiGregorio and Furtak related the Raman peak shift of silicon carbide whiskers in alumina to
residual stress and related the results to micromechanical predictions (96). The piezo-Raman method has also been used to measure
stress on thermally grown oxide scales. In the case of alumina scales, the desired technique is clearly piezoluminescence, due to its
high intensity and large peak shift with stress. For other scales that do not exhibit luminescence, the piezo-Raman method must be
used. Birnie et al. measured stress distributions in chromium oxide scales by using Raman microscopy (97). Similar to oxide scales,
residual biaxial stresses in CVD-grown diamond have also been measured with the piezo-Raman method (98). Another large area of
use for the piezo-Raman method is in the field of fiber composites. Since Raman is a scattering spectroscopy, incident light can be
focused onto a fiber that is embedded in a translucent matrix. This allows for the direct measurement of stresses on fibers through
the matrix that can be related to interfacial shear strength of the fiber composite. Extensive work has been performed on carbon fiber
composites (99–101) and Nicalon fibers in a Pyrex matrix (102).
1.07.4.3 Emerging Techniques

As explained above, piezospectroscopy can be used to measure the mean hydrostatic stress in polycrystalline materials. However,
recent work has showed the potential for gaining information about the stress tensor in polycrystalline materials by using the
polarization effects on the intensities of the R-lines of alumina. He and Clarke (103) found that the area ratio of the R2 to R1 lines
changes with the angle between the incident laser polarization and the c-axis of the ruby crystal, and that this can be used to
determine the c-axis orientation of sapphire or of individual micron-sized grains in polycrystalline alumina. Resolving stress
components using both R-lines in a single crystal is therefore feasible. Moreover, a dependence on the ratio of the areas of the R-lines
on both the stress and the collection polarization optics was found (104), which can be used to extract up to two stress states from
a polycrystalline alumina scale. Raghavan and Imbrie recently measured the piezospectroscopic effect on the vibronic bands that are
present on the sides of the R-lines and showed that using these bands, along with the R-lines, may allow for the measurement of the
complete stress state in polycrystalline alumina (105).
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Similarly, Raman spectroscopy can be used to measure the complete stress state in single crystals, given the existence of enough
Raman peaks from the sample. Since the Raman effect is generated by a change in polarizability, which is a tensor property that
varies with the crystallographic orientation, the intensities of Raman peaks will be affected by the orientation of the incident electric
field of the laser light relative to the crystallographic orientation. This approach has been used to determine the crystallographic
orientation of an unknown grain in polycrystalline alumina. Zhu and Pezzotti extended this method to measuring the complete
stress state at a crack-tip in single-crystal sapphire (106). Since sapphire has six Raman active peaks, each of which shifts with stress
to different degrees depending on the crystallographic orientation, six independent measurements of the stress can be made from
the same spectrum, which allows one to solve for the complete stress state in the probed volume.
Recently, cathodoluminescence (or electron-stimulated luminescence spectroscopy) has been used to measure stresses by
tracking luminescent peak shifts in a scanning electron microscope (107). This approach has all the benefits of piezoluminescence,
but with spatial resolutions that are orders of magnitude higher than those present in electron microscopes. The technique is an
emerging approach for measuring stresses at the nanoscale.
1.07.4.4 Concluding Remarks about Piezospectroscopy

Piezospectroscopy can be used to measure stress in nonmetallic materials, with a spatial resolution of w1 mm far exceeding the
spatial resolutions associated with powder diffraction and strain gauge approaches. For polycrystalline materials, the mean
hydrostatic stress is measured. Under some circumstances, information about the stress tensor can also be obtained. Piezolumi-
nescence is almost exclusively performed on a-Al2O3 and takes less than 1 s to acquire data. The piezo-Raman method can be
applied to any material exhibiting Raman peaks but tends to be weaker, requiring longer data acquisition times.
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1.08 Testing of Small-Sized Specimens
E Lucon, National Institute for Standards and Technology, Boulder, CO, USA

1.08.2 Tensile Testing 136
1.08.3 Impact (Charpy) Testing 138
1.08.3.1 Reconstitution of Charpy V-Notch Specimens 138
1.08.3.1.1 Other Examples of the Use of Reconstitution 139
1.08.3.2 Miniaturized Charpy V-Notch Specimens 139
1.08.3.2.1 Estimation of Full-Size Upper Shelf Energy Based on Subsize Test Data 140
1.08.3.2.2 Estimation of Full-Size Transition Temperatures Based on Subsize Test Data 142
1.08.4 Fracture Toughness Testing 142
1.08.4.1 Lower Shelf (Brittle) Region 143
1.08.4.2 Ductile-to-Brittle Transition Regime 143
1.08.4.2.1 Precracked Subsize Charpy V-Notch Specimens 143
1.08.4.2.2 Subsize Cylindrical Bar Specimens 144
1.08.4.2.3 Additional Investigations and Modifications of the Master Curve Approach 145
1.08.4.3 Upper Shelf (Ductile) Region 146
1.08.4.3.1 Miniature Disk-Shaped Specimens 146
1.08.4.3.2 Miniature Compact Tension Specimens 146
1.08.5 Fatigue Testing 147
1.08.5.1 High-Cycle Fatigue Testing (S–N Curves) 148
1.08.5.2 Fatigue Crack Propagation Testing (da/dN Curves) 148
1.08.6 Creep Testing 149
1.08.7 Creep Crack Growth Testing 151
1.08.8 Extreme Miniaturization (Part 1): Small Disk Testing 151
1.08.8.1 Shear Punch Testing 151
1.08.8.2 Small Punch Testing 152
1.08.8.2.1 Derivation of Tensile and Fracture Properties 152
1.08.8.2.2 Derivation of Creep Properties 155
1.08.9 Extreme Miniaturization (Part 2): Use of Microfabrication Technology 158
1.08.10 Concluding Remarks and Future Trends 159
Acknowledgments 160
References 160
1.08.1 Introduction
It is essential to properly evaluate the mechanical properties of industrial components and structures because this evaluation is
vitally important in performing reliable assessments of material integrity and making correct predictions of residual life. This
evaluation is particularly useful when embrittlement and property degradation are suspected, due to exposure to high temperatures
(typically those greater than 280 * C), aggressive environments, or neutron irradiation (such as in the case of nuclear power plant
components). Under these circumstances, the actual mechanical behavior of the components or structures under investigation must
be reliably characterized without being overly conservative in estimates. Reference mechanical data, which are relevant to materials
in as-received or ‘virgin’ condition, are usually scarce and are often unavailable for older structures, which require more careful
assessment for continued operation. On the other hand, even if reliable information was available for the as-received materials, its
usefulness would be questionable, since actual service conditions and related damage mechanisms can deeply affect material
behavior. As a result, it is necessary to extract data from the component itself, so that both metallurgical conditions and actual
mechanical properties can be directly assessed. Economic and public safety implications are also important and must be considered
when performing this type of analysis.
The basic types of mechanical properties used for structural integrity assessments are tensile, fracture, and fatigue. The first two
properties are characterized by different physics-based size effects: microstructure (scaled by grain size) for tensile properties, and
three-dimensional stress fields, as well as their relaxation by geometry-controlled loss of constraint, for fracture properties.
The evaluation of the mechanical properties is normally a destructive technique, since it requires sampling material directly from
a component or structure. This can generally be done only when the sample size is so small that simple repairs, or even no repairs
(i.e., a virtually nondestructive sample technique), are eventually needed to allow further operation of the component, as in the case

www.iran- mavad.com
136 Testing of Small-Sized Specimens
of hardness measurements. This requires the use of very small specimens that usually do not comply with the requirements of
commonly used test standards, which are typically designated as ‘small-size’, ‘subsize’, or ‘miniaturized’.
An industrially and scientifically relevant example lies in the characterization of in-service nuclear reactor pressure vessels.
Surveillance capsules, which are used for periodically monitoring the degradation of vessel materials, offer limited space for storing
mechanical specimens and typically require a limited specimen size. Often, broken samples (usually Charpy specimens) are all that
remain from previous test campaigns, and material consumption must be optimized if additional mechanical property measure-
ments must be performed.
Several nonstandardized test techniques for subsize or miniaturized specimens are currently available that are aimed at assessing
the mechanical properties of service-exposed plant components and structures in a virtually nondestructive manner. This chapter
reviews several of these techniques, emphasizing important features such as:
l their advantages with respect to conventional test techniques (based on standard, full-size specimens),
l any characteristics of the necessary instrumentation,
l recommendations on the use of the results,
l the significance and reliability of the test results, and
l the techniques’ transferability to testing actual components and structures.
1.08.2 Tensile Testing
Several publications are available in the literature that address the determination of tensile properties through testing very small
specimens (1–6). In most cases, flat samples (sheet-type) are used, with dogbone geometry and the following nominal dimensions:
l gauge section length A between 3.1 and 9 mm;
l thickness T between 0.05 and 1 mm;
l gauge length width W between 0.5 and 2 mm.
Panayotou et al. (1) report the use of a ‘wire-type’ miniature round sample with reduced section diameter D ¼ 0.25 mm, which
experienced serious problems in both fabrication and testing. Sharpe and Fowler (4) reported obtaining stress–strain curves from
even smaller specimens, which had an overall length of 3 mm and a square cross section (0.2 " 0.2 mm). The smallest specimen
documented in the literature was described by Sharpe et al. (6). The results obtained from testing this specimen showed a coefficient
of variation (ratio of standard deviation to mean value) on the order of 5% for both yield and tensile strengths, while data for both
parameters were found to be approximately 5% lower than the results obtained from conventional tensile specimens.
The literature documents tests on both unirradiated (1,3–6) and irradiated (2) samples. Specific aspects emphasized by the
different authors were:
l the necessity of minimizing extraneous bending strains, which must be maintained in the elastic regime (1,5);
l the importance of the fabrication technique, which must be appropriate for the material being tested (2,4) and which can have
consequences for the measured tensile properties, particularly on the yield strength (3);
l high quality of the test instrumentation, including a precise, well-aligned test frame (1,5);
l good control and accuracy of the specimen dimensions, which directly relate to the reliability and reproducibility of the test data
(1,4,6).
When these manufacturing, handling, and procedural issues are effectively controlled, miniature tensile test data can be
expected to agree satisfactorily with tensile strengths measured from larger, more conventionally sized specimens (6,7), provided
that the dimensions of the samples are not below a minimum threshold, which depends on the material itself (8). The elongation
and reduction of area values have generally been reported as more dependent on specimen size and geometry than tensile
strengths (8–12).
In 2000, a group of U.S. and Japanese researchers published a detailed characterization of the size limitations of miniature
tensile specimens, as applied to several austenitic and ferritic/martensitic steels (13). It was shown that yield stress values inde-
pendent of specimen size could be obtained for specimen thicknesses in excess of 0.2 mm for the steels investigated. On the other
hand, geometry-independent tensile stress (UTS) values required a thickness-to-width, T/W, ratio in excess of approximately 0.2. In
most commercial steels, grain sizes are in the order of 20 mm or less, which correspond to at least 10 grains across a section with
T ¼ 0.2 mm ¼ 200 mm. This is generally considered to be more than adequate for practical purposes (14). Indeed, Igata et al. (8)
demonstrated that for 304 and 316 austenitic stainless steels, yield and tensile stresses were size independent for thickness-to-grain
size ratios greater than 6:1.
An example of an investigation on the reliability of miniature tensile specimen measurements is a project initiated at SCK$CEN
(the Belgian Nuclear Center) in 1999 (15,16). The tensile specimens investigated were small enough to be extracted from the fatigue
precracked region of a broken reconstituted Charpy-V specimen (Figure 1), and had the following nominal dimensions: length
L ¼ 10 mm, gauge section length A ¼ 5 mm, cross-section width W ¼ 1.5 mm, and cross-section thickness T ¼ 1 mm.
This miniaturized tensile test geometry was validated based on the comparison with benchmark tensile parameters obtained
from larger conventional samples for several pressure vessel steels; one example is given in Figure 2 for a nuclear-grade weld that is
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Testing of Small-Sized Specimens 137
Figure 1 Miniature tensile specimen extracted from a previously tested, reconstituted, and precracked Charpy sample. (HAZ indicates the heat-affected
zone.)
Figure 2 Tensile strengths measured on conventional and miniature samples for a reactor pressure vessel weld material. (UTS ¼ Ultimate Tensile
Strength.)
designated as 72 W. If suitable precautions are taken to minimize misalignment and extraneous displacements, even the scatter of
results is shown to be comparable to that of standard specimen data.
The following experimental aspects were recognized to be of paramount importance when extremely tiny specimens are tested
and can be considered to have general applicability.
1. Extreme caution must be exercised in order to avoid any extraneous deformation induced by gripping and mounting of the
specimen.
2. Because using an extensometer to measure the elongation of the specimen is impractical, the low force levels attained during
the tests (typically, less than 1 kN at general yield) cause the contribution of the load-train compliance (machine plus
gripping devices) to prevail over the actual specimen compliance for approximately 75% of the linear elastic range of the
test. Therefore, when the elastic slope used for calculation of the 0.2% offset plastic deformation is estimated, only the last
portion should be considered (approximately 25%) of the initial range that immediately precedes extensive plastic defor-
mation (yielding) of the specimen. Otherwise, serious underestimation of the yield strength may result. Noncontact
extensometry is an appealing alternative solution, based on optical methods such as Moiré interferometry (17) and digital
correlation (18).
3. As a general note, it is well known that the scatter of mechanical test results tends to increase as specimen dimensions are reduced
(i.e., the smaller the amount of the material sampled, the more pronounced the effect of microstructural inhomogeneities on the
test results). Thus, in the case of miniature tensile tests, the minimum recommended number of specimens per temperature is
three (and preferably five).
At the time of writing, the most popular approaches for characterizing the constitutive stress/strain behavior of irradiated
materials were based on various kinds of punch tests, as well as microhardness and instrumented hardness tests (along with the
aforementioned miniature tensile tests). Punch tests will be subsequently described, whereas hardness-based methods are outside
the scope of this chapter, as specimen geometry does not factor into these tests.
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Finally, the utility of analyzing the deformation behavior of a tensile specimen by finite element analysis (FEA) was demon-
strated by Odette et al. (19,20). Self–consistent, true stress–true strain constitutive equations were derived by comparing experi-
mental engineering stress–strain behavior to the corresponding finite element simulations. This shows that, in order to be more
effective and reliable, small-specimen tensile testing must be closely integrated to finite element (FE) simulations, as well as
fundamental models of deformation and fracture (21).
1.08.3 Impact (Charpy) Testing
Whenever original mechanical property certifications are available for components from a plant that has been in service for many
years, impact test data (such as ductile-to-brittle transition temperature and absorbed energy at room temperature) are normally
reported, along with the tensile properties of the as-received material. Any possible scenario involving fracture, particularly in the
case of unstable crack propagation, must be avoided. In most cases, current regulations use impact properties as key data to indicate
the fracture resistance of structures and components. The ultimate goal of impact testing is to qualitatively assess fracture resistance;
in contrast, for a quantitative assessment, one must turn to actual fracture toughness testing.
The comparison between data from manufacturing certification and the post-service impact properties of the materials under
investigation can indicate whether embrittlement and toughness degradation of the component have occurred during service.
However, in most cases, the available material for impact testing is insufficient for machining conventional Charpy-V specimens
(notched bars with a 10 " 10 mm2 cross section and a 55 mm length); often, only previously broken Charpy specimens are
available for machining new specimens.
Two options are viable for this type of testing:
1. the reconstitution of additional Charpy specimens by joining a central portion of the material under investigation (the length
of the insert typically ranges between 10 and 20 mm) to two end tabs from a common mild steel; or
2. the use of miniaturized Charpy V-notch (MCVN) specimens that have various ‘nonstandardized’ geometries.
These two options will be addressed separately in the following sections.
1.08.3.1 Reconstitution of Charpy V-Notch Specimens

The shortage of vintage material representative of the pressure vessel of older nuclear power plants, and the interest or need to revisit
some destructively tested pressure vessel surveillance material, have justified the development of reconstitution techniques over the
last 30 years. The most popular reconstitution technique that can be used in a hot-cell environment and allows broken Charpy-V
specimens to be reconstructed under well-defined technical conditions (22) is called ‘arc-stud welding’. This technique consists of
fixing additional material around a material of interest (the insert) in order to obtain, after some machining, a test specimen of
standard dimensions. The simplest example is the classical 10 " 10 " 55 mm Charpy V-notch specimen, reconstituted from
a previously tested half-Charpy by adding two end pieces (Figure 3). The stud-gun welding setup is a moderately priced welding
tool that allows reliable and good-quality cross-sectional welds to be obtained.
The potential of the reconstitution technique can be thoroughly exploited only if it is possible to guarantee that the material of
interest was not altered by the reconstitution process, which can be accomplished by limiting the temperature within the test
volume to values low enough not to induce annealing effects or metallurgical changes. Moreover, test results from reconstituted
Figure 3 Schematic diagram of the reconstitution technique.
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specimens should ideally be identical to those obtained on nonreconstituted (standard) samples, or else deviations should be
understood and accounted for.
Based on the comparison between impact test results obtained from standard and reconstituted samples, the following
conclusions were documented in (22).
l The agreement between standard and reconstituted specimens was excellent in terms of ductile-to-brittle transition tempera-
tures, independent of insert size.
l For insert lengths between 10 and 12 mm, a significant loss of upper shelf energy (USE) was observed. (In Charpy testing, the
upper shelf energy is defined as the asymptotic value of absorbed energy that is recorded in the temperature range where all
specimens exhibit a fully ductile behavior.) Such a loss can be classified into two or three categories, based on the combination of
the welding technique and the geometry of the impact pendulum striking edge (23).
l Large variations could be observed in welding parameters, even between institutions that use the same welding technique.
More advanced welding techniques for reconstituting impact specimens are used in different laboratories (24–26), including
laser welding, which can be expensive but guarantees extremely small heat-affected zones once the optimal reconstitution
parameters have been established.
1.08.3.1.1 Other Examples of the Use of Reconstitution

During the 1980s, the reconstitution technique was used by the Central Electricity Generating Board (CEGB) in the United Kingdom
for obtaining uniaxially loaded creep specimens as part of an EPRI (Electric Power Research Institute, Palo Alto, California)-
sponsored research program (27,28). Material from operating power plants taken from boat-shaped samples (29,30) was machined
in the form of blanks with a 3 mm diameter and 15 mm length. The blanks were friction- or electron-beam welded to end pieces and
then machined down to the final specimen size (2 mm diameter, 10 mm gauge length, and 6 mm diameter shank size).
For direct measurements of fracture toughness, compact tension (C(T)) specimens were obtained (25,31) by inserting a block of
the material to be evaluated directly into the crack propagation path within an existing C(T) sample. The insert material was taken
from previously tested Charpy specimens, as shown in Figure 4(a) (31), or from 0.5 in. (12.5 mm) thick C(T) specimens, as shown
in Figure 4(b) (25).
During the reconstitution procedure, it is important to ensure that the temperatures reached within the test sections do not exceed
certain threshold values that can influence the properties of the insert material. Specifically, the welding parameters are controlled in
order to minimize the dimensions of the heat-affected zone and its influence on fracture toughness and crack growth properties.
1.08.3.2 Miniaturized Charpy V-Notch Specimens

The possibility of using subsize specimens to monitor the properties of primary power plant components is receiving increasing
attention in plant life extension studies. In the case of pressure vessels of nuclear light-water reactors (LWRs), the extension of the
Figure 4 (a) C(T) specimen reconstituted from broken halves of Charpy samples, reprinted from McConnell, P.; Sheckherd, J. W.; Perrin, J. S.; Wullaert,
R. A. Experience in Sub-Sized Specimen Testing. ASTM STP 888W. In The Use of Small Scale Specimens for Testing Irradiated Specimens ; Corwin, W. R.,
Lucas, G. E., Eds.; ASTM: Philadelphia, PA, 1986; pp 353–368. (b) C(T) specimen reconstituted from previously tested C(T) sample, reprinted from
Tomimatsu, M.; Kawaguchi, S.; Iida, M. Reconstitution of Fracture Toughness Specimen for Surveillance Test. ASTM STP 1329. In Small Specimen Test
Techniques; Corwin, W. R., Rosinski, S. T., van Walle, E., Eds.; ASTM: Philadelphia, PA, 1998; pp 470–483.
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surveillance program entails either machining subsize specimens from previously tested Charpy surveillance specimens or recon-
stituting additional samples from the broken pieces. The main issues concerning the use of subsize Charpy specimens are related to
correlating transition temperatures and USE values between subsize and full-size (standard) specimens. An extensive review of such
correlations was compiled by Sokolov and Alexander at Oak Ridge National Laboratory (32).
Different subsize Charpy specimens have been tested around the world, the smallest being miniature samples with 1.5 " 1.5 mm
(33) and 1 " 1 mm (34) cross sections, both used in Japan. However, only two subsize Charpy specimen types are officially
standardized at present:
1. the Kleinstprobe (KLST), originally from the German DIN 50 115 Standard (35), whose nominal dimensions are length
L ¼ 27 mm, width W ¼ 4 mm, thickness B ¼ 3 mm, notch depth N ¼ 1 mm, notch angle a ¼ 60* , and notch root radius
r ¼ 0.1 mm; and
2. the reduced half-size (RHS) specimen, which is scaled down with respect to a full-size Charpy specimen by a scaling factor of
0.483 (i.e., cross section 4.83 " 4.83 mm, length L ¼ 26.565 mm).
Both geometries are included in the ASTM E2248 standard (36). Amendment 1 of the ISO 14556 standard (37) addresses only
the KLST specimen, although other configurations (including RHS) are also mentioned.
The next two subsections are based on research undertaken in 1998 (38,39), consisting of the analysis of 565 instrumented
impact tests (232 performed on full-size and 333 on KLST subsize Charpy-V specimens). Nine materials (all nuclear pressure vessel
steels) were considered, both unirradiated and irradiated, for a total of 19 different conditions examined.
1.08.3.2.1 Estimation of Full-Size Upper Shelf Energy Based on Subsize Test Data
The published correlations (32,38–44), which allow predicting full-size USE values based on values of subsize specimen USE, can be
classified into two categories.
The first method, which is commonly used in Europe, consists of establishing an empirical ratio between the full-size USE
(USEfs) and the subsize USE (USEss), based on a large number of tests. The second approach, which is quite popular in North
America and Japan, attempts to correlate USE values with the ratio of various geometrical parameters GPx for different specimen
geometries in the form of:
USEfs GPfs
¼ : [1]
USEss GPss
Equation [1] can also be expressed in terms of a normalization factor, NF, which is precisely the ratio of the geometrical
parameters mentioned above:
USEfs ¼ NF " USEss : [2]
The most common expressions for NF that can be found in the literature are the following:
ðBbÞfs
NF1 ¼ ; [3]
ðBbÞss
based on the ratio of fracture areas, with B ¼ specimen thickness and b ¼ specimen ligament size (40,41),
½ðBbÞ3=2 (fs
NF2 ¼ ; [4]
½ðBbÞ3=2 (ss
based on the ratio of nominal fracture volumes (40,41),

ðBb2 Þfs
NF3 ¼ ; [5]
ðBb2 Þss
based on a different expression for the ratio of nominal fracture volumes (42,43), and
" 2#
Bb
LKt
NF4 ¼ " 2 #fs ; [6]
Bb
LKt ss
where L ¼ span and Kt ¼ elastic stress concentration factor (44).

When considering the ratio of geometrical parameters between full-size and KLST specimens, the following numerical values are
obtained from eqns [3]–[6]: NF1 ¼ 8.9, NF2 ¼ 23.7, NF3 ¼ 26.5, and NF4 ¼ 13. In addition, Sokolov and Alexander (32) established
the empirical value of NF5 ¼ 21.3 by averaging values of the ratio USEfs/USEss that was obtained on 10 different materials (mostly
pressure vessel steels with different heat treatments). When considering the nine steels analyzed in (38,39), the average value of the
normalization factors obtained is NF6 ¼ 21.56, with standard deviation s ¼ 2.64.
On the other hand, Figure 5 shows a clear relationship between subsize and full-size USE values for the conditions examined in
(38,39), which can be effectively represented by an exponential fitting function.
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Figure 5 Exponential relationship between subsize and full-size USE values for KLST specimens. Reprinted from Lucon, E.; Chaouadi, R.; Fabry, A.;
Puzzolante, J. -L.; van Walle, E. Correlations between Standard and Miniaturised Charpy-V Specimens. SCK CEN Report BLG-797, 1998 (unclassified).
l
Figure 6 Comparison between predicted and measured full-size USE values. Reprinted from Lucon, E.; Chaouadi, R.; Fabry, A.; Puzzolante, J. -L.;
van Walle, E. Correlations between Standard and Miniaturised Charpy-V Specimens. SCK CEN Report BLG-797, 1998 (unclassified).
l
Predicted values of USEfs obtained by applying the six different normalization factors and the exponential fitting function of
Figure 5 above are compared to experimentally measured values (USEfs,exp) in Figure 6, with respect to an ideal 1:1 prediction line
(predicted USEfs ¼ measured USEfs) and ) 20% tolerance bounds.
Figure 6 shows that:
l the approaches based on the normalization factors NF1, NF3, and NF4 yielded unsatisfactory predictions for the materials
considered;
l normalization factors NF2, NF5, and NF6 provide reasonably small average (absolute) deviations from the measured values, in
the range of 10–15%, with the smallest value corresponding to NF6;
l the largest absolute deviation for any normalization factor is always greater than 30%. In other words, regardless of the approach
chosen, the presence of ‘outlier’ materials appears unavoidable.
Based on the calculations performed, the approach of using a simple normalization factor to predict USEfs is not recommended,
due to the risk of significantly under- or overpredicting the measured values. Use of a simple fitting function, such as the one
depicted in Figure 5, appears to be preferable.
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Figure 7 Comparison between index temperatures measured on full-size and subsize KLST specimens, with fitting lines. Reprinted from Lucon, E.;
Chaouadi, R.; Fabry, A.; Puzzolante, J. -L.; van Walle, E. Correlations between Standard and Miniaturised Charpy-V Specimens. SCK$CEN Report BLG-797,
1998 (unclassified).
1.08.3.2.2 Estimation of Full-Size Transition Temperatures Based on Subsize Test Data

Various definitions of index temperatures (or ductile-to-brittle transition temperatures, DBTT) have been introduced for conven-
tional Charpy-V impact tests on nuclear materials, which would be used in regulatory codes or material specifications. Each defi-
nition relates to a predefined level of absorbed energy (41 J or 68 J), lateral expansion (0.89 mm), or shear fracture appearance
(FATT50 ¼ fracture appearance transition temperature, corresponding to 50% shear fracture appearance).
For the KLST subsize specimen, the criteria based on the energy and lateral expansion levels mentioned above were redefined
(normalized) as 41 / 1.9 J, 68 / 3.1 J, and 0.89 / 0.3 mm, based on the mean ratio of upper shelf values (45,46). The
conventional level of shear fracture appearance (50%), being a relative measurement, needs no such redefinition. The mean
difference in terms of index temperatures between subsize and full-size specimens was established on the basis of numerous
correlation tests (45,46) as
Tfs ¼ Tss þ 65 * C; [7]
where Tfs ¼ T41J, T68J, T0.89mm, FATT50(fs) and Tss ¼ T1.9J, T3.1J, T0.3mm, FATT50(ss). The standard deviation was reported as 15 * C,
yielding a 95% confidence interval () 2s) of ) 30 * C. Figure 7 shows the calculated values of index temperatures for full-size
samples with respect to the corresponding equivalent index temperatures for KLST specimens for the materials investigated in
(38,39). The mean correlation line calculated from the analyzed data after imposing unity for the slope is
Tfs ¼ Tss þ 59:6 * C; [8]
with a 95% confidence interval of 43.4 * C
(and a standard deviation s ¼ 21.7 * C).
If the data are fitted into a conventional straight line (i.e., without imposing unity for the slope), the result is
Tfs ¼ 1:17Tss þ 57:8 * C; [9]
which yields a lower value for the mean quadratic residual (360.1) than eqn [8] (462.1).
Although the average shift from eqn [8] (59.6 * C) was reasonably close to the value reported in the literature (65 * C), the energy-
related index temperatures (T41J and T68J) showed significant scatter. On the other hand, the standard deviation obtained for
DT0.89/0.3mm and DFATT50 was reasonably consistent with the values reported in the literature (15 * C). As a result, the use of index
temperatures related to energy levels is not recommended for correlation purposes. Moreover, it should be noted that for some
irradiated materials, some of the predefined energy/lateral expansion levels cannot even be reached, due to severe degradation in
material toughness.
1.08.4 Fracture Toughness Testing
In recent years, direct measurement of fracture toughness for assessing the integrity of potentially embrittled components and
structures has been widely recognized as a more physically based alternative to the indirect evaluation of toughness through the use
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of Charpy-based data. In the nuclear field, the traditional approach of measuring the increase in transition temperature at the 41 J
absorbed energy level from conventional impact tests is often overruled by more advanced approaches, such as the analysis of the
instrumented Charpy diagram (47) or the assessment of the 100 MPa m1/2 reference temperature shift with use of the master curve
approach, according to the ASTM E1921 standard (48).
1.08.4.1 Lower Shelf (Brittle) Region

The requirements on specimen size are particularly severe in the field of linear elastic fracture mechanics, when the behavior of the
material under investigation is totally or prevalently brittle. Minimum specimen dimensions (at least for ‘conventional’ specimen
geometries, such as compact or bend samples) are required to ensure a sufficient degree of crack-tip triaxiality (constraint), but are
generally impractical for residual life evaluations of service-exposed plant components.
A novel specimen configuration was proposed that could guarantee a sufficiently high level of constraint and stress triaxiality at
the crack tip while using a limited amount of sample material: the cylindrical bar CB(T) specimen, precracked by rotary fatigue and
tested in tension (49–51). This geometry, shown schematically in Figure 8, offers the following advantages with respect to
conventional compact or bend specimens:
l machining is simpler, quicker, and therefore cheaper;
l precracking and testing are considerably simpler and do not require the same amount of complexity and sophistication in terms
of test equipment;
l the specific crack configuration (circumferential and axisymmetric) at the tip of the machined notch provides a sufficient degree
of stress triaxiality, particularly at elevated stress levels (50);
l therefore, a limited amount of material is sufficient to obtain reliable estimates of fracture toughness in prevalently brittle
conditions.
The fatigue precracking of a cylindrical bar specimen is achieved by rotary fatigue, monitoring the crack depth in terms of either
specimen deflection (49) or decrease of applied force (50), or by preliminarily estimating the number of fatigue cycles to failure for
a predetermined bending moment (51). A sufficiently deep and concentric fatigue crack can be obtained in 30–60 min, by the use of
a rotational speed between 4000 and 5000 rpm.
The actual fracture toughness test is similar to a conventional tensile test in which the value of applied force at fracture is used (in
the case of linear elastic behavior) to estimate the critical value of the stress intensity factor Kc by the use of standard equations
available in fracture mechanics handbooks (52–54). The use of an extensometer can be helpful to verify the linearity of the force/
displacement record until fracture, but it is not strictly needed if the material is expected to exhibit fully linear elastic behavior under
the test conditions.
1.08.4.2 Ductile-to-Brittle Transition Regime

The reliability of fracture toughness measurements in the ductile-to-brittle transition regime by use of miniature samples was
assessed in a study conducted at SCK$CEN in 2001 (55). Results were analyzed according to the previously mentioned master curve
procedure. Two geometries were investigated: (1) the precracked subsize Charpy V-notch specimen and (2) the subsize cylindrical
bar CB(T) with diameter D ¼ 4 mm.
1.08.4.2.1 Precracked Subsize Charpy V-Notch Specimens

The subsize Charpy specimen geometry used in (55) was the same as that previously indicated for impact testing (i.e., the KLST
specimen). Fatigue precracking was achieved on a resonant testing machine, decreasing the applied moment in several
computer-controlled steps in order to fulfill the requirements of the test standard. Crack extension could be accurately
controlled up to a nominal crack-size-to-width ratio a/W z 0.5. During fatigue precracking, the maximum value of the applied
stress intensity factor Kmax was always kept below 17 MPa m1/2, and for the last 0.6 mm of precracking, Kmax did not exceed
13 MPa m1/2.
Fracture toughness tests were performed in three-point bend loading on a universal testing machine equipped with a 1 kN load
cell. Tests were performed in machine crosshead displacement control with a speed of 0.2 mm min'1. Every specimen was
instrumented with a clip-on gauge for measuring crack mouth opening displacement (CMOD). Force and CMOD values were used
Figure 8 Cylindrical bar specimen (aka cracked round bar).
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Figure 9 Toughness data analyzed with the master curve (MC) approach for a German pressure vessel steel.
for the evaluation of fracture toughness through standard formulas for the bend test geometry provided in the ASTM E1921
standard. This specimen geometry was validated by direct comparison with similar data obtained for two reactor pressure vessel
steels by use of larger specimens (full-size precracked Charpy-V specimens and standard C(T) samples). Values of the reference
temperature T0 were calculated by use of ASTM E1921 for the different specimen sizes and/or geometries were found to be in
agreement within ) 10 * C. It is worth noting that the typical uncertainty associated with T0 measurements is also on the order of
) 10 * C (56). A direct comparison between toughness data (normalized to the 25.4 mm ¼ 1 in. thick C(T) reference geometry)
obtained from subsize and larger specimens is shown in Figure 9. The results obtained in this study confirm similar findings
documented in the literature for other pressure vessel steels (57,58).
On the other hand, an important issue emerging from the research performed was that the limited size of such miniature
samples exposed them to the risk of significant loss of constraint, which forced tests to be carried out at temperatures well below T0
in order to obtain a sufficient amount of valid data. From this point of view, it was shown (59) that the most efficient sample size for
subsize Charpy-V specimens, in terms of material consumption and number of tests required for a valid T0 determination, is the 1:2
scaled Charpy (cross section 5 " 5 mm, length 27.5 mm).
1.08.4.2.2 Subsize Cylindrical Bar Specimens

CB(T) samples (Figure 8) with a 4 mm diameter and a 24 mm length were used in (55) to validate toughness measurements in the
transition region and were analyzed with the master curve approach (60). For these tests, specimen elongation was measured by
means of two extensometers mounted in opposition with a gauge length of 12.5 mm. This allowed the evaluation of possible
bending components due to specimen misalignment or fatigue precrack eccentricity. In order for the test to be valid, a limit was set
for the maximum difference between the measurements yielded by the two extensometers (30% of the elongation at rupture).
Furthermore, a 15% limit was placed on the maximum allowable difference between the theoretical and the experimental
compliance of the specimen.
The fracture toughness value of the individual specimen was evaluated by the use of formulas appropriate to the specific
geometry, which have been validated through comparison with finite element analyses (61). Furthermore, in the master curve
analysis, a revised procedure (61) was proposed that introduces the following modifications with respect to the ASTM 1921
standard (which does not include this type of specimen):
l a modified limit for the maximum stress intensity factor measurable from a specimen of given size;
l a correction for the loss of constraint resulting from the stress relaxation ahead of the crack tip, leading to a small-scale yielding
(SSY) condition where the size of the plastic zone is negligible, with respect to the specimen dimensions.
Fracture toughness data and reference temperatures obtained from small cylindrical specimens compared favorably with results
yielded by larger samples, with reference temperature values in agreement within ) 10 * C (55). An example is shown in Figure 10
(for the same German pressure vessel steel shown in Figure 9).
Regarding the issue of testing at low temperatures in order to avoid an excessive loss of constraint and subsequent data
invalidation, the miniature cylindrical specimen has a significant advantage over the subsize precracked Charpy sample: the
previously mentioned correction for the loss of constraint allows reducing the downward shift in test temperature with respect to T0
and therefore the risk of approaching lower shelf conditions.
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Figure 10 Toughness data analyzed using the master curve approach, obtained for a German pressure vessel steel using specimens of different size and
geometry (CRB ¼ cracked round bars – alternative denomination of CB(T) specimens).
1.08.4.2.3 Additional Investigations and Modifications of the Master Curve Approach

For the use of small specimens in measuring fracture toughness in the transition regime, Odette and coworkers developed the master
curve-shift (MC-DT) method (62,63) as an engineering expedient to treat the effects of structural geometry, irradiation, loading
rates, and safety margins.
According to this method, a relatively small number of small specimens can be used to index a baseline cleavage fracture
toughness curve, Kc, as a function of test temperature. This curve typically deviates from SSY conditions, and the data can be adjusted
to conditions of higher constraint, that is, specimens of larger dimensions, by an amount DTg (see Figure 11). Additional
temperature shifts can be imposed to account for strain rate, irradiation effects, statistical weakest link-type size effects (64), and
a margin of safety. Microstructurally based models have been developed to predict these shifts, as well as both the shape and the
position of the reference curve (65,66).
An alternative approach uses mechanistic models through the analysis of the fracture surfaces with confocal microscope tech-
niques and the determination of CTOD values at specimen failure (21,63). Additional small tensile specimens can be tested to
derive the constitutive laws for the material, which can be used in numerical simulations of the deformation ahead of the crack tip,
and ultimately to estimate the material’s toughness.
Figure 11 Schematic illustration of the MC-DT method. The heavily dashed curve represents the basic master curve shape. Reproduced from Lucas, G.
E.; Odette, G. R.; Sokolov, M. A.; Spaetig, P.; Yamamoto, T.; Jung, P. Recent Progress in Small Specimen Test Technology. J. Nucl. Mater. 2002, 307–311,
1600–1608.
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Research efforts from the same group at the University of California at Santa Barbara have led to an even more aggressive approach
to reducing fracture specimen sizes by developing a small precracked bend bar that is nominally one-sixth of a full-size Charpy
specimen, that is, 1.65 " 1.65 " 9.2 mm (67,68). This specimen was labeled ‘deformation and fracture minibeam’ (DFMB), and was
tested in both notched and unnotched forms. The measured shape of the Kc(T) curve for the DFMB specimen deviated from the
conventional master curve shape, and a relatively steeper transition behavior was observed (21). As part of a U.S.–Japanese collab-
oration (68), even smaller DFMBs (with 1 " 1 mm cross sections) were used for irradiation in high-energy spallation proton beams.
1.08.4.3 Upper Shelf (Ductile) Region

1.08.4.3.1 Miniature Disk-Shaped Specimens
An example of a material sample extracted from a service-exposed plant component is a trepan, a long cylindrical sample with
diameter , 20 mm and length , 120 mm. By considering the shape of a trepan, a novel specimen geometry was developed for
fracture toughness testing in the elastic–plastic (upper shelf) regime, which can be easily extracted by ‘slicing’ trepans: the minia-
turized disk-shaped compact specimen, MDC(T). Its nominal dimensions are thickness B from 5 to 8 mm and diameter D from 16
to 20 mm (Figure 12).
Because the use of a clip-gauge for monitoring load-line displacement (LLD, which is needed for calculating J-integral values) is
impractical on such a tiny specimen, an alternative ‘indirect’ methodology was developed for inferring the LLD from machine actuator
displacement. The technique is based on removing the extraneous displacements from the actuator displacement, due to compliance
of the test setup and elastic deformations of the grips and the specimen. These components are quantified by testing an unnotched
specimen and obtaining the compliance curve of the test setup as a function of the applied force by least-squares regression.
MDC(T) specimens should not be used when the material under investigation exhibits significantly linear elastic behavior,
because the specimen dimensions do not fulfill the size requirements imposed by the standards. As a result, overestimations of the
actual fracture toughness of the component would be obtained (unless the component thickness is close to the specimen thickness).
On the other hand, in the upper shelf regime, MDC(T) specimens seem to provide sufficient J-capacity to reliably estimate the
critical toughness of some ferritic steels, as depicted in Figure 13, where results from D ¼ 16 mm MDC(T) specimens are compared
with data from 1TCT (B ¼ 25.4 mm) specimens for a 1CrMoV rotor steel (16).
The data shown in Figure 13 were obtained by using the multispecimen technique. J–R curves can also be derived with the
single-specimen potential drop (PD) technique, in which crack propagation is analytically correlated with the increase of potential
difference measured across the machined notch on a specimen through which electric current is flowing (69,70).
1.08.4.3.2 Miniature Compact Tension Specimens

Miniature compact specimens, MC(T), with thickness B ¼ 4.15 mm were qualified in (71,72) for measuring the fracture toughness
of steels under fully ductile conditions (upper shelf regime). Results obtained from MC(T) specimens of five ferritic steels, in terms
of critical toughness values and crack resistance curves, were compared with measurements performed on standard C(T) specimens
with B ¼ 25 mm thickness.
The first investigation (71) concluded that the MC(T) specimens systematically underestimated the fracture toughness measured
by the conventional 1TC(T) sample. Figure 14 shows an example for a nuclear pressure-vessel steel tested at room temperature.
Additional investigations (72) confirmed that work-hardening tends to lower the tearing resistance of very small specimens. This
was clearly indicated by test results obtained from 0.5TC(T) specimens (B ¼ 12.7 mm) extracted from prestressed 1TC(T) samples
and from 1TC(T) specimens with very deep fatigue precracks. In both cases, crack resistance curves from work-hardened specimens
closely matched MC(T) data in the early stages of crack extensions. It was also seen that the use of alternative fracture toughness
parameters, such as the crack-tip opening displacement (CTOD) or the crack-tip opening angle (CTOA) (73), significantly improved
the agreement between the 1TC(T) and MC(T) test results.
Figure 12 The miniature disk-shaped compact MDC(T) specimen.
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Figure 13 J–R curves obtained in the upper shelf region for a rotor steel by use of miniature DC(T) and 1TCT specimens. Reprinted from Lucon, E.
Material Damage Evaluation of Primary Power Plant Components Using Sub-Size Specimens. Adv. Eng. Mater. 2001, 3 (5), 291–302.
Figure 14 Comparison between 1TC(T) and MC(T) measurements of fracture toughness for a reactor pressure vessel steel. Reprinted from Lucon, E.;
Scibetta, M.; Chaouadi, R.; van Walle, E. Use of Miniaturized Compact Tension Specimens for Fracture Toughness Measurements in the Upper
Shelf Regime. J. ASTM Int. 2006, 3, 1.
Figure 15 shows test results (71,72) indicating that an empirical correlation was established between critical J-integral values at
crack initiation, as measured from miniature and conventional compact specimens. The correlation allows the derivation of
acceptable estimates of a material’s critical toughness with an accuracy of ) 34% at a 95% confidence level:
2:0586
J1TCðTÞ ¼ JMCðTÞ þ 0:0013$JMCðTÞ ; [10]
where J1TC(T) and JMC(T) are critical toughness values obtained from 1TC(T) and MC(T) specimens, respectively.
The results obtained also demonstrated that the current limits for the specimen-measuring capacity in the ASTM E1820 test standard
were far too restrictive, and that such restrictions could be significantly relaxed. Along with similar published research (74), this
contributed to the revision of such limits, which were effectively doubled when E1820 was revised from the 2006 to the 2008 version.
1.08.5 Fatigue Testing
There have been comparatively limited research efforts on fatigue testing relative to other types of mechanical tests, due to various
factors, including a higher complexity of test requirements, the potential need to impose push–pull (tension–compression) loading
as well as tension–tension loading, higher costs, and a more difficult interpretation of the data (75).
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Figure 15 Correlation obtained between MC(T) and 1TC(T) test results with ) 2s confidence bounds. The different symbols indicate critical values
calculated by use of different single-specimen (unloading compliance, normalization) or multiple-specimen techniques.
Nevertheless, the results available in the literature suggest that the effects of specimen size in fatigue testing are generally limited
within ranges of practical interest.
1.08.5.1 High-Cycle Fatigue Testing (S–N Curves)

Efforts to miniaturize the size of high-cycle fatigue specimens have been pursued, particularly in Germany and Japan.
In Germany, Möslang and coworkers (76) developed an optimized miniature fatigue specimen for the characterization of fusion-
relevant structural materials, based on detailed finite element simulations. The specimen had a cylindrical gauge section with 2 mm
diameter and 7.6 mm length. The results documented for this specimen indicated an excellent agreement in terms of the S–N curve
(stress amplitude versus number of cycles to failure, also known as the Wöhler curve) between these small samples and much larger
conventional specimens.
In Japan, Hirose et al. (77) developed a similarly sized hourglass-shaped specimen for fatigue testing that also showed satis-
factory results and little, if any, effect of specimen size on the results.
It is worth mentioning that for high-cycle fatigue testing, the hourglass geometry allows the achievement of higher strain ranges
in tension/compression tests and a greater ease of temperature control (21). On the other hand, the strain ranges of technological
interest are also achievable by use of a cylindrical specimen. In addition, cylindrical specimens allow the testing of a greater volume
and surface area, and the results can be applied in design in a more straightforward fashion.
1.08.5.2 Fatigue Crack Propagation Testing (da/dN Curves)

Similar efforts have been documented for reducing the size of specimens to be tested when generating fatigue crack propagation
data (da/dN curves).
The earliest investigation (78) proposed the use of modified Charpy specimens with the same width, but twice the depth of
a standard Charpy specimen. This specimen, however, should not be classified as having a truly subsize geometry. Li and Stubbins
(79) developed a miniature bend bar with nominal dimensions of 7.9 " 2 " 0.8 mm. Tests performed at room temperature on an
austenitic 304 stainless steel, a high nickel Inconel 718 alloy, and a modified 9Cr–1Mo steel showed that crack growth rates da/dN
that are measured as a function of applied stress intensity factor range DK tend to agree well with trend curves obtained on the same
materials from large standard C(T) specimens.
In 2006, Shin and Cai (80) published crack-propagation data obtained from small cylindrical specimens with lengths ranging
from 26 to 200 mm and with diameters ranging from 8 to 15 mm. It was observed that specimens longer than 42 mm provided
acceptable results, regardless of their diameters, in terms of both surface and interior growth data. If only interior growth was
considered, valid results were obtained with specimens as small as 8 mm diameter and 26 mm length. Such dimensions allow
fatigue samples to be machined out of the remnants of previously tested Charpy specimens.
Recently, the satisfactory agreement between subsize and conventional specimen fatigue crack growth data has been questioned
by Shin and Lin (81), who claimed that under closer examination, miniature specimen crack propagation rates actually differ by
factors of 2–4 from standard specimen data (Figure 16). They attributed this difference to varying constraint conditions between
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Figure 16 Comparison of FCP rates between miniature and large specimens for an aluminum alloy (7075-T651) and 304 stainless steel. Reprinted
from Shin, C. S.; Lin, S. W. A Critique on Evaluating Fatigue Crack Propagation Properties Using Miniature Specimens. Adv. Mater. Res. 2011, 146–147, pp
646–649.
Figure 17 Comparison of FCP rates between subsize and standard specimens in terms of the effective stress intensity factor range, which accounts
for crack closure effects. Reprinted from Shin, C. S.; Lin, S. W. A Critique on Evaluating Fatigue Crack Propagation Properties Using Miniature Specimens.
Adv. Mater. Res. 2011, 146–147, pp 646–649.
large specimens (which remain in a plane strain state throughout the test) and subsize specimens (which also start in plane strain
but quickly transition to a predominantly plane stress state, as the crack propagates). Due to the weaker plastic constraint associated
with the plane stress state, a higher degree of premature crack closure was observed.
By plotting da/dN values as a function of the closure-corrected effective stress intensity factor range DKeff, which accounts for the
effects of premature crack closure, the miniature specimen data could largely be brought in line with the standard specimen data, as
Figure 17 shows. The relation between da/dN and DKeff that is established on subsize samples can be used as a conservative estimate
of structural fatigue life.
1.08.6 Creep Testing
In order to predict the creep behavior of components and structures that operate at high temperatures (typically > 0.4 Tm, where Tm
is the melting temperature of the material), ‘bulk’ material creep properties are required and can be obtained by using specimens
with cross sections sufficiently large in comparison with the material’s metallurgical features. Furthermore, a relatively large gauge
length (25–50 mm) allows for a high degree of accuracy in strain measurements.
When a limited amount of material is available for creep measurements, the most popular approach is to reconstitute
conventional specimens by using accurately controlled welding methods (82). Newer material extraction methods have been
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proposed that use material slivers to produce smaller specimen designs, such as limited reconstituted specimens or disk testing (83).
An interesting example was documented as part of the EPRI/CEGB remaining life project (27,28) in the form of small uniaxial creep
specimens with 1.5–3 mm diameter gauge lengths that are electron-beam (EB) welded to conventional end pieces. The small
specimens compared favorably with larger specimens (28), as long as oxidation was avoided. In general, it is essential that
controlled atmospheres be used for both fabrication and testing to avoid significantly reducing creep life due to surface oxidation of
the smaller-diameter specimens (84).
In general, it has been proposed (85) that specimen diameters as small as 1 mm can be used to produce ‘bulk’ material creep
properties, provided that the cross section is large in comparison with the material’s grain size. On the downside, a gauge length
shorter than 10 mm can significantly reduce the accuracy of strain measurements and make them sensitive to relatively small
temperature fluctuations. The effects of specimen misalignment are also more pronounced.
A completely different approach from the conventional test is represented by indentation or impression creep, which involves
the application of a constant force by means of a punch or die onto the specimen surface while monitoring the change of uniaxial
compressive displacement with time at high temperature (86,87). Typical specimens tested with this method measure
10 " 10 " 2.5 mm. Excellent agreement with conventional uniaxial creep results was reported for tests performed on servo-electric
test machines (87,88).
The most innovative small specimen for creep testing proposed to date is the diametrically loaded elliptical or circular ring-type
specimen shown in Figure 18 (85,89). This specimen can be loaded either in tension or in compression, and its test-section area
(beam cross section) is about 5–10 mm2, corresponding to dimensions as small as 2a ¼ 10 mm, d z 10 mm, and b0 z 2 mm. Refer
to Figure 18 for the meaning of the symbols.
Results obtained with this geometry on a Cr–Mo steel (P91 grade) at 650 * C indicated an excellent agreement in terms of
minimum creep strain rate (MSR), as shown in Figure 19. The ring specimens (circular or elliptical) are easy and inexpensive to
Figure 18 Diametrically loaded ring creep test specimen. The depth (length) of the ring is b0, perpendicular to the plane of the figure. Reproduced from
Hyde, T. H.; Sun, W. A Novel, High-Sensitivity, Small Specimen Creep Test. J. Strain Anal. 2009, 44, 171–185.
Figure 19 Minimum creep strain rate data for P91 steel obtained from uniaxial and circular ring creep tests at 650 * C. Reproduced from Hyde, T. H.;
Sun, W. A Novel, High-Sensitivity, Small Specimen Creep Test. J. Strain Anal. 2009, 44, 171–185.
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manufacture, and the experimental setup is simple to operate. Analytical relationships to determine material creep properties were
obtained by means of finite element analysis and were validated by comparisons with conventional specimen data. The method is
versatile and can be used on a wide range of materials. It is suitable for determining minimum creep strain rate data, particularly at
relatively low equivalent uniaxial stresses.
1.08.7 Creep Crack Growth Testing
Creep crack growth (CCG) properties are increasingly required for remaining-life assessments of components subject to high
temperature during service, such as boiler tubes, steam pipes, steam turbine casings, and steam turbine rotors.
The earliest published works on CCG testing with small specimens were performed by Jaske (90) and Majumdar et al. (91), who
used small single-edge-notched-tension, SE(T), samples of Type 316 stainless steel with 12.7 " 12.7 mm cross section and short
cracks (0.1–0.5 mm deep). A good correlation was shown among CCG data of miniature specimens and larger standard-size
specimens.
Small single-edge notched tension SE(T) specimens of several Cr–Mo steels (both base metal and weldments) were tested in air
at 538 * C by Jaske and Viswanathan (92). The specimens had a thickness of 1.5 mm, while the gauge sections had widths of 5, 7.5,
and 10 mm and lengths of 10, 15, and 20 mm, respectively. They were precracked in fatigue, with the propagation of the crack
monitored by the use of the direct current (DC) potential drop technique. The same technique was also used to assess creep crack
growth during the actual tests.
The results obtained demonstrated that reliable CCG data could be obtained with miniature SE(T) test results for base metals, in
comparison with full-size C(T) specimens. Conversely, the results obtained on weldments were not as successful, since for the
smallest samples, no crack growth was observed in the notch region and significant creep deformation was detected in the gauge
section, which was well away from the notch region. The authors conclude that the problem of local strength variation in weld
specimens can be overcome by increasing the initial precrack length in future testing (a/W > 0.1).
1.08.8 Extreme Miniaturization (Part 1): Small Disk Testing
In the field of experimental techniques based on subsize or miniaturized specimens, methodologies based on testing small disks
represent a virtually nondestructive method for characterizing the mechanical properties of service-exposed plant components.
Indeed, the very small size of the specimens means that the amount of the material sampled from the component is practically
negligible. Moreover, a considerable number of disk specimens can be extracted from mechanical machining leftovers or from
conventional specimens that were broken during previous tests.
Two main classes are considered here: the shear punch test and the small punch test (or bulging type disk test). The former is
addressed first, due to its relative simplicity.
1.08.8.1 Shear Punch Testing

In shear punch testing (93,94), the disk is clamped, the punch is a flat cylindrical penetrator, and the die is a close fit to the punch
diameter. The contact angle between the punch and the specimen remains constant with applied force as the punch travels through
the specimen, and shear properties (rather than tensile properties) are directly measured. Earlier specimens were similar to trans-
mission electron microscope (TEM) foils with 3 mm diameter and 0.25 mm thickness; later investigations used larger samples with
6–10 mm diameters and larger punch sizes (95).
The deformation is concentrated into the narrow region between the punch and the die, with some limited bending
outside the annulus region, in addition to the shear deformation. Figure 20 shows examples of shear stress versus
displacement curves with displacement (deflection) measured both at the machine actuator and at the loading point on the
punch. The effect of test setup compliance is significant (96), and the advantage of using low-compliance loading devices is
evident.
Shear punch tests can be used to estimate yield and ultimate tensile strength properties by the use of forces at deviation
from linearity and maximum forces to obtain effective shear yield and ultimate stresses, which in turn empirically correlate
to corresponding uniaxial properties (93,97), see Figure 21. The correlation slope m is around 2, depending on
the characteristics of the test system and the amount of bending occurring during the test. A similar empirical
correlation was established between the strain-hardening exponent obtained from shear punch tests and the tensile uniform
elongation (98).
Recent improvements in the test apparatus included a shortened, stiffer penetrator and a more direct measurement of the punch
displacement, resulting in an improved correlation between shear and tensile properties (99). It was also reported that yield and
ultimate tensile stresses were only weakly dependent on the ratio between specimen thickness t to grain size d for t/d , 5 (100).
Some applications of shear punch testing that have been documented in literature are the study of the performance of total hip and
knee replacements (101), the characterization of bulk metallic glass (102), and the investigation of the behavior of propellants and
explosives during impulsive loading (103).
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Figure 20 Examples of shear stress–displacement curves showing the effect of test setup compliance. Reprinted from Toloczko, M. B.; Kurtz, R. J.; Abe, K.;
Hasagawa, A. Tensile Property Estimates Obtained Using a Low Compliance Shear Punch Test Fixture. In Effects of Radiation on Materials: 21st International-
Symposium, ASTM STP 1447; Grossbeck, M. L., Allen, T. R., Lott, R. G., Kumar, A. S., Eds.; ASTM: West Conshohocken, PA, 2004, pp 655–669.
Figure 21 Empirical relationship between shear yield stresses ssy from shear punch tests and tensile yield stresses sy from uniaxial tests.
Reprinted from Hankin, G. L.; Toloczko, M. B.; Hamilton, M. L.; Garner, F. A.; Faulkner, R. G. Validation of the Shear Punch – Tensile Correlation Technique
Using Irradiated Materials. J. Nucl. Mater. 1998, 258–263, pp 1651–1656.
1.08.8.2 Small Punch Testing

1.08.8.2.1 Derivation of Tensile and Fracture Properties
The small punch test, also known as the disk bend test, was developed in the mid-1980s (104,105) and used small TEM-size disks
(3 mm diameter, w0.25 mm thickness) centrally loaded by a spherical ball or hemispherical punch and expanded into a larger
lower die size. The test system was a module that could be placed between the loading platens of a tensile machine and subse-
quently loaded (105). The outcome is a bulge in the disk rather than a shear cut, as in the previously described methodology. An
example of an experimental setup used for small punch tests is shown in Figure 22.
Note that, although the TEM-size disk is the most commonly used geometry, round specimens with diameters up to 10 mm and
thicknesses up to 0.5 mm have been used. The use of square specimens (10 " 10 mm) has also been reported (106).
The general form of the force/deflection test record is shown in Figure 23. Five distinct regions can be identified:
1. Elastic region,
2. Departure from linearity,
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Figure 22 Example of test setup for performing small punch tests.
Figure 23 Example of force/deflection curve for a small punch test on a specimen with diameter ¼ 8 mm and thickness ¼ 0.5 mm. The five regions
mentioned in the text are indicated in the figure.
3. Local bending, transitioning to a membrane stress regime,

4. Membrane stress regime, and
5. Final failure region.
The general form of the test record suggests that yield stress is associated with the change in slope between regions 1 and 2, where
the ultimate tensile stress appears with peak force and ductility with maximum deflection. Note that for steels showing low ductility,
regions 4 and 5 may be absent or minimized.
Once force and deflection data are recorded, characteristic values of force, deflection, and energy are identified on the test record.
These values are generally fed into semiempirical correlations in order to obtain estimates of several mechanical properties present
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for the material under investigation. Such correlations were developed by comparing characteristic parameters from the small punch
test with tensile properties, transition temperature data, and fracture toughness values measured through conventional tests.
Typically, the correlations are strongly dependent on the material (or the class of material in the most favorable scenario) under
investigation, and cannot be expected to be applicable on a more general level (106).
A relevant example is the correlation between transition temperatures that are measured from standard Charpy specimens,
FATT50, and those measured from small punch tests, TSP (107,108). If one plots the punch fracture energy, defined as the area under
the force–deflection curve up to specimen fracture or maximum force, as a function of temperature, a typical transitional behavior is
observed (see Figure 24). The value of the small punch transition temperature TSP is established at the midway position between the
lower- and upper-shelf energies.
Several empirical correlations between TSP and FATT50 have been published (107–110). Each relationship is specific to the
material considered and is directly influenced by the details of the disk and punch geometry, loading configuration, and test
procedure. Most empirical relationships have the form:
FATT 50 ¼ A þ B " TSP [11]
where the values of fitting constants A and B depend on material and experimental configuration (107). Moreover, Foulds and
Viswanathan (107) showed a clearly linear relationship between TSP and FATT50 (Figure 25), while Ha and Fleury (108) stated
that:
TSP
¼ 0:35 [12]
FATT50
The strong reduction in transition temperature from Charpy to small punch tests was attributed to the much lower strain rate that
is associated with disk testing.
Other researchers have derived alternate methods for estimating fracture toughness from small punch test data. They tend to be
more mechanistic in nature and are based on characteristic strains and correlations with critical fracture toughness values in both the
brittle and ductile regimes.
Ha and Fleury (108) published a semimechanistic model that provided small punch-based estimates of the plane-strain stress
intensity factor KIc and the critical value of the J-integral at crack initiation JIc, which were shown to be in good agreement with KIc
and JIc estimates obtained from Charpy tests.
Figure 24 Example of fracture energy transition curve obtained from small punch tests for a 12Cr1Mo steel. Reprinted from Ha, J. S.; Fleury, E.
Small Punch Tests to Estimate the Mechanical Properties of Steels for Steam Power Plant: II. Fracture Toughness. Int. J. Pres. Ves. Pip. 1998, 75 (9),
pp 707–713.
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Figure 25 Relationship between TSP and FATT50 for CrMoV rotor steels. Reprinted from Foulds, J. R. Viswanathan, R. Small Punch Testing for
Determining the Material Toughness of Low Alloy Steel Components in Service. J. Eng. Mater. Technol. 1994, 116, 457–464.
These approaches show definite promise, although they are based on a number of assumptions and are valid only for a specific
test and loading configuration.
An alternative methodology for assessing constitutive behavior and fracture properties by means of small punch testing was
developed in the mid-1990s in a research project sponsored by EPRI (111,112). The experimental setup (depicted in Figure 26)
included the use of a displacement transducer (clip-on gauge) for measuring the actual specimen deformation, as well as
a magnifying video camera for determining the instant of fracture initiation.
The force/deflection curve of the small punch test was reproduced through FE analyses, by iteratively deriving the consti-
tutive parameters (the true stress/true strain curve) and the tensile properties of the material. Based on a theoretical fracture
criterion, the critical fracture toughness KIc was calculated when a critical value of strain energy density (corresponding to
fracture initiation in the small punch test, as identified in the analysis of the video) was reached in a fracture mechanics test on
a conventional C(T) specimen, which was also simulated by FE calculations. A schematic of the methodology is shown in
Figure 27.
Published results (106,112) were satisfactory in terms of stress–strain curves, but not in terms of fracture toughness predictions.
The main issue in this case seems to be the exact identification of crack initiation in the video recording of the test.
A similar approach was more recently proposed involving 10 " 10 " 0.5 mm through–thickness-notched specimens of A508
pressure vessel steel (113). Crack initiation was detected by acoustic emission, and conversion to a toughness value was obtained
through analytical modeling. Published results showed promise when compared with data obtained for A508 from conventional
tests.
1.08.8.2.2 Derivation of Creep Properties

Creep testing with small punch samples has been almost exclusively studied in Europe, with more limited studies in Japan. Typical
specimens are disks with diameters of 8–10 mm and thickness of 0.5 mm, which are tested using a punch diameter of w2 mm.
More limited creep work has been published with disks with a 3–4 mm diameter.
The applied loading is held constant at a high temperature during the test. With a few exceptions, tests are performed in an inert
argon environment in order to minimize oxidation effects, and large deformations are recorded with respect to the specimen
thickness. Figure 28 shows the test data obtained for a P91-welded joint (114).
As in conventional creep curves, there appear to be primary, secondary, and tertiary regions. However, detailed finite
element analyses (115) showed that two distinct zones can be observed for the punch displacement during the test: (1) dishing
of the supporting edge, and (2) necking near the edge of the contact zone. The failure location is near the edge of contact
between the punch and the specimen, and analytical expressions were determined by relating the strain at the edge of the
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Figure 26 Configuration of the experimental setup used for performing SP tests with the approach developed for EPRI. Reprinted from Bicego, V.;
Lucon, E.; Sampietri, C. The ‘Small Punch’ Technique for Evaluating Quasi Non-Destructively the Mechanical Properties of Steels. In Fracture from Defects
– ECF 12: Proceedings of the Twelfth European Conference on Fracture; Brown, M. W., de los Rios, E. R., Miller, K. J., Eds.; EMAS Publishing, 1998; Vol. 1,
pp 1273–1278.
contact position to the punch displacement (115). Similarly, a relationship between the strain, the punch displacement, and
the ratio P/s of the force to membrane stress was determined. As a result, the experimentally obtained deflection/time curves
could be analytically converted to strain versus time curves, and stationary strain rates could be obtained from the secondary
stages of the creep tests (115).
Excellent agreement with conventional creep data was documented, as shown in Figure 29, for a 14MoV63 alloy steel (116).
At present, the small punch creep test does not have a universally accepted route for interpreting the primary, secondary, and
tertiary contributions to the overall displacement/time curves (89). The available literature on the subject mainly focuses on creep
rupture life, and only a limited number of researchers have tried to use the full creep curves to derive all creep properties, including
the Norton creep law (117), Kachanov damage model constants (118), and rupture-time dependence on stress and ductility.
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Figure 27 Schematic of the methodology for deriving stress–strain curves and fracture toughness parameters. Reprinted from Bicego, V. Lucon, E.
and Sampietri, C. The ‘Small Punch’ Technique for Evaluating Quasi Non-Destructively the Mechanical Properties of Steels. In Fracture from Defects –
ECF 12: Proceedings of the Twelfth European Conference on Fracture; Brown, M. W., de los Rios, E. R., Miller, K. J., Eds.; EMAS Publishing, 1998; Vol. 1,
pp 1273–1278.
Figure 28 Typical displacement–time curves obtained from small punch tests on a P91 welded joint. Reproduced from Sturm, R.; Jenjo, M.; Ule, B.;
Solar, M. Small Punch Testing of Smart Weld Materials. In Proceedings of the 2nd International Conference on Structural Integrity of High Temperature
Welds; IOM3 Communications: London, November 2003, pp 269–278.
Figure 29 Comparison of creep data between small punch and conventional uniaxial tests for a 14MoV63 steel. Reproduced from Dobe!s, F.; Mili!cka, K.
On the Monkman-Grant Relation for Small Punch Data. Mater. Sci. Eng. A 2002, 336 (1–2), pp 245–248.
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In other words, as the behavior of the small punch specimen is complex, there is, as yet, no commonly accepted method for data
interpretation.
Nevertheless, at the time of writing, detailed test procedures for specimen setup, temperature control, and data analysis have
been established, and a code of practice exists for small punch specimen creep testing (119).
1.08.9 Extreme Miniaturization (Part 2): Use of Microfabrication Technology
In a 1982 article, Petersen (120) announced a new manufacturing paradigm and a new construction material to the world of
mechanical structures: lithography of silicon. In the decades since, the field of MEMS (micro-electro-mechanical systems), which
consists principally of the design and fabrication of structures in silicon by photolithography, has blossomed. This process allows
the economical and precise fabrication of a variety of devices, mainly sensors for acceleration and pressure (121), but also functional
devices, such as nozzles for automotive fuel injectors and ink-jet printers (122).
The materials science of the components of microelectronic devices, particularly ultra-large-scale integration (ULSI) chips, also
blossomed during the same decades (123). These studies naturally included mechanical properties, because of their importance to
the general reliability of microfabricated devices, including both electrical and mechanical reliability. The techniques for microscale
mechanical testing can be found in the literature; starting points include (124,125). However, microscale test devices have thus far
only been applied to microscale materials, such as vapor-deposited thin films, and exotic materials, such as carbon nanotubes. This
is because of the difficulty in fabricating and handling specimens from conventional ‘bulk’ materials that are small enough to be
tested with the microscale apparatus. This is not a large issue for the microscale materials because they are very small to begin with,
and they can often be cofabricated with the test apparatus, for example, by physical vapor deposition. The principal instance of
cross-fertilization between the worlds of microscale materials and conventional structural materials has been nanoindentation
(126), which not only enables hardness testing of thin films, but also hardness testing of conventional structural materials at
unprecedented spatial resolutions.
The possibility of adapting techniques from the world of microfabrication for downsizing the testing of conventional materials is
currently being explored (127). The particular motivation for this study is to facilitate testing in harsh environments. The down-
sizing of mechanical test specimens and apparatus is advantageous for developing new materials for harsh environments for the
following reasons:
1. Supplies of special specimen material (e.g., nanostructured or developmental alloys) may be limited.
2. A smaller specimen size means that a smaller ‘harsh environment’ is needed, which leads to safer tests and less waste material.
3. Certain harsh treatments, for example, irradiation methods, may be limited in penetration depth into the material surface. With
a sufficiently small specimen, full thickness treatment may be convenient.
4. Smaller specimens may facilitate in situ testing within a given harsh environment.
Since mechanical testing begins with the specimen, we examined available techniques of producing small components incor-
porating bulk structural materials. Photolithography by commercial vendors was utilized, with acceptable results for the first test
case. Specimens 25 mm thick by 70 mm wide were produced from commercially obtained foils of stainless steel and aluminum (see
Figure 30).
Photolithography of metal grips seemed problematic, but photolithography of silicon has been extensively developed for
MEMS. Silicon wafers 250 mm thick are widely available, and wedge grips that match the typical bow-tie specimen geometry
normally used for testing sheet metal (128) were fabricated. However, contrary to the usual orientation of wedge grips, where the
Figure 30 Microfabricated tensile specimens fabricated by photolithography.
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1600
1400
Engineering stress, MPa

1200
1000
800
SS302 sp 1202
600
400
200
0
0 0.01 0.02 0.03 0.04 0.05
Engineering strain
Figure 31 Typical engineering stress–strain curve obtained for microtensile tests of SS302.
wedges clamp the flat faces of the specimen, here the grips were designed to mate with the specimen edges. For the geometry used in
this testing (127), no problems were seen. To maintain grip-to-grip alignment and spacing, these were integrated in a compliant
frame. The benefits of microfabrication had already come into play: the expansion of the component from grips alone to grips in
a compliant frame did not increase the cost of fabrication.
Ideally, the MEMS device would be expanded beyond the grips and compliant frame to include a source of force to apply tensile
force to the specimen. This development remains in the future for tension testing. Instead, an external actuator developed for thin-
film testing (129) was modified and used to supply and measure the force. Testing under an optical microscope (a common
microscale approach) was no problem, because of the small size of the frame, and allowed the acquisition of images that were
analyzed by digital image correlation to provide strain data. Credible stress–strain curves for the full-hard stainless steel specimen
material were documented (see Figure 31) (127).
1.08.10 Concluding Remarks and Future Trends
An extensive review of the current state of the art of small-specimen test technology (SSTT) has been presented, covering a number of
experimental techniques aimed at characterizing the mechanical properties of materials and components through the use of subsize
or miniaturized specimens. It appears that viable test techniques are currently available for all the designs considered and that the
experimental requirements can be met, even though some of the specimen designs are extremely small. (It is the personal opinion of
the author that SSTT should only be used when conventional, full-scale testing is not feasible or advisable. The use of well-
established test procedures and specimen geometries generally reduces data uncertainty and favors the public acceptance of the
results obtained.) Nevertheless, it is clear that several potential issues and future challenges require continued effort from the
scientific community.
The first of these issues is the existence of inherent size effects, which are closely related to the number of metallurgical features
included in the specimen test region. Scientists seem to agree that a homogeneous structure, with at least six to 10 grains or 200 to
500 microstructural features within the deforming section, should allow characterizing the ‘bulk’ properties of a material by means
of very small specimens. In all cases, specimen dimensions should contain representative microstructures of the material under
investigation.
Second, for toughness-related methodologies, the constraint changes induced by miniaturization must be addressed either by
correlating small-specimen data with conventional test results (e.g., subsize Charpy impact tests) or by ensuring that minimum size
requirements, such as specimen-measuring capacity, are met (e.g., fracture toughness test methods). Nevertheless, as stated by
Birkett (130), reduced constraint can be realistic in applications where the actual constraint does not correspond to the maximum
value provided by a ‘conventional’ test, and the degree of conservatism in an assessment must be reduced. An aspect that should not
be overlooked is that the degree of constraint could be related to more fundamental material properties, which could be measured
in a more meaningful way through the use of smaller specimens.
Another issue to consider is that the measurement uncertainties increase as the size of test specimens decreases. Statistical
measures of uncertainty, such as the number of small specimens tested, need to be duly considered in view of the way in which
uncertainties propagate through model predictions.
The usefulness of FE studies for the optimization and validation of small-specimen test techniques has been clearly established.
In order to be most effective, most of these techniques must be closely integrated with FE simulations and fundamental models of
deformation and fracture (21). The importance of harmonizing mechanical characterization techniques with nondestructive
evaluations and microstructural analyses has also been acknowledged.
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A straightforward comparison of SSTT results with data measured from larger specimens, tested in accordance with well-
established test standards, remains a more practical approach for validating and qualifying results obtained from nonstandard
specimens. These efforts are particularly fruitful when conducted in the framework of international round-robin collaborations and
interlaboratory comparisons.
For tests performed at high temperature (creep, creep crack growth, and others) on oxidation-sensitive materials, it is imperative
that miniature tests be conducted in an inert environment, such as high-purity argon or vacuum.
Regulations and codes are still hesitant in allowing the use of small specimens, and most test standards do not implicitly or
explicitly cover specimen miniaturization. Nevertheless, convincing data are available to support the reliability of mechanical
properties measured by means of the techniques described in this chapter. Substantial efforts are required from the scientific and
standardization communities in order to give SSTT its well-deserved recognition.
The contents of this chapter almost exclusively rely on applied research, and draw heavily on comparisons between small-size
and full-size specimen results, as a means of validating SSTT. A different approach is basic science, whereby a researcher would strive
to find the underlying (physical) sources of size effects and what might be done to address them. An example would be, in tensile
testing, investigating the possibility of predicting the behavior of a multigrain specimen based on the information on the behavior
of individual grains and grain boundaries. In the field of fracture, one of the goals could be to reach an understanding of the role that
constraint effects play on fracture toughness without testing specimens large enough to provide the same degree of constraint as in
actual structures or components.
In conclusion, the available literature seems to indicate that SSTT has reached a robust state of maturity. Tests that were
considered novel or innovative only a short time ago are now routinely used in a number of ongoing and future experimental
programs. The biggest current challenge may be to successfully transfer some of the laboratory-based methodologies in order to
provide real-time, in situ measurement of properties of components in use in the field.
Acknowledgments
The valuable contribution of Dave Read (NIST, Boulder CO), the sole author of Section 1.08.9 on Microfabrication Technology, is
gratefully acknowledged.
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1.09 Advanced High Strength Bainitic Steels
C Garcia-Mateo and FG Caballero, National Center for Metallurgical Research (CENIM-CSIC), Madrid, Spain

1.09.2 Theory for Bainite Phase Transformation 166
1.09.3 First Approaches to the Design of Carbide-Free Bainitic Steels, AHSS-GEN3 for Automotive Applications 167
1.09.4 A New Steel Concept for the Twenty-First Century: Nanostructured Bainitic Steels (NANOBAIN) 171
1.09.5 Accelerating Low-Temperature Bainite Transformation 175
1.09.6 Advanced Characterization of Nanostructured Steels 177
1.09.7 Understanding the Mechanical Properties of Advanced Bainitic Steels 182
1.09.7.1 Strength 183
1.09.7.2 Ductility 184
1.09.7.3 Toughness 186
Acknowledgments 187
References 188
1.09.1 Introduction
The automotive industry is one of the greatest markets for materials produced in the steel sector, but it is also one of the most
dynamic, due mainly to governmental requirements that change according to newer, stricter environmental and security policies.
In terms of materials used, it is no surprise that cars made in the 1970s and those made in the twenty-first century differ greatly.
Requirements for faster, cheaper, lighter, safer, more reliable, and more environmentally friendly cars have opened the door for new
materials to be used instead of steel, such as Al, Mg, and plastics. Far from being intimidated, the steel community has used these
new challenges as the main driving force to keep reinventing steel through continuing research and development, which helps to
satisfy these new objectives. Steel now represents 57% of the material content of an average car (1).
In recent years, we have witnessed an increased emphasis on the development of new advanced high strength steel (AHSS).
Descriptive terminology has evolved to describe the ‘First Generation,’ GEN1, of AHSSs, which are steels that possess primarily
ferrite-based microstructures, and the ‘Second Generation,’ GEN2, of AHSSs, which are austenitic steels with high Mn content, and
which include steels that are closely related to austenitic stainless steels. First-generation AHSSs have been referred to by a variety of
names, including dual phase (DP), transformation-induced plasticity (TRIP), complex phase (CP), and martensitic (MART) steels.
Second-generation austenitic AHSSs include twinning-induced plasticity steels, Al-added lightweight steels with induced plasticity
(L-IP"), and shear band strengthened steels (SIP).
The new generation of AHSSs, GEN3, must address some fundamental challenges:
1. What types of microstructures are needed to reach the performance and cost targets of AHSS-GEN3, while avoiding the man-
ufacturability (formability and weldability) issues that hinder the application of AHSS-GEN1?
2. How do we quantitatively relate the material’s microstructure to its macroscopic performance, i.e., stress versus strain, forming
limit diagram, stretch formability, weldability, and other properties?
3. How do we achieve the required microstructures with a cost-effective chemistry and in a practical thermal mechanical processing
route that is less costly than that needed for AHSS-GEN2?
From a theoretical point of view (2), the increase in both strength and ductility in AHSSs requires an optimum combination of
hard and soft second-phase particles in the microstructure. As a result, AHSS-GEN3 will include materials with complex micro-
structures that consist of a high strength phase (e.g., ultrafine-grained ferrite, martensite, or bainite) and significant amounts of
a constituent that has substantial ductility and work hardening (e.g., austenite). The goal is to achieve properties that lie in the
intermediate band, identified in Figure 1 (3). By using the new generation of AHSSs, automakers estimate a potential reduction of
almost 35% of the total weight of a vehicle’s body structure (4).
So far, AHSS-GEN1 such as TRIP steels cannot be easily used for a wide variety of car components, because their formability is
relatively poor (5). When total elongation is increased, properties governed by local elongation, such as stretch flangeability and
bendability, tend to deteriorate (6). For securing large total elongation, it is beneficial to have a microstructure composed of a soft
phase, such as ferrite, and a harder second phase, such as bainite and/or martensite (7). The presence of retained austenite in the
microstructure will enhance the total elongation even further by means of the TRIP effect (8). In contrast, for a good hole
expansibility and bending behavior, the microstructure should be rather homogeneous. Otherwise, local strain concentration will
occur at the soft phase near the hard phase, and as a consequence, stretch flangeability and bendability will deteriorate (5,6).
When the microstructure is composed of a uniform matrix structure of a fine lath, such as that found in bainitic ferrite, an
excellent stretch flangeability is expected (9). In addition, if a hard second phase is present, such as martensite, the expected hardness
heterogeneities will allow good deep drawability to be obtained (10). It has been also shown that bendability is not related to
Comprehensive Materials Processing, Volume 1 http://dx.doi.org/10.1016/B978-0-08-096532-1.00114-X 165

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166 Advanced High Strength Bainitic Steels
Figure 1 Comparison of total elongation vs yield strength of conventional steels and those expected for the third generation of AHSS. Note: IF:
Interstitial free, ISO: Isotropic, DP: Dual phase, CP: Complex phase.
ductility, and as a result, heterogeneity in the microstructure should be as low as possible (6). Thus, a carbide-free bainitic
microstructure consisting of a bainitic ferrite matrix and a mixture of austenite and some martensite seem to be optimal to achieve
a good combination of the previously mentioned in-use properties.
1.09.2 Theory for Bainite Phase Transformation
‘Bainite’ named for E. C. Bain (11) is the generic term for fine aggregates of ferrite (a) platelets (or laths) separated by regions of
residual phases, untransformed austenite (g), or cementite (q). The transformation occurs from austenite (g) at temperatures
between those at which pearlite and martensite form. The aggregates of plates that share common crystallographic orientations are
designated as ‘sheaves,’ whereas individual plates are also called subunits. There is a considerable amount of extensively reviewed
experimental evidence (12–21) that allows the presentation of the displacive mechanism theory as the most plausible explanation
for bainite transformation.
The mechanism by which bainite grows places strict limits on the temperature range for transformation, as well as on the
maximum fraction of transformation that can be achieved. These criteria for bainite formation are embedded in the concept of the
T00 curve, which is the locus of points, on a temperature vs C concentration plot, where austenite and ferrite of the same chemical
composition have the same free energy, taking into account the stored energy of the ferrite due to the displacive mechanism of
transformation (400 J mol'1) (15,22).
Thus, bainite formation is expected to occur below the T00 temperature when
DGg/a < 'GSB and DGm < GN [1]
'1
where GSB y400 J mol is the stored energy of bainite and DGg/a is the free energy change of the transformation of g without any
change in chemical composition (23). The first condition refers to the limits of growth, while the second refers to the nucleation
conditions; thus, DGm is the maximum free energy change that accompanies nucleation under paraequilibrium conditions. GN is
the universal nucleation function (24) and defines the minimum free energy change that is necessary in any steel in order to nucleate
bainite. The temperature at which both conditions are fulfilled is known as the bainite start temperature, BS.
Soon after the diffusionless growth of a bainitic ferrite subunit is over, excess C is partitioned to the surrounding austenite. The
process continues by successive nucleation of subunits until the C concentration of the residual austenite reaches the value at which
the free energy of bainite becomes less than that of austenite of the same composition, i.e., the T00 curve. This trend is known as the
‘incomplete reaction phenomenon’ because the transformation ends before the C concentration of austenite reaches the equilib-
rium value. Due to the negative slope of a temperature versus austenite C concentration plot of the T00 curve, the lower the
transformation temperature, the further the transformation can proceed, because a higher amount of C in solution is allowed in
austenite; in other words, higher fractions of bainitic ferrite are obtained. Cementite can then precipitate from the enriched austenite
between the ferrite plates and within the bainitic ferrite plates (both upper and lower bainite); the difference comes from the
competition between the rate at which cementite can precipitate from ferrite and the speed with which C is partitioned from
supersaturated ferrite into austenite.
Upper bainite forms at higher temperatures, permitting the excess C to partition before it can precipitate in ferrite. In lower
bainite, the slower diffusion associated with lower transformation temperatures provides an opportunity for some of the C to
precipitate in the supersaturated ferrite (25). Silicon can prevent the precipitation of cementite from the austenite between the plates
of bainitic ferrite, but it has only a limited effect on precipitation from supersaturated ferrite, where the driving force for cementite
formation is much larger (26). Silicon has very low solubility in cementite, and must be trapped in cementite during its para-
equilibrium growth. The bainite transformation temperatures do not allow or limit the mobility of Si, which dramatically reduces
the free energy change associated with precipitation, with a correspondingly large reduction in precipitation kinetics (26). The C that
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Advanced High Strength Bainitic Steels 167
is partitioned into the residual austenite after bainitic transformation does not precipitate as cementite, but remains there to make
the austenite stable at ambient temperature (27–29).
The microstructure obtained in Si-rich steels consists of fine plates of bainitic ferrite separated by C-enriched regions of austenite,
and we will return to it later in this chapter.
The martensitic-type growth of bainite causes a certain type of deformation, which is an invariant plane strain with a larger shear
component (s z 0.26) and a dilatational strain (d z 0.03) normal to the habit plane (13,23,30–33). In plain language, this means
that the transformation involves a change not only in the crystal structure, but also in the material deformation. The magnitude of
these strains is so large that the transformation product is constrained to be in the form of a thin plate, a shape that minimizes the
strain energy when the plate is elastically accommodated. If the strain is elastically accommodated, then the strain energy of bainitic
ferrite amounts to about 400 J mol'1. However, direct observations have shown that there is considerable plastic relaxation in the
austenite adjacent to the bainite plates (32–34), which involves multiple-slip systems (12). It is only when plastic relaxation takes
place that the dislocations associated with the plastic strain are inherited by the product phase, which is bainitic ferrite. In this sense,
experimental results on the distribution of dislocation density in the bainitic ferrite plate as a function of the distance to the closest
austenite–ferrite interface revealed a progressive increase in the dislocation density as the interface was approached (21,35).
Dislocations in the central region of the ferrite plate result from the lattice-invariant deformation at the earlier stage of bainite
growth, whereas the higher dislocation density in bainitic ferrite in the vicinity of the austenite–ferrite interface is related to the
plastic deformation that occurs in the surrounding austenite to accommodate the transformation strain as growth progresses and
dislocations are inherited by the freshly formed bainitic ferrite. The dislocation debris generated in this process resists the advance of
the austenite–ferrite interface, the resistance being greatest for strong austenite (36). Consequently, the yield strength of the
austenite must therefore feature in any assessment of plate size. In this scenario, the plates are expected to become thicker at high
temperatures, because the yield strength of the austenite will then be lower. The thickness must also be influenced by impingement
between adjacent plates, and a large nucleation rate, i.e., a large driving force, corresponds to a finer microstructure.
1.09.3 First Approaches to the Design of Carbide-Free Bainitic Steels, AHSS-GEN3 for Automotive Applications
As cementite is a hard and brittle phase that can impede the mechanical properties of regular bainitic steels, metallurgists soon
realized that cementite should be eliminated in order to make bainite a desirable microstructure. As previously mentioned, Si
additions can prevent the precipitation of cementite. By doing so, the C that is partitioned into the residual austenite after bainitic
transformation does not precipitate as cementite, but remains there to make the austenite stable at ambient temperature (27–29).
The final microstructure consists of fine plates of bainitic ferrite separated by C-enriched regions of austenite.
In previous research by Bhadeshia and Edmonds (27,29) and Miihkinen and Edmonds (37–39), it was found that a carbide-free
bainite microstructure has, in principle, some potential advantages:
1. Cementite is responsible for initiating fracture in high strength steels; its absence is expected to make the microstructure more
resistant to cleavage failure and void formation.
2. The ductile films of austenite, which are intimately dispersed between the plates of ferrite, have a crack-blunting effect. They
further add to toughness by increasing the work of fracture, as the austenite is induced to transform to martensite under the
influence of the stress field of a propagating crack. This is called the TRIP.
3. There is a possibility of simultaneously improving the strength and toughness of a given material, because of the ultrafine grain
size of the bainitic ferrite plates. The microstructure derives its strength from the fine grain size of the ferrite plates, which are less
than 1 mm in thickness.
These original experiments (27,29) were carried out in order to demonstrate the role that the T00 curve has in greatly influencing
the mechanical properties of carbide-free bainitic steels. The experimental alloys developed for this purpose are not necessarily the
optimal alloys for certain mechanical properties and some types of product development.
The essential principles that govern the optimization of carbide-free bainitic microstructures are well established, particularly
that an increase in the amount of bainitic ferrite in the microstructure is needed in order to eliminate large regions of untransformed
austenite, which can transform to hard, brittle martensite when placed under stress. With this principle in mind, it was recently
experimentally demonstrated that models based on the phase transformation theory can be successfully applied to the design of
hot-forged, carbide-free bainitic steels (40–42). Two medium C steels, 0.3 wt.% C (with enough Si, 1.5 wt.%, to avoid cementite
precipitation), 1.30 wt.% Cr, 0.25 wt.% Mo, 3.5 wt.% Ni, and both with and without V (0.1 wt.%), were specifically designed to
achieve the highest combination of strength and toughness for bainitic microstructures after air cooling. Toughness values of
w130 MPa m1/2 were obtained for strength values in the range of 1600–1700 MPa. Following the success of the first experiments of
Caballero et al. (40,41), a second set of alloys was designed (43). For such a design, the alloys’ chemical composition was carefully
chosen, following (42), so as to have the same T00 and time-temperature-transformation (TTT) diagram as those rich Ni alloys in
(40,41), but without Ni, for economic reasons and to give the alloys enough hardenability to avoid the formation of proeutectoid
ferrite during cooling.
Table 1 shows the chemical composition of Ni2 that corresponds to one of the first sets of alloys used as a reference to design the
second set of alloys, 0.3BAIN 1 to 4 in Table 1. Figure 2 (43) shows that the T00 curve and TTT diagrams for the newly designed steels,
0.3BAIN 1 to 4, and those for the Ni2 steel, match perfectly. Theoretical BS and MS temperatures are identical for all steels and are
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Table 1 Chemical composition of bainitic steels, wt.%
Steel C Si Mn Ni Cr Mo V
Ni1 0.31 1.51 <0.01 3.52 1.44 0.25 0.10

Ni2 0.30 1.51 <0.01 3.53 1.42 0.25 –
0.3BAIN 1 0.29 1.50 2.25 – – 0.26 –
0.3BAIN 2 0.29 1.46 1.97 – 0.46 0.25 –
0.3BAIN 3 0.29 1.49 1.56 – 1.47 0.25 –
0.3BAIN 4 0.27 1.71 1.53 1.47 0.17 0.24 –
0.2BAIN 5 0.22 1.50 2.23 – – 0.25 –
0.2BAIN 6 0.21 1.46 1.56 – 1.49 0.24 –
Figure 2 (a) T00 curve and (b) TTT diagram of 0.3BAIN steels and Ni2, used as a reference after Caballero, F. G.; Santofimia, M. J.; Capdevila, C.;
García-Mateo, C.; De García Andrés, C. Design of Advanced Bainitic Steels by Optimisation of TTT Diagrams and T0 Curves. ISIJ Int. 2006, 46
(10), 1479–1488.
shown as the diffusionless part of the TTT diagram. This is not surprising, since those steels have been designed to have the same
maximum volume fraction of bainite at a given temperature (43). According to the calculated TTT diagrams, a two-step cooling
schedule seemed the most suitable method to obtain a fully bainitic microstructure in the new alloys.
The proposed alloys were hot rolled in several passes finishing at 930 * C, and the bainitic microstructure in all the steels was
obtained by air cooling from different temperatures (shown as finishing cooling temperature also referred as interrupted accelerated
cooling temperature (FCT) in Table 2) after an initial accelerated cool at 70 * C s'1. Experimental data on the microstructures are
presented in Table 2. It is clear that, regardless of the FCT temperature, the microstructure is fully bainitic, with more than 75%
being bainitic ferrite. Further analysis using SEM, Figures 3(a) and 3(c), and TEM, Figures 3(b) and 3(d), confirmed that in all the
cases, both the bainitic ferrite and the retained austenite are free of carbides, which validates the steel design procedure.
Bearing in mind that an in-use property, such as weldability, may be an important issue from the point of view of the final
customer, a parallel set of calculations and adjustments in chemical compositions were performed; in particular, a reduction in the
C equivalent was sought.
Table 2 Quantitative data on microstructure of 0.3BAIN and 0.2BAIN steels. FCT is interrupted accelerated cooling temperature;
Vb is the volume fraction of bainitic ferrite; VM is the volume fraction of martensite; Vg is the volume fraction of austenite
Steel/FCT Vb VM Vg
0.3BAIN 1/450 * C 0.73 ) 0.04 0.24 ) 0.05 0.03 ) 0.01

0.3BAIN 1/600 * C 0.76 ) 0.03 0.21 ) 0.04 0.03 ) 0.01
0.3BAIN 2/500 * C 0.77 ) 0.04 0.13 ) 0.05 0.10 ) 0.01
0.3BAIN 2/550 * C 0.80 ) 0.04 0.09 ) 0.05 0.10 ) 0.01
0.3BAIN 3/500 * C 0.88 ) 0.02 0.02 ) 0.03 0.11 ) 0.01
0.3BAIN 3/550 * C 0.86 ) 0.02 0.03 ) 0.04 0.11 ) 0.01
0.3BAIN 4/500 * C 0.88 ) 0.02 0.09 ) 0.04 0.03 ) 0.01
0.2BAIN 5/500 * C 0.91 ) 0.02 – 0.09 ) 0.01
0.2BAIN 5/550 * C 0.93 ) 0.02 – 0.09 ) 0.01
0.2BAIN 6/500 * C 0.90 ) 0.02 – 0.11 ) 0.01
0.2BAIN 6/550 * C 0.91 ) 0.02 – 0.12 ) 0.01
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Figure 3 SEM and TEM micrographs of some 0.3BAIN steels after air cooling from different temperatures: (a, b) 0.3BAIN 1/600 * C; (c, d) 0.3BAIN
2/* 500 C. After Caballero, F. G.; Santofimia, M. J.; Capdevila, C.; García-Mateo, C.; De García Andrés, C. Design of Advanced Bainitic Steels by Optimisation of
TTT Diagrams and T0 Curves. ISIJ Int. 2006, 46 (10), 1479–1488.
It is necessary to mention that steels with different C content will exhibit the same T00 curve (14,44). The driving force for the
formation of new plates decreases as the C concentration in the untransformed austenite approaches the T00 composition, at which
the free energy of ferrite and austenite phases of the same composition become identical. In addition, C increases the strength of the
parent austenite from which bainite grows, and some approaches have also considered plastic deformation as an additional source
of Gibbs energy dissipation during bainite transformation (45). Besides the independence of the T00 curve from the average C
content of the steel, the maximum volume fraction of bainite formed at a given transformation temperature will increase as the C
content of the steel decreases, since the critical T00 value is reached at a later stage (27,29). Moreover, the bainite region in the TTT
diagram is expected to shift to higher temperatures and shorter times as C content is reduced, as C is a strong austenite stabilizer. As
a result, the 0.2BAIN 5 and 6 steels, shown in Table 1, were designed in order to improve the in-use properties of the former
advanced bainitic steels. This third set of alloys with a C content of 0.2 wt.% also followed a hot rolling schedule in several passes,
and finished at 913 * C for 0.2BAIN 5 and 904 * C for 0.2BAIN 6. The desired bainitic microstructure was obtained in both steels by
air cooling from different temperatures, 500 and 550 * C, shown as FCT in Table 2, after an initial accelerated cool at w50 * C s'1.
Microstructure data of both steels are presented in Table 2. As an example, Figures 4(a) and 4(c) show SEM and Figures 4(b) and
4(d) show TEM micrographs of the microstructure obtained after air cooling from 500 * C in 0.2BAIN steels. Experimental results
reveal that both steels have the desired microstructure, which consists of mainly bainitic ferrite and retained austenite. Martensite
was not present in either microstructure. The high volume fraction of bainitic ferrite in these samples, , 90%, suggests that austenite
will be homogeneously distributed in the form of thin films of austenite along lath boundaries, as SEM and TEM micrographs
confirmed, and as Figure 4 shows.
Finally, the TEM micrographs in Figure 4 confirm that the microstructure in both steels consists of carbide-free upper bainite.
Resultant microstructures of 0.2BAIN steels are similar to those obtained in the second set of alloys with 0.3 wt.% C, as shown in
Figure 3. However, a reasonable decrease of w100 HV in hardness was detected in the bainitic microstructures for 0.2BAIN 5 and 6
steels, due to their lower C content alloys.
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Figure 4 SEM and TEM micrographs of some 0.2BAIN steels after air cooling from different temperatures: (a, b) 0.2BAIN 1/500 * C; (c, d) 0.2BAIN
1/550 * C. After Caballero, F. G.; Santofimia, M. J.; Capdevila, C.; García-Mateo, C.; De García Andrés, C. Design of Advanced Bainitic Steels by Optimisation
of TTT Diagrams and T0 Curves. ISIJ Int. 2006, 46 (10), 1479–1488.
The corresponding mechanical properties for the 0.3BAIN alloys are reported in Table 3. The low yield/ultimate tensile strength
ratios (YS/UTS) are due to the presence of austenite and the generally large dislocation density in the microstructure. Consequently,
retained austenite increases the strain-hardening rate of the steel, and likewise, tensile elongation is controlled by the volume
fraction of retained austenite. Retained austenite is a ductile phase, as compared to the bainitic ferrite, and would be expected to
enhance ductility, provided that the austenite is homogeneously distributed along lath boundaries (film austenite). However,
Table 3 Tensile property results at 20 * C of 0.3BAIN and 0.2BAIN steels. FCT is interrupted accelerated
cooling temperature; YS yield strength; UTS ultimate tensile strength; TE total elongation
Steel/FCT YS, MPa UTS, MPa YS, UTS TE, %
0.3BAIN 1/450 * C 1240 ) 31 1796 ) 21 0.69 18 ) 1

0.3BAIN 1/600 * C 1204 ) 29 1701 ) 9 0.71 16 ) 1
0.3BAIN 2/500 * C 1187 ) 16 1606 ) 30 0.74 17 ) 2
0.3BAIN 2/550 * C 1128 ) 32 1539 ) 21 0.73 16 ) 2
0.3BAIN 3/500 * C 1194 ) 35 1652 ) 6 0.72 18 ) 1
0.3BAIN 3/550 * C 1204 ) 18 1642 ) 12 0.73 18 ) 1
0.3BAIN 4/500 * C 1339 ) 16 1763 ) 18 0.76 16 ) 1
0.2BAIN 5/500 * C 1192 ) 82 1382 ) 31 0.86 24 ) 2
0.2BAIN 5/550 * C 1146 ) 17 1347 ) 8 0.85 25 ) 3
0.2BAIN 6/500 * C 1033 ) 64 1319 ) 12 0.78 23 ) 2
0.2BAIN 6/550 * C 999 ) 54 1306 ) 16 0.76 25 ) 3
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Figure 5 Yield strength and total elongation of advanced bainitic steels, 0.3BAIN and 0.2BAIN families, in comparison with other commercial steels.
After Caballero, F. G.; Santofimia, M. J.; Capdevila, C.; García-Mateo, C.; De García Andrés, C. Design of Advanced Bainitic Steels by Optimisation of
TTT Diagrams and T0 Curves. ISIJ Int. 2006, 46 (10), 1479–1488.
isolated pools of austenite (blocky austenite) would unfavorably influence both elongation and UTS, presumably because of the
strain localization in these areas (27). From the data shown in Table 3, it is clear that the steels present a combination of high
strength and good ductility.
The tensile test results of 0.2BAIN 5 and 6 steels, which are also reported in Table 3, are shown in Figure 5 in comparison with
0.3BAIN 1 to 4 steels, as well as with other commercial steels. The results generally suggest that 0.2BAIN 5 and 6 steels have
considerable potential for automotive application, since they can reach very high tensile strength levels (above 1300 MPa) while
retaining significant ductility. Their total elongations are comparable to those in TRIP steels, which is very impressive for such high
YS and UTS. Regarding the product of UTS " total elongation reached by these steels (higher than 30 000 MPa%), the properties are
higher than the ferritic TRIP steels under developments (typically 22 500 MPa%) (46). In terms of formability assessment, addi-
tional investigations should be performed. However, the present results suggest that the ratio YS/UTS is low and is also comparable
to those obtained in DP steels (polygonal ferrite and martensite as hard phase), which can be beneficial for overall drawability.
1.09.4 A New Steel Concept for the Twenty-First Century: Nanostructured Bainitic Steels (NANOBAIN)
Strengthening grain boundaries causes them to act as pinning points, which impede further dislocation propagation. Since the
lattice structure of adjacent grains differs in orientation, it requires more energy for a particular dislocation to change directions and
move into the adjacent grain. The grain boundary is also much more disordered than inside the grain, which also prevents the
dislocations from moving in a continuous slip plane. Impeding this dislocation movement will hinder the onset of plasticity, and
hence increase the yield strength of the material. In other words, the strength of materials increases as the crystal grain size decreases.
This principle, referred as the Hall–Petch strengthening principle, receives a lot of attention, and it is extensively applied to improve
the overall strength of structural materials.
Grain refinement under severe plastic deformation (SPD) processes, such as equal-channel angular extrusion (ECAP),
accumulative roll bonding (ARB), and high pressure torsion (HPT), although limited in the shape of the final product and in
the quantity that can be produced at reasonable cost, have opened up new ways to produce steels with nanosized grain
structures. Examples include fine nanostructured wire with a strength in excess of 3 GPa where a pearlite wire is cold-drawn to
a high strain of more than 4; the pearlite lamellar spacing is then reduced to a few tens of nanometers (47,48). A similar
concept was used to develop the commercial steel wire known as Scifer, which has an ultimate tensile strength of 5.5 GPa and
yet is very ductile in fracture (49,50). It is obtained by drawing a martensite–ferrite microstructure in the form of 10 mm
diameter rods into strands which individually have a diameter of 8 mm. This amounts to a huge deformation with a true strain
in excess of 9. The dislocation cell size in the material becomes 10–15 nm, which is where much of the strength of Scifer
comes from (50).
Other examples are metals subjected to ECAP in which redundant work is used in order to achieve large plastic strains while
maintaining the external shape of the object being deformed (51,52). ARB involves the repeated rolling and folding of sheet
material in order to accomplish strain increments without thinning the sample entering the rolls; the process is well-suited for large-
scale production, but does not lead to particularly fine grains, which tend to be closer to micrometers than nanometers in size (53).
HPT is a procedure in which a disk-shaped sample with a diameter up to 20 mm and a thickness of about 0.2 mm is put between
two anvils and subjected to a high pressure of 2–7 GPa, while at the same time one of the anvils forces the sample to deform by
torsion. This process leads to a microstructure with grain sizes that are typically about 100 nm (54).
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As mentioned, the main difficulty in using sever deformation to increase strength is that the deformation necessary to accu-
mulate a large number density of defects limits the size and form of the product to that of a single strand in the case of Scifer.
Deformation processes, such as ECAP and ARB, maintain the overall dimensions of the original material, but the range of shapes
that can be achieved is limited (51,53,55,56). In general, there is still a large gap between SPD processes on the laboratory scale
between fundamental research and its application in large-scale production.
Thermomechanical processing is particularly suited for large-scale production of fine-grained steels, where the refinement of the
microstructure is achieved by phase transformation from the deformed parent austenite (57–59). The mechanisms of the micro-
structural refinement are recrystallization of austenite, enhanced nucleation of ferrite from deformed (unrecrystallized) austenite
under large supercooling, and inhibition of grain growth of the obtained ferrite. Microalloying of Ti and/or Nb and precise control
of rolling conditions (temperature, reduction, and pass schedule) have realized a minimum average grain size of 5 mm (59). At
laboratory scale, the minimum grain size achieved was 1 mm (60), which was accomplished by lowering the finished rolling
temperature and achieving a greater one-pass reduction of over 50%.
The natural question that arises from this research is, what is the theoretical minimum grain size achievable by means of this
technology? This question can be answered by noting that the excess energy stored in the form of grain boundaries cannot exceed
the free energy change DGga
V owing to the transformation of the austenite (61). For an equiaxed polycrystalline grain structure, the
grain-boundary surface per unit volume SV is related to the grain size L (mean lineal intercept) by the equation SV ¼ 2=L. Then, the
stored energy per unit volume due to the grain boundaries is
DGV ¼ sSV ¼ 2s=L [2]
where s is the energy per unit area of the boundary. The limiting grain size is obtained by equating this stored energy to the driving
force
( ga (
(DG ( , sa Sa ' sg Sg [3]
V V V
For equiaxed austenite grains, it becomes

( ga ( 2sa 2sg
(DG ( , ' [4]
V
La Lg
It follows that the smallest ferrite grain size can be achieved when all of DGga
V is used up in creating a/a grain boundaries, such
that
min 2sa
La ¼ (( ga (( [5]
DGV þ 2sg =Lg
This relationship would have to be modified when the austenite is pancaked before transformation, and there are other details
such as crystallographic texture that must be taken into account (61).
min
The variation in the limiting ferrite grain size (La ) is shown in Figure 6 as a function of DGga
V , and is calculated using eqn [4]
with sa ¼ 0.6 J m'2; given the absence of data, the 2sg =Lg term in eqn [5] was set to zero. These calculations are presented as the
min
‘ideal’ curve in Figure 6. The curve indicates that at large grain sizes, La is sensitive to DGgaV and therefore to the undercooling
below the equilibrium transformation temperature. However, reductions in grain size in the submicro range require huge values of
DGgaV , meaning that the transformations would have to be suppressed to large undercoolings to achieve a fine grain size.
min
Figure 6 Plot of the logarithm of ferrite grain size vs the free energy change at Ar3. The ideal curve represents the values of La . The points are
experimental data; in some cases it is assumed that the grain size quoted in the literature corresponds to the mean lineal intercept. The curves marked low
min
and high Mn represent calculated values of La , after allowing for recalescence. After Yokota, T.; Garcia-Mateo, C.; Bhadeshia, H. K. D. H. Formation of
Nanostructured Steels by Phase Transformation. Scripta Mater. 2004, 51 (8), 767–770.
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As Figure 6 shows, the points are experimental data; in some cases, it is assumed that the grain size quoted in the literature
min
corresponds to the mean lineal intercept. The curves, marked as low and high Mn, represent calculated values of La after allowing
for recalescence (61). Figure 6 also shows points corresponding to measured ferrite grain sizes from the low and high Mn steels as
min
described in (61); it is evident that La ¼ Lg , except at the lowest undercooling. Despite the large scattering, the data indicate that in
spite of tremendous efforts, the smallest ferrite grain size obtained commercially using thermomechanical processing is stuck
at w1 mm.
The reason for this minimum grain size is recalescence, which is the heating of the sample caused by release of the latent heat of
transformation at a rate so high that it cannot easily be dissipated by diffusion. This rise in temperature owing to recalescence
reduces the effective undercooling, and is therefore the driving force for transformation (61). Figure 6 clearly indicates that the
recalescence-corrected curves show better agreement with the experimental data, indicating that at large undercooling rates, the
achievement of fine grain size is limited by the need to dissipate enthalpy during rapid transformation.
Displacive transformations lead to fine microstructures as a natural consequence of their atomic mechanisms. The martensite
phase exhibits a lath morphology which has been recognized to be heavily dislocated and hierarchically substructured into packets,
blocks, and laths (62,63). The transformation-induced dislocation density of lath martensite has been found in the order of the
heavily deformed metals, with a lath thickness less than a few 100 nanometers (64). Very strong martensitic steels with strength
>3 GPa already exist (65). This kind of martensite is produced in fairly large steel samples by rapid cooling from the austenitic
condition. However, the dimensions of these steels can be limited by the need to achieve a uniform microstructure – a fact implicit
in the original concept of hardenability. Increasing hardenability requires the addition of expensive alloying elements. The rapid
cooling can lead to undesirable residual stresses (66,67), which can ruin critical components and must be factored into component
life assessments.
It would be nice to have a strong material that can be used for making components that are large in all their dimensions and does
not require mechanical processing or rapid cooling to reach its desired properties. To achieve this goal, some facts have to be
considered:
1. The material must not rely on perfection to achieve its properties. Strength can be generated by incorporating a large number
density of defects such as grain boundaries and dislocations, but the defects must not be introduced by deformation if the shape
of the material is not to be limited.
2. Defects can be introduced by phase transformation. But to disperse these defects on a sufficiently fine scale, the phase change
must occur at large undercoolings (large free energy changes).
3. Recalescence limits the undercooling that can be achieved. Therefore, the product phase must have a small latent heat of
formation and grows at a rate which allows the ready dissipation of heat.
Recently, an innovative design procedure based on phase transformation theory (68) was successfully applied to design strong,
tough, and affordable submicron and nanocrystalline steels without using deformation, rapid heat treatment, or mechanical
processing. Furthermore, the material can be produced in a form which is large in all its three dimensions. The new material relies on
a microstructure called bainite, which was discovered in 1930; the novelty is in the alloy design, which leads to the fine scale and
controlled response to heat treatment.
In this section, a general overview on the novel ways and means to produce strong nanostructured bainitic steels is presented.
The excellent combination of mechanical properties is mainly a consequence of the scale of the microstructure.
It is established (36) that the bainitic ferrite plate thickness for this microstructure depends primarily on the strength of the
austenite at the transformation temperature, and the chemical free energy change that accompanies transformation. Thus, strong
austenite and/or a large driving force results in finer plates, the former because there is a large resistance to interface motion and the
latter because an increased nucleation rate leads to microstructural refinement. Both magnitudes (austenite strength and driving
force) increase as the transformation temperature decreases. Is there a lower limit in the temperature at which bainite can be
obtained? According to bainite phase transformation theory, there is no such limit (24,69). Figure 7 shows where theoretical bainite
and martensite start temperatures, BS and MS, were calculated for Fe–2Si–3Mn as a function of the C content.
By applying the same models based on phase transformation theory (68) as those used and described for AHSS-GEN3 bainitic
steels (40–43), a new variant of low temperature, carbide-free bainitic steels has been developed by Bhadeshia and coworkers
(69–72). The new variant of steel grades has a chemical composition (shown in Table 4) that is tailored to have low transformation
temperatures, BS and MS. The alloys contain high amounts of C to ensure good strength and a low transformation temperature
regime, and Mn and Cr in sufficient quantities to provide enough hardenability, which ensures that no other transformations will
interfere with bainite formation. An addition of Mo is made to reduce impurity embrittlement and to increase hardenability. An Si
content of 1.5 wt.% is the minimum required to avoid cementite precipitation during bainite formation. The experimental BS and
MS temperatures are summarized in Table 4, and clearly show that the goal of a low transformation temperature was successfully
achieved. The heat treatment consisted of austenitization followed by isothermal holding between BS and MS. In the steels
designated as NANOBAIN 1 and 2 (shown in Table 4), bainite transformation can take between 2 to some 60 days (see Table 5) to
complete transformation in the temperature range of 352–125 * C (69,70). In a commercial scenario, it may be useful to accelerate
transformation without losing the ability to utilize low temperatures. Certain elements increase the free energy change (see
Figure 8) when austenite transforms and hence should accelerate its decomposition, which explains the Co- and Al-containing
alloys in Table 4 (NANOBAIN 3 and 4). In doing so, the time to finish the bainitic transformation is drastically decreased,
which can be seen by comparing NANOBAIN 3 and 4 with NANOBAIN 1 and 2 in Table 5.
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Figure 7 Calculated transformation temperatures as a function of the carbon concentration.
Table 4 Chemical compositions of NANOBAIN steels, wt.%, and experimental BS and MS temperatures in * C
Steel C Si Mn Cr Mo V Co Al BS MS
NANOBAIN 1 0.78 1.59 1.94 1.33 0.30 0.11 – – 120 325

NANOBAIN 2 (at.%) 0.98 (4.34) 1.46 (2.76) 1.89 (1.82) 1.26 (1.28) 0.26 (0.14) 0.09 (0.09) – – 125 335
NANOBAIN 3 0.83 1.57 1.98 1.02 0.24 – 1.54 – 120 360
NANOBAIN 4 0.78 1.49 1.95 0.97 0.24 – 1.60 0.99 155 380
Table 5 Summary of quantitative experimental data. Vb is the volume fraction of bainitic ferrite, the remainder of the
microstructure being retained austenite. PAGS stands for the prior austenite grain size. T stands for the isothermal
transformation temperature, and t for the stereologically corrected value of the bainitic ferrite plate thickness
Steel (PAGS, mm) T, * C Time, h Vb t, nm
NANOBAIN 1 300 26 0.65 –

250 72 0.84 –
190 216 0.87 –
NANOBAIN 2 (49 ) 2) 300 30 0.55 124 ) 4
250 96 0.63 55 ) 2
200 216 0.70 35 ) 1
NANOBAIN 3 (88 ) 2) 300 5 0.66 106 ) 10
250 11 0.77 38 ) 2
200 120 0.79 38 ) 1
NANOBAIN 4 (44 ) 2) 300 4 0.66 57 ) 4
250 8 0.77 45 ) 3
200 72 0.78 40 ) 4
In all the alloys, the microstructure thus obtained is composed of a mixture of bainitic ferrite (up to 87%) and retained austenite.
The amount of bainitic ferrite increases as transformation temperature decreases, which is a direct consequence of the negative slope
of the T00 curve.
Figure 9 illustrates the typical low-temperature bainite microstructure at different magnification. The lighter phases in
Figures 9(a) and 9(b) are microblocks of retained austenite (>1000 nm), whereas the darker featherlike features are sheaves
of bainite, which are groups of bainitic ferrite plates that share a common crystallographic orientation and are separated by
thin films of retained austenite. Only at much higher magnification, shown in Figures 9(c) and 9(d), it is possible to resolve
the bainite sheaves, which are composed of ferrite subunits also called plates (lower profile phase). It is possible to observe
the presence of retained austenite between the bainite sheaves as submicron blocks (100–1000 nm) and nanofilms (<100 nm)
(the higher profile phases). It is at much higher magnifications, as in Figures 9(e) and 9(f), where the real scale of the
microstructure is appreciated. Observe the incredibly thin and long slender plates of bainitic ferrite (lighter phase) in an
intimate mixture with even thinner nanofilms of retained austenite (darker phase). It is well established (27) that bainitic
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Figure 8 Effect of addition of Co (NANOBAIN 3) and Co þ Al (NANOBAIN 4) on the free energy change DGga.
microstructures formed at low temperatures contain retained austenite, mainly with a submicron and nanofilm morphology.
This is one consequence of the higher bainitic ferrite fraction that is reached at low transformation temperatures. Quite
remarkably, the plates formed at the lowest transformation temperature, 200 * C, in all the grades of steel have a width that is
less than 40 nm (see Table 5) with each plate separated by an even finer film of retained austenite. Increasing the trans-
formation temperature to 300 * C leads to an increase of the plate thickness, up to 124 nm in NANOBAIN 2 (see Table 5).
Also, in Figures 9(e) and 9(f), dislocation debris becomes evident in both the bainitic ferrite and the surrounding austenite.
Extensive transmission microscopy failed to reveal carbides in the microstructure; only a few minute cementite particles were
observed in the ferrite (20 nm wide and 175 nm long) within a sample of NANOBAIN 1 that was transformed at 190 * C for
two weeks (71).
This fine scale is responsible for much of the mechanical properties of the microstructure, with hardness values in excess of
600 HV and strength up to 2.5 GPa (70,72) with reasonable ductility, TE < 30%, and good fracture toughness, KIC < 50 MPa m1/2.
The dispersion of films of austenite undoubtedly helps render the steel tough.
As previously mentioned, analysis indicates that the largest effects on plate thickness are the strength of the austenite and the free
energy change accompanying transformation, and a small independent effect is also present due to the transformation temperature
(36). In the present case, the observed refinement is mainly a consequence of high C content and a low transformation temperature
that enhances the strength of the austenite.
Further and more detailed microstructural characterization will be presented later in this chapter.
1.09.5 Accelerating Low-Temperature Bainite Transformation
From the point of view of large components, a slow transformation has the advantage of allowing transformation to a uniform
microstructure that is free from residual stresses or complex processing. But if a commercial scenario needs faster heat treatments,
there are some approaches that can be applied. First, the transformation can be accelerated by making controlled additions of
substitutional solutes to the steel, so the free energy change as austenite changes into ferrite is enhanced, as previously mentioned.
There are essentially two choices, Al and Co, in concentrations less than 2 wt.%, that have been shown to accelerate the trans-
formation in the manner described (73). See Table 5 and Figure 8 for examples of this. Both are effective, either on their own or in
combination. As bainite nucleates in austenite grain boundaries, a further rate increment is possible by increasing the possible
potent nucleation sites, i.e., refining the prior austenite grain size (PAGS). Table 6 gathers the results of transformation kinetics
when the PAGS for NANOBAIN 3 and 4 is reduced when compared with those in Table 5, which correspond to a larger PAGS. It is
possible to surmise that an increase in the number density of austenite grain surface nucleation sites due to grain refinement would
lead to a substantial acceleration of bainite transformation. There is also a reduction of the bainitic ferrite plate, t, presumably
because of the presence of a greater number of nucleation sites. Consistent with the increased driving force in the Co and Al alloyed
steels, the total volume fraction of bainite obtained following prolonged holding at any given temperature has increased, as shown
in Tables 5 and 6.
Another way of increasing the number density of nucleation sites might be by starting bainitic transformation from
a deformed austenite in a pancake structure. Additionally, generated defects, such as dislocations and shear bands, may act as
nucleation sites. The problem is that in displacive transformations such as bainite, the overall transformation might be slowed
and even stopped by a phenomenon known as mechanical stabilization (74). An alternative, as studied by Haze et al. (75), is to
work in the elastic regime, which is present below the yield strength of the parent austenite. As a result, it has been demonstrated
that a compressive uniaxial stress increases the bainite start temperature and accelerates the transformation. The observed effects
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Figure 9 Micrographs of the resolved microstructure in NANOBAIN 2 after isothermal transformation at (a, c, e) 200 * C and (b, d, f) 250 * C.
are most pronounced at higher transformation temperatures, where the mechanical component of the driving force is relatively
large.
Another category of solutions consists of modifications to heat treatment. Various two-step heat treatments have been inves-
tigated by several authors (76–78), including partial prequenching followed by isothermal transformation to bainite. However,
these results are not conclusive and are even sometimes contradictory. Hasan et al. (79) recently tried a temperature-cycling heat
treatment that produced no conclusive results, as compared with standard isothermal heat treatment.
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Table 6 Summary of quantitative experimental data. Vb is the volume fraction of bainitic ferrite, the remainder of the
microstructure being retained austenite. PAGS stands for the prior austenite grain size. T stands for the isothermal
transformation temperature, and t for the stereologically corrected value of the bainitic ferrite plate thickness
Steel (PAGS, mm) T, * C Time, h Vb t, nm
NANOBAIN 3 (29 ) 2) 300 10 0.75 64

250 14 0.79 49
200 72 0.87 30
NANOBAIN 4 (28 ) 2) 300 8 0.63 52
250 10 0.79 41
200 72 0.83 45
1.09.6 Advanced Characterization of Nanostructured Steels
The multiphase character of the bainitic microstructure (bainitic ferrite, retained austenite, and, in some cases, martensite), together
with its unique microstructural and morphological peculiarities, is a true challenge from the characterization point of view, as well
as a direct consequence of the complexity of bainite formation mechanism and kinetics. The levels of complexity increase as the
microstructure moves toward the nanoscale, as in the case of the NANOBAIN steels.
Soon after the diffusionless growth of a bainitic ferrite subunit is over, the excess of C is partitioned to the surrounded austenite.
If cementite precipitation from austenite is hindered by the addition of Si, the C that is partitioned into the residual austenite after
bainitic transformation does not precipitate, but remains there to make the austenite stable at ambient temperature (27–29). As it
has been shown, the microstructure obtained through this process consists of fine plates of bainitic ferrite separated by C-enriched
regions of austenite. The characterization of such enrichment is interesting not only in order to probe the described mechanism, but
also to explain some important issues such as the mechanical stability of austenite, temper resistance, and strength.
Quantitative XRD is a fast and relatively easy approach to this measurement that provides additional information about the
fraction and microstrain of ferrite and austenite. In order to obtain accurate information from the XRD analysis, a careful and
methodical sample preparation and experimental setting are needed, with further details of these scenarios in Refs. (80,81). The
austenite C content can be estimated by using Dyson and Holmes’ equation (82), and for ferrite, that proposed by Bhadeshia et al.
(83). Both relate austenite and ferrite lattice parameters to the composition of the steel. Although these expressions have been
validated in several works (69,81,84), additional considerations should take into account the effects of substitutional elements. The
bainite transformation in steels is a displacement reaction, in which the ferrite is initially supersaturated, with respect to C. In the
absence of carbide precipitation, prevented in the present alloys by the use of Si, the excess of C in the bainitic ferrite is subsequently
rapidly partitioned into the residual austenite, but substitutional elements do not partition during the bainite reaction (85); in other
words, (xFe/xj)bulk ¼ (xFe/xj)g ¼ (xFe/xj)a, where j denotes any substitutional element in the alloy, and xFe and xj are the concentra-
tions of Fe and of the substitutional elements, respectively. For austenite, this condition is introduced in Dyson and Holmes’
P
equation, in conjunction with the fact that ðxi Þg ¼ 100; i denotes all elements in the chemical composition, giving rise to a system
in which the austenite’s C content is accurately calculated by an iteration process. The analysis is equivalent for ferrite, but uses its
corresponding expressions. Experimental results thus obtained are presented in Figure 10, which correspond to the fully bainitic
microstructure that is obtained after different isothermal heat treatments in NANOBAIN 2. The measured C concentrations in
austenite lie closer to the T00 value boundary and far from the paraequilibrium phase boundary, and are consistent with the
mechanisms described. Results also indicate that the C concentration in the bainitic ferrite was much higher than that expected from
paraequilibrium thermodynamics between austenite and ferrite. This supersaturation was attributed to the trapping of C at the
dislocations in the bainitic ferrite.
The dislocation structure of bainite is often attributed to the shear transformation mechanism. However, such a mechanism
would not lead to dislocations in the ferrite if the shape deformation were elastically accommodated. Thermoelastic equilibrium in
martensite and shape memory alloys depends on the elastic accommodation of the shape deformation, and the movement of any
interfaces must occur without the creation of defects (86). It is only if the shape deformation is accompanied by plastic relaxation
that the dislocations associated with this plastic strain are inherited by the product phase.
The average dislocation density in ferrite and austenite of these novel microstructures was determined by TEM performed on
NANOBAIN 2 steel transformed at 300 * C to be (0.51 ) 0.27) " 1015 m'2 and (0.18 ) 0.02) " 1015 m'2, respectively (35). These
values are above those reported for conventional bainite, 1.7–4.0 " 1014 m'2 (87), and, in general terms, they are similar to those
measured for martensitic microstructures (64). A progressive increase in the dislocation density in ferrite was also observed as the
austenite–ferrite interface was approached (35). This increase is related to the plastic deformation that occurs in the surrounding
austenite to accommodate the transformation strain as growth progresses, as well as the following inheritance of those dislocations
by the expansion of the growing bainitic ferrite plate. By means of other techniques, such as XRD profile broadening analysis and
high-resolution dilatometry, similar levels of dislocation density were obtained in NANOBAIN 3 and 4 (73), and also in a variation
of NANOBAIN 3 with higher Co content (88). Figure 11 gathers these and other results, where the solid line represents the results of
an empirical model (34) to determine the dislocation density as a function of transformation temperature in displacive trans-
formations, i.e., bainite (B) and martensite (M). As expected, these results show a tendency to increase the dislocation density from
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Figure 10 A comparison of experimental data against calculated T00 and A03 phase boundaries. The larger points on the left are the measured mole
fractions of carbon in bainitic ferrite, and the smaller points on the right represent the carbon concentrations of austenite. The dashed vertical line
represents the average mol fraction of carbon in the alloy NANOBAIN 2.
Figure 11 Calculated dislocation density and also by means of X-ray peak broadening analysis; B stands for bainitic microstructure. Also included values
reported by other authors for martensitic (M) and bainitic microstructures. Reference (35) refers to an empirical model to determine the dislocation
density as a function of transformation temperature in displacive transformations, i.e., bainite and martensite. After Garcia-Mateo, C.; Caballero, F. G.;
Capdevila, C.; de Andres, C. G. Estimation of Dislocation Density in Bainitic Microstructures Using High-Resolution Dilatometry. Scripta Mater. 2009, 61
(9), 855–858.
3.77 ) 2.05 " 1014 m'2 to 4.20 ) 1.90 " 1015 m'2 as the transformation temperature decreases from 375 to 250 * C, and in all cases
they are well above those reported for allotriomorphic ferrite, 3.7–5.0 " 1013 m'2 (87,89). The results are in good agreement with
those measured by other authors for bainitic and martensitic microstructures (34,64, 90).
The trapping of C on these dislocations, i.e., Cottrell atmospheres, has never been observed before in bainitic steels until atom
probe tomography (APT) was used to characterize bainitic microstructures formed at 200 and 300 * C in NANOBAIN 2 steel at the
atomic scale. The large field of view and rapid analysis capability of this technique facilitated the analysis of dislocations in these
materials.
A C atom map obtained from NANOBAIN 2 after 10 days at 200 * C is shown in Figure 12(a) (20). Carbon distribution is not
uniform in the analyzed volume, and both carbon-rich and carbon-depleted regions are clearly distinguishable. This volume
encompasses a central C-enriched (10.4 ) 0.6 at.% C) austenite film bounded by two bainitic ferrite plates (<1 at.% C) and
dislocation tangles in the vicinity of a ferrite–austenite interface at the bottom of the volume and a C-enriched cluster at the top of
the volume. It is evident from the proximity histograms across the dislocations in bainitic ferrite, shown in Figure 12(d), that
dislocations only trap the C atoms, as originally suggested by Kalish and Cohen (91). The lateral extent of the Cottrell atmosphere in
the vicinity of a dislocation was estimated to be z 5 nm. The average C level of the Cottrell atmosphere in this example was
estimated to be 13.4 ) 0.8 at.% C. Carbon trapping at crystal defects prevents the decarburization of supersaturated bainitic ferrite,
and therefore alters the carbide precipitation sequence during low-temperature bainite formation (85). Finally, the proximity
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Figure 12 (a) Carbon isoconcentration surfaces at 8 at.% C superimposed with the carbon atom map, and proximity histograms across
(b) a carbon cluster, (c) a ferrite–austenite interface, and (d) a dislocation network in the vicinity of the ferrite–austenite interface in bainitic
ferrite after NANOBAIN 2 transformation at 200 * C for 10 days. After Caballero, F. G.; Miller, M. K.; Garcia-Mateo, C. Carbon Supersaturation
of Ferrite in a Nanocrystalline Bainitic Steel. Acta Mater. 2010, 58 (7), 2338–2343.
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histogram across the z3 nm thick cluster, shown in Figure 12(b), shows a maximum C content of z15 at.%, higher than that
associated with dislocations, but with Cr and Mn contents too low (less than 2 at.%) to be identified as a carbide. In addition, Si
does not change at all through the interface, indicating that the concentration of Si is uniform throughout both phases. These
features resemble those C clusters with a modulated structure consisting of alternating carbon-rich and carbon-poor bands reported
for Fe–Ni–C martensite after natural aging (92,93).
It has been also demonstrated that the austenite adjacent to the bainitic ferrite undergoes twinning deformation, and that the
density of such twins increases as the transformation temperature decreases (21,94). Accommodation twinning is apparent in TEM
micrographs of NANOBAIN 2 steel transformed at 200 * C for 10 days, as shown in Figure 13. The bright field image in Figure 13(b)
illustrates the austenite in contact with a bainitic ferrite plate exhibiting extensive twinning, apart from dislocation debris associated
with the austenite–ferrite interface. These twins are lenticular in shape with a thickness of approximately 2–10 nm. The corre-
sponding diffraction pattern of Figure 13(c) confirms that the bainitic ferrite obeys the Kurdjumov–Sachs orientation relationship
with the austenite and inheriting twins. It is known that impurities such as phosphorus, Ca, and Si can segregate on incoherent twin
boundaries with high free volume (95,96). A concentration profile by APT in (21) showed fine-scale modulation in the C atom map
of a NANOBAIN 2 sample transformed at 200 * C for 2 days. These carbon-enriched planes, whose thickness compares well with that
of the twins illustrated in Figure 13(b), were identified as twin boundaries in retained austenite. Their average C content was
estimated to be 9.6 ) 0.8 at.%. The formation of nanoscale twins requires a significant amount of C in austenite, together with large
shape strains. These requirements and the observed crystallographic features are consistent with a displacive transformation
mechanism for bainite (12).
It is believed that solute segregation on defects, such as those presented in Figure 12(d), play an important role in C redistri-
bution during bainite transformation. Dislocations associated with plastic relaxation in austenite are inherited by any bainite that
subsequently forms, and segregation at dislocations is expected to bind and thus prevent or hinder the C atoms from diffusing out of
the ferrite lattice. This explains the high level of C that exists in the bainitic ferrite after transformation and the small extent of C
enrichment that is detected in the residual austenite. Moreover, the increase in the amount of C in bainitic ferrite as the trans-
formation temperature decreases is consistent with the fact that the dislocation density of bainitic ferrite is higher, the lower the
reaction temperature is (90).
Figures 12(a) and 12(c) both show an example of an austenite–ferrite interface in NANOBAIN 2 after transformation at 200 * C
for 10 days. Results confirm, as XRD did in Figure 10, the small extent of C enrichment in the residual austenite, as compared to
nominal C concentration of the steel, 4.34 at.%, and the high level of C in bainitic ferrite, well beyond that expected from para-
equilibrium with austenite (w0.12 at.% C).
It is also clear from the APT data in Figure 12(c) that there is no significant segregation of either substitutional elements or C to
the austenite–ferrite interface. Consistently with previous work (22), quantitative data confirm the absence of any partitioning of the
substitutional elements between the phases involved. The results are fully consistent with the diffusionless transformation of
austenite to bainite (14). The absence of any significant C buildup at the interface indicates that the interface must be semicoherent,
with a high degree of coherency, consistent with the shape change effect mentioned earlier. Thus, the interface may not provide
a very large sink for C atoms.
It has been shown that XRD measurements of a residual austenite lattice parameter, ag, are used for an overall determination of C
content in austenite. However, a limitation to this technique is that it provides an average value of the C content over the volume
analyzed; therefore, this method is not useful for the local and discrete measurements that are required for detecting variations of C
content between films or blocks of austenite. The technique of APT has been used to provide additional and new evidence of the
heterogeneous distribution of C in austenite, a fundamental issue that controls ductility in this type of microstructure (80,97). The
Figure 13 Transmission electron micrographs of NANOBAIN 2 steel transformed at 200 * C for 10 days: (a) General microstructure; (b) nanoscale
twins in retained austenite; and (c) corresponding diffraction pattern. a is bainitic ferrite and g is austenite. After Caballero, F. G.; Yen, H. W.; Miller, M. K.;
Yang, J. R.; Cornide, J.; Garcia-Mateo, C. Complementary Use of Transmission Electron Microscopy and Atom Probe Tomography for the Examination of
Plastic Accommodation in Nanocrystalline Bainitic Steels. Acta Mater. 2011, 59 (15), 6117–6123.
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study was performed at different stages of the bainitic transformation at 200 * C of the NANOBAIN 2 alloy. Table 7 shows
a comparison of the C content of retained austenite measured by APT. Keep in mind that TEM examination of samples tempered at
400 * C revealed that this higher temperature treatment did not introduce any appreciable change in the microstructure (19,84). APT
allowed not only the determination of the C content within nanosized retained austenite films, but also an estimation of their size.
However, this size might be higher than the estimated value, since the full extent of the coarse features was not observed in the
limited volume of analysis, as noted in Table 7 with an asterisk. This is related to the fact that coarse features observed in SEM, such
as blocky austenite, are not readily observed in randomly located APT samples. Therefore, to some extent, the APT data presented
here are biased in terms of the population of the austenite sizes measured. Keeping this in mind, it seems evident that the amount of
C detected in thin films of similar size (5–6 nm) increases as the bainitic ferrite transformation progresses, increasing from 5.3 to
14.4 at.% in Table 7, a result that is consistent with the progressive C enrichment of austenite as more bainitic ferrite forms and
rejects part of the excess of C into it. Results shown in Table 7 indicate that the two essential morphologies of austenite in Si-rich
bainitic steels, namely thin films and blocks, also contain different quantities of C in solid solution. This result is in agreement with
previous experiments that used convergent beam Kikuchi line diffraction pattern (CBKLDP) on upper bainite of Zhang and Kelly
(98), or by fringe spacing measurements on carbide-free bainite by Self et al. (99), and the synchrotron XRD study by Stone et al.
(100) performed on nanoscale bainitic steels.
The APT results clearly indicate that in certain austenite regions, the measured C concentration exceeds the T00 concentration,
7.0 at. %. This is a consequence of the fact that the austenite films that are trapped between neighboring subunits of bainitic
ferrite have a higher C content than the blocks of residual austenite located between the sheaves of bainite (14). Although such
austenite can no longer transform to bainite, it can continue to accumulate C from suitable sources. Such circumstances arise
naturally during the bainite reaction when a region of austenite that has been affected by the dumping of C from an extant bainite
Table 7 For NANOBAIN 2, carbon content in austenite obtained by XRD and APT. Also reported is the thickness
of the austenite regions analyzed by APT
Heat treatment at 200 * C APT, at.% Thickness of g measured in APT, nm
48 h 5.30 ) 2.84 6
96 h 7.25 ) 3.77 5
240 h 4.79 ) 3.02a 13
7.39 ) 1.31 30
5.39 ) 0.18 50c
5.14 ) 3.05 8
14.4 ) 2.80 5
6.00 ) 0.20 300c
9.00 ) 0.50 20
10.21 ) 1.72 18
11.00 ) 1.78 8
12.10 ) 1.79 11
9.01 ) 0.79 20
4.77 ) 0.24 550c
(8.26 ) 3.20)b
240 h þ temper at 400 * C for 30 min 6.12 ) 0.77 110
7.32 ) 2.55 50
9.47 ) 0.41 25
10.02 ) 0.43 20
5.74 ) 0.55 250c
11.27 ) 0.79 20
8.42 ) 0.47 20
8.40 ) 0.42 60
7.26 ) 0.65 80
8.45 ) 0.57 50
7.27 ) 0.38 32
(8.16 ) 1.65)
240 h þ temper at 450 * C for 30 min 3.75 ) 0.95 8
4.19 ) 1.26 35
3.72 ) 0.73 15
(3.89 ) 0.26)
a
Error bars representing the statistical scatter in the APT composition profiles or proxigrams.
b
Values in brackets are mean values of the APT measurements listed inside the same cell. Their corresponding error bars are standard
deviations of the mean value representing the dispersion of a collection of APT measurements.
c
The real thickness might be higher than the represented value since the full extent of the coarse feature was not observed in the
volume analyzed.
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Figure 14 For NANOBAIN 2, examples of carbon atom maps and corresponding concentration profiles across austenite–ferrite interfaces for nanoscale
films of austenite and submicron blocky austenite, after transformation at 200* C. a is bainitic ferrite and g is austenite. After Caballero, F.; Miller, M.;
Clarke, A.; Garcia-Mateo, C. Examination of Carbon Partitioning into Austenite During Tempering of Bainite. Scripta Mater. 2010, 63 (4), 442–445.
plate becomes isolated by the formation of new supersaturated bainite plates in close proximity. The subsequent partitioning of
C from these initially supersaturated bounding plates can raise the C content of the entrapped austenite film to any level within
the range between the T00 value (7.0 at.%) and the Ae03 value (20.7 at.%), calculated at 200* C for the NANOBAIN 2 chemical
composition.
Finally, nanoscale austenite films with thickness in the range of 5–50 nm show APT C content values ranging from 4.79 to
14 at.%, with an average value of 7.41 ) 3.2 at.%, which is slightly higher than the corresponding T00 (7.0 at.%) values and less than
the paraequilibrium Ae03 value (20.7 at.%). Conversely, austenite nanofilms with a thickness greater than 50 nm or with submicron
blocky austenite regions exhibit APT C content ranging from 4.77 to 6 at.%, with an average value of 5.4 ) 0.6 at.%, which is lower
than the corresponding T00 (7.0 at.%) values. Examples of both nano and submicron austenite are illustrated in Figure 14, where
only a portion of a block of austenite was detected in the analysis volume (97).
1.09.7 Understanding the Mechanical Properties of Advanced Bainitic Steels
A carbide-free bainitic steel can be produced using very simple heat treatments on equally simple steel chemical compositions after
proper and careful design, based on the bainite transformation theory. Further analysis of the microstructure has revealed a plethora
of unique microstructural and morphological peculiarities, which are direct consequences of the atomic mechanisms that rule
bainitic transformation. As expected, the degree of complexity in understanding and characterizing microstructures increases as the
nanoscale is approached. For example, in the case of retained austenite, austenite can be found as a block between the bainite
sheaves and as thin films between the subunits of bainitic ferrite. Being a displacive transformation, there is a certain dislocation
density associated with these transformations, which increases as transformation temperature decreases, and under some condi-
tions, such dislocations may be trapped. There is also the heterogeneous distribution of C in retained austenite, plate thickness, and
other factors to consider.
The relation between the mechanical properties and the different microstructural characteristics can be as complex as the bainitic
microstructure itself. Therefore, trying to correlate the mechanical properties of bainitic microstructures with those microstructural
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features might turn into a difficult task with more than one possible solution, but on the other hand, it is absolutely necessary to
understand the mechanisms that govern these properties and to keep improving the design process of such grades.
This subject is the aim of ongoing research, and some of the results and principles presented have been obtained and validated
for submicron bainite. The transfer of knowledge from the microscale to the nanoscale is not always obvious. This section intends to
present some of those relationships for toughness, strength, and ductility properties.
1.09.7.1 Strength
Figure 15 represents the engineering stress versus strain curves in NANOBAIN 3 for the microstructures obtained after trans-
formation at the indicated temperatures. Deformation of bainitic microstructures at room temperature is characterized by
continuous yielding, as might be expected from microstructures with unlocked dislocations that are introduced by the plastic
accommodation of the shape change. Although there is evidence that ferrite retains an excess concentration of C even after
annealing, the majority of dislocations are believed to be mobile. There are a variety of obstacles to dislocation motion (such as
solute atoms, boundaries, or thin films of retained austenite), each with a different ability to obstruct plastic deformation. As many
of the obstacles are not uniformly distributed, dislocations can penetrate into obstacle-free areas at low stresses, giving rise to
a gradual deviation from elastic deformation. Another scale of heterogeneity can arise when a representative fraction of the softer
phase is included in the microstructure, such as blocks of retained austenite. Plastic deformation at first focuses on the softer phase,
and the hard phase only begins to deform when the softer phase has strain hardened sufficiently to transfer load, which leads to
a continuous yielding.
It is well established (23,73) that the main operative strengthening mechanisms that contribute to the strength of carbide-free
bainitic steels are plate thickness, dislocation density, and excess C in solid solution. In relation to the microstructure-sized
contribution to strength, the well-known Hall–Petch relation, s a (L)'1/2, applies to coarse-grained microstructures, since it relies on
the existence of sufficient space on a slip plane to build a pileup of dislocations. On the other hand, bainitic ferrite grows in the form
of very fine plates. The mean free path through these plates is only about twice the thickness of the plate, and plate thickness is
typically in the submicrometer range. As a result, dislocation pileups cannot form and the Hall–Petch relation ceases to apply in
these situations. Instead, yielding involves the spread of dislocations present in the plate boundaries between pinning points, until
the resulting loop hits the perimeter of the plate. When the energetics of this process are considered (101,102), the grain size
strengthening becomes s z 115 (L)'1, where L ¼ pt/2 is the mean lineal intercept of the ferrite plate measured in a direction
normal to the plate length and t is the plate thickness (103). The contribution arising from the dislocation density introduced during
displacive growth is given by sr ¼ 7.34 " 10'6 r0.5 (104), where r is in m'2. The strengthening due to C in solid solution varies with
the square root of concentration (105), whereas for the substitutional solutes, there is a direct relationship (106). As APT results are
probed in NANOBAIN, the high-dislocation density introduced into the microstructure is also responsible for trapping C as Cottrell
atmospheres (85). Therefore, there may be no independent contribution of C in solid solution, but rather through its effect on the
mobility of dislocations.
Table 8 contains a summary of the mechanical properties, measured at room temperature, that were obtained for NANOBAIN 3
and 4. Bainitic microstructures obtained by transformation at such low temperatures have reached an extraordinary combination of
properties, with YS greater than 1.2 GPa and UTS ranging from 1.7 to 2.3 GPa, the latter in the case of the 200 * C microstructure.
Calculations have revealed that the biggest contribution to strength is due to the size of ferrite plates. Thus, in those microstructures
Figure 15 Engineering stress–strain curves at room temperature of microstructures obtained following transformation at the temperatures indicated.
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Table 8 Mechanical property characterization data. T stands for the isothermal transformation
temperature, and TE for the total elongation achieved during tensile tests
T, * C YS, GPa UTS, GPa TE, % KIC, MPa m1/2 YS, UTS
NANOBAIN 3 200 1.4 2.2 4.6 27.5 0.6

250 1.5 2.1 19.0 37.5 0.7
300 1.2 1.8 29.0 44.0 0.7
NANOBAIN 4 200 1.4 2.3 7.6 27.8 0.6
250 1.4 1.9 9.4 31.7 0.7
300 1.2 1.7 27.5 51.5 0.7
obtained by transformation at 200 * C, with >70% of the finest bainitic ferrite (see Table 6), the plate thickness contribution to
strength is about 1.6 and 1.1 GPa for NANOBAIN 3 and 4, respectively. On the other hand, sr due to dislocations is about 500 MPa
for both alloys. Those contributions are weakened as ferrite plates become coarser, less dislocated, and less profuse, i.e., as the
transformation temperature is increased (see Table 6). Thus for the 300* C microstructures, the plate thickness contribution is only
about 700 MPa and is between 200 and 300 MPa from the dislocation density.
So far, all the strength contributions analyzed correspond to ferrite, which is the strongest, dominant phase. As a result, it is
difficult to assess the retained austenite contribution to strength in these steels. Qualitatively, austenite can affect strength by
transforming to martensite during testing through the TRIP effect. The low YS/UTS ratios shown in Table 8 are due to the presence of
austenite and the large dislocation density in the microstructure, which is introduced during displacive growth (107). Consequently,
retained austenite increases the strain-hardening rate of the steel.
1.09.7.2 Ductility
Similarly, it can be considered that ductility is controlled by the volume fraction of retained austenite (94), which is also capable of
enhancing ductility through its ability to transform to martensite via the TRIP effect. The transformation implies a relaxation of the
local stress concentration and extrastrain hardening by means of two sources: (1) a progressive increase in the volume fraction of
a hard phase, and (2) additional plastic deformation, due to transformation strains. In order to take full advantage of this effect, the
mechanical stability of austenite (i.e., its ability to transform to martensite under strain) must be moderate. In alloys that contain
austenite of low mechanical stability, the strain-induced transformation occurs in early stages of deformation, resulting in little or
no benefit of the strain hardening that is related to deterring plastic instability or necking in the later stages of deformation. On the
other hand, if austenite becomes mechanically more stable and transforms at higher strains, the associated strain hardening
effectively increases resistance to necking and fracture. However, if austenite is too stable, the presence of large amounts of austenite
at necking (an instability criterion) does not guarantee the presence of an effective TRIP effect. The strain-induced transformation
will enhance ductility if retained austenite is moderately stable against straining. It is well established that the strain-induced
transformation of austenite to martensite takes place between the MS and the Md temperature, a point above which the
austenite becomes completely stable (108,109). Therefore, there is a temperature between MS and Md at which the strain-induced
transformation is moderately suppressed and the resulting strain hardening is held in a large strain range, leading to the maximum
benefit of the TRIP effect. In other words, if Md >> TTEST, strain hardening is consumed at early stages of deformation, and there is
no ductility enhancement; on the other hand, if Md << TTEST, this means that the austenite is far too stable and may transform close
to fracture strain or not transform at all. Therefore, the test temperature also influences the mechanical stability of retained austenite.
The evolution of the fraction of austenite that transforms to martensite by the TRIP effect can be calculated with the Sherif
equation (108), ln Vg0 ' ln Vg ¼ k1 εDGa g , where Vg0 and Vg represent the initial austenite fraction and the remaining fraction after
0
TRIP, respectively. Therefore, Md corresponds to the temperature at which Vg0 ¼ Vg ; k1 is a constant, ε is the plastic strain, and DGa g
0
represents the chemical free energy change for the transformation of austenite to ferrite of the same chemical composition.
Therefore, the model takes retained austenite chemical composition and the test temperature into account. These calculations are
presented in Figures 16(a) and 16(b), where the evolution of the retained austenite fraction that transforms to martensite by the
TRIP effect for NANOBAIN 4 is presented. It is obvious that a high Md temperature leads to less stable austenite (a fast trans-
formation), and reduces the potential beneficial effect that strain-induced transformation may have on ductility. Figure 16(b)
clearly states that an increase in the test temperature leads to a more stable austenite, decreasing its rate of decomposition to
martensite.
As austenite to martensite transformation involves the coordinated movement of atoms, the motion of glissile interfaces
becomes impossible when the defect density is high enough, meaning that dislocations present in the microstructure may
mechanically stabilize austenite retarding or even impede martensitic transformation. As the dislocation density due to the dif-
fusionless growth of bainite increases as the transformation decreases, this feature must be considered when dealing with
NANOBAIN microstructures.
The amount of retained austenite is an important factor to be considered that affects the efficiency of the TRIP effect in enhancing
the final ductility of bainitic microstructures. It seems that the formation of strain-induced martensite, which is vital to reach
acceptable ductility properties, can only be tolerated if the austenite maintains a uniform and percolated structure through the
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Figure 16 For NANOBAIN 4, (a) Transformed fraction of austenite vs plastic strain; calculation for the bainitic microstructures developed at isothermal
temperatures of 200, 250, and 300 * C, and (b) effect of the test temperature on the transformed fraction of austenite.
material (110,111). A prominent feature in both works is that in all the studied instances, fracture of carbide-free bainitic tensile
specimens occurs when retained austenite content is reduced to about 10%. These results are consistent with the percolation
threshold theoretically calculated in (110).
Heterogeneities in the microstructure that lead to effective variations of the austenite stability are favorable for spreading the
effect of the transformation all along straining and for postponing localization. There is thus a possibility for microstructural
engineering to attempt to control the sources of heterogeneities (112). In this sense, Hase (76) demonstrated that a bimodal size
distribution of retained austenite (i.e., different stabilities), achieved through a two-step isothermal heat treatment, led to
a remarkable increase of ductility even though the volume fraction of such a phase was smaller.
Finally, the strength mismatch between the different phases (bainite, austenite, and martensite) may play an important factor in
controlling the stability of retained austenite (112,113). In other words, the matrix is playing an important role in the stability and
efficiency of the TRIP effect.
The incremental work hardening exponent n is defined as n ¼ d(ln s)/d(ln εp), where s ¼ k εnp represents the flow curve in the
region of uniform true plastic deformation and k is the strength coefficient. Figure 17 represents the evolution of the incremental
work hardening exponent, n, in two nano-bainitic microstructures, which were obtained by isothermal transformation at 220 and
250 * C in a new variant of NANOBAIN steels. The straight line corresponds to the instability criterion εp ¼ n. In the case of the
220 * C microstructure, there is a continuous increase toward the instability criteria that is never reached, explaining the fact that all
the elongation is uniform. In the case of the 250 * C microstructure, the exhibited behavior is remarkable; after the initial rapid
increase, there is a decrease of up to 2.5% true plastic strain, and then there is a clear increase in the hardening that leads to high
values of uniform elongation (11.6%) and even higher fracture elongation (21.3%).
The observed differences in the ductility and retained austenite mechanical stability cannot be rationalized in terms of a single
contribution like the ones just described, but rather a combination of some of them, which is a consequence of the composite
character of the microstructure formed by a hard phase (bainitic ferrite) and a soft phase (austenite) with a complex, interconnected
deformation behavior.
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Figure 17 For a NANOBAIN steel, curves of the incremental work hardening exponent, n, of bainitic microstructures obtained by transformation at
different temperatures (220 and 250 * C) and tested at room temperature. The straight line represents the instability criterion.
1.09.7.3 Toughness
In order to enhance the toughness behavior of bainitic microstructure, a reduction of the effective grain size, together with the
absence of hard brittle phases as cementite and high C martensite, is the most effective way to avoid toughness degradation. As for
the latter, the mechanical stability of retained austenite present at the microstructure should be considered, because during the
deformation processes, unstable austenite may transform to martensite, leading to a decrease in toughness. As already mentioned,
austenite morphologies, both blocky and thin films, have very different stabilities, in accordance with the constraints exerted by the
surrounding plates of ferrite. These constraints may even halt martensitic transformation and its morphology, as smaller retained
austenite islands contain a lower potential nucleation site for the transformation to martensite, which requires a higher driving force
for martensite nucleation (12,114,115). Finally, chemical composition is an important factor that controls the mechanical stability
of austenite. Elements such as C, Mn, Si, and Al (12,116,117) significantly enhance the austenite mechanical stability, and among
them, C is the element that exhibits the strongest influence.
For these reasons, blocks of retained austenite are more prone to transform to martensite, and its presence should be
minimized in favor of the thin film morphology, which is far more stable. However, Chatterjee et al. (118) have demonstrated
that the tendency of the martensite to crack in this type of microstructure depends on its absolute size. Thus, martensite
islands with a smaller size than the distance between cracks on single martensite plates, which is determined to be 10 mm
(119), do not readily crack and therefore cause brittle behavior. In this sense, Miihkinen (38) also demonstrated that even if
cementite is present, there is a critical carbide size that may need to be exceeded before a large reduction in fracture toughness
is experienced.
Another important factor controlling the toughness behavior in bainitic microstructures arose recently, which is the coa-
lescence of bainite plates, and its presence leads to a dramatic deterioration in toughness (120). Coalesced bainite occurs when
adjacent small platelets of bainite (i.e., subunits) merge to form a single larger plate. This leads to a markedly bimodal
distribution of plate thicknesses, with the fine plates about 0.2 mm thick and the larger plates 2–3 mm thick. The TEM
micrograph shown in Figure 18 (121) shows a higher resolution image of coalesced bainite in a medium C bainitic steel, where
a visible sheaf of bainite is initiating as many identically oriented platelets of an austenite grain boundary, and with each
platelet separated by a retained austenite film. The platelets later merge into a single coarse crystal. The films of austenite
disappear along the length of the sheaf, resulting in a homogeneous plate, and the excess C in the bainitic ferrite precipitates
within the ferrite as cementite. It is particularly noticeable in Figure 18 that there is a precipitate-free zone at its borders. This is
because only the C near the interface with the austenite can partition once coalescence begins, whereas the C far from the
interface must precipitate (122).
Fracture may be controlled by various microstructural features, such as a bainite packet (123). Bainite is a microstructure made
up of packets of parallel plates in the so-called morphological packet. The good toughness of this microstructure could be related to
the high density of the high-angle boundaries that these microstructures usually present (124). This kind of boundary acts as an
obstacle to cleavage propagation, forcing the cleavage crack to change the microscopic plane of propagation in order to accom-
modate the new local crystallography (125). Low-angle boundaries are not effective obstacles and, consequently, seem to have no
influence on the toughness of steels. For this reason, from the point of view of fracture mechanics, it is more convenient to use the
concept of a crystallographic packet, which is defined as the continuous set of ferrite plates with a crystallographic misorientation
lower than a certain angle (15* ).
The stress concentration associated with high heterogeneous distribution of hardness–strength is another factor that can impair
toughness. In this sense, Caballero et al. (121) explain toughness deterioration that is observed in the 0.3BAIN steel family on the
basis of the stress concentration associated with the presence of microstructural banding.
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Figure 18 TEM micrograph in a medium-C, high-Si, high-Mn bainitic steel illustrating carbide precipitation inside coalesced bainite.
Caballero, F. G.; Chao, J.; Cornide, J.; García-Mateo, C.; Santofimia, M. J.; Capdevila, C. Toughness Deterioration in Advanced High Strength
Bainitic Steels. Mater. Sci. Eng. A 2009, 525 (1–2), 87–95.
Figure 19 Comparison of ultimate strength vs fracture toughness of Conventional quenched and tempered steels (QT), maraging steels, other bainitic
steels, and NANOBAIN steels. Reproduced from Miihkinen, V. T. T.; Edmonds, D. V. Tensile Deformation of Two Experimental High-Strength Bainitic
Low-Alloy Steels Containing Silicon. Mater. Sci. Technol. 1987, 3(6), 432–440 and Miihkinen, V. T. T.; Edmonds, D. V. Fracture Toughness of Two
Experimental High-Strength Bainitic Low-Alloy Steels Containing Silicon. Mater. Sci. Technol. 1987, 3(6), 441–449.
Finally, the properties of the present alloys are compared against published data in Figure 19 (29,38,39), which highlights the
fact that novel bainitic steels exhibit an exceptional combination of mechanical properties that place this new type of microstructure
in an advantageous position for different applications such as transport, construction, and offshore industries, as well as defense
applications.
Acknowledgments
It is our special pleasure to acknowledge Professor H. K. D. H. Bhadeshia for his helpful guidelines on NANOBAIN research and
development, and Professor C. Garcia de Andres for encouraging us to do this work. Research at the Oak Ridge National Laboratory
SHaRE User Facility was sponsored by the Scientific User Facilities Division, Office of Basic Energy Sciences, U.S. Department of
Energy.
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111. Sherif, M. Y. Characterisation and Development of Nanostructured, Ultrahigh Strength, and Ductile Bainitic Steels. Ph.D. Thesis, University of Cambridge, 2006.
112. Lani, F.; Furnemont, Q.; Van Rompaey, T.; Delannay, F.; Jacques, P. J.; Pardoen, T. Multiscale Mechanics of TRIP-Assisted Multiphase Steels: II. Micromechanical Modelling.
Acta Mater. 2007, 55 (11), 3695–3705.
113. Ryu, J. H.; Kim, D.-I.; Kim, H. S.; Bhadeshia, H. K. D. H.; Suh, D.-W. Strain Partitioning and Mechanical Stability of Retained Austenite. Scripta Mater. 2010, 63 (3), 297–299.
114. Lanzillotto, C. A. N.; Pickering, F. B. Structure Property Relationships in Dual-Phase Steels. Met. Sci. 1982, 16 (8), 371–382.
115. Balliger, N. K.; Gladman, T. Work Hardening of Dual-Phase Steels. Met. Sci. 1981, 15 (3), 95–108.
116. Jacques, P. J.; Girault, E.; Mertens, A.; Verlinden, B.; Delanny, F. The Developments of Cold-Rolled Trip-Assisted Multiphase Steels. Al-Alloyed Trip-Assisted Multiphase
Steels. ISIJ Int. 2001, 41, 1068–1074.
117. Nohara, K.; Ono, Y.; Ohashi, N. Composition and Grain Size Dependence of Strain Induced Martensitic Transformation in Metastable Austenitic Stainless Steels. Tetsu To
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118. Chatterjee, S.; Bhadeshia, H. K. D. H. TRIP-Assisted Steels: Cracking of High-Carbon Martensite. Mater. Sci. Technol. 2006, 22 (6), 645–649.
119. Bhadeshia, H. K. D. H.; Keehan, E.; Karlsson, L.; Andrén, H. O. Coalesced Bainite. Trans. Indian Inst. Met. 2006, 59 (5), 689–694.
120. Keehan, E.; Karlsson, L.; Andren, H. O. Influence of Carbon, Manganese and Nickel on Microstructure and Properties of Strong Steel Weld Metals: Part 1-Effect of Nickel
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121. Caballero, F. G.; Chao, J.; Cornide, J.; García-Mateo, C.; Santofimia, M. J.; Capdevila, C. Toughness Deterioration in Advanced High Strength Bainitic Steels. Mater. Sci. Eng.
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593–597.
123. Brozzo, P.; Buzzichelli, G.; Mascanzoni, A.; Mirabile, M. Microstructure and Cleavage Resistance of Low-Carbon Bainitic Steels. Met. Sci. 1977, 11 (4), 123–129.
124. Gourgues, A. F.; Flower, H. M.; Lindley, T. C. Electron Backscattering Diffraction Study of Acicular Ferrite, Bainite, and Martensite Steel Microstructures. Mater. Sci. Technol.
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125. Rodriguez-Ibabe, J. M. The Role of Microstructure in Toughness Behaviour of Microalloyed Steels. Mater. Sci. Forum 1998, 284–286, 51–62.
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1.10 Thermomechanical Processed Steels
M Militzer, The University of British Columbia, Vancouver, BC, Canada
1.10.1 Overview of Thermomechanical Processing 191

1.10.1.1 Definition and Significance of Thermomechanical Processing 191
1.10.1.2 Historical Survey 191
1.10.1.3 Key Aspects of TMCP 193
1.10.2 Properties and Composition of TMCP Steels 196
1.10.2.1 Properties of TMCP Steels 196
1.10.2.2 Chemical Composition of TMCP Steels 198
1.10.3 Austenite Conditioning during Thermomechanical Treatment 200
1.10.3.1 Austenite Formation and Dissolution of Precipitates during Reheating 200
1.10.3.2 Recrystallization, Grain Growth, and Strain-Induced Precipitation during Rolling 202
1.10.4 Phase Transformations during Accelerated Cooling 206
1.10.4.1 Accelerated Cooling Practices 206
1.10.4.2 Transformation Products 207
1.10.4.3 Transformation Kinetics 208
1.10.4.4 Precipitation Strengthening 211
1.10.5 Summary and Outlook 212
1.10.5.1 Summary on the Role of Nb Microalloying 212
1.10.5.2 Recent Developments in TMCP Steels and Future Trends 213
References 214
1.10.1 Overview of Thermomechanical Processing

1.10.1.1 Definition and Significance of Thermomechanical Processing
Thermomechanical processing (TMP) has become an integral part of the production of many types of steels, ranging from carbon
steels to alloyed grades. TMP was pioneered in plate steel production and is intrinsically linked to the introduction of microalloyed
steels, that is, those with an addition of Nb, Ti, and/or V in amounts of usually less than 0.1 wt.%. Advanced low-carbon plate steels are
now increasingly manufactured by a thermomechanical-controlled process (TMCP) and are marketed as TMCP steels. The TMCP
concept combines controlled hot rolling with accelerated cooling (ACC) to control the microstructure through processing. The
microstructure provides the ‘fingerprints’ of a steel product that determines its properties; that is, TMCP enables the production of
as-rolled steels with final properties that are tailored to the requirements and specifications of a particular application. In addition,
TMCP has led to the development of new steels with highly desired combinations of properties that would have been impossible to
achieve with more conventional processing approaches. Even though the terminology TMCP is essentially linked to plate steels, the
TMCP concept of microstructure control is the essence of what is now known as TMP and can be applied to other steel products, such as
long products, strips, sheets, beams, bars, wires, pipes, and rails. These steel products cover an extremely wide range of applications,
including gas and fuel transportation pipes, high-rise buildings, car park decks, bridges, power transmission towers, lightning poles,
building beams and panels, offshore structures, shipbuilding, car bodies, rail tracks, and transformer sheets, among others. Figure 1
shows some typical examples of the application of TMCP steel plates. In all these applications, tremendous benefits can be derived
from modern steels that have been manufactured by optimized TMP routes. TMP is central to the concept of controlled processing
that, over the past three decades, has transformed steelmaking into a modern, cost-effective, and high-quality manufacturing industry.
Although the term TMP is now generally used to indicate controlled processing, most steel products are thermomechanically
processed in one way or another. The ancient blacksmith ‘thermomechanically processed’ a piece of iron that was heated up such
that it became red-hot and soft and could be hammered into a desired shape before quenching it in a bucket of water. This basic
manufacturing process mirrors the one performed in a modern plate or strip mill where steel slabs are reheated before hot rolling
them to the desired thickness and shape, and subsequently cooling them to room temperature. A key metallurgical feature of iron
and most low-alloy steels is that they have a face-centred cubic (FCC) crystal structure (austenite: g) at typical hot working
temperatures that undergoes a phase change to a a body-centred cubic (BCC) crystal structure (ferrite: a) when cooling to room
temperature. This phase transformation is exploited as a primary metallurgical tool to tailor a steel’s properties to the desired
specifications for a customer.
1.10.1.2 Historical Survey

Before describing the metallurgical fundamentals and advancements in state-of-the-art TMCP, a brief historical perspective will be
provided on the evolution of TMP as a controlled process tool in the steel industry. The invention of high-production steelmaking

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192 Thermomechanical Processed Steels
Figure 1 Typical applications of TMCP steels: Offshore wind farms (e.g., Alpha Ventus), high rise buildings (e.g., Shanghai World Financial
Center), sport stadiums (e.g., Olympic Stadium Athens), bridges (e.g., Samuel Beckett Bridge), pipelines, shipbuilding (e.g., Navigator Aries).
Copyright Dillinger Hütte GTS.
processes, most notably the iron blast furnace, was an essential component of the Industrial Revolution in the nineteenth century
(1). The development of a large-scale steel industry enabled the production of mass-produced steels used in major infrastructure
projects, such as railways and bridges, as well as for shipbuilding. Powerful rolling mills were constructed to hot-roll steel into the
dimensions required for specific applications. At the end of the nineteenth and the beginning of the twentieth centuries, steelmaking
practices were increasingly augmented by dedicated steel research in the laboratory. Steel compositions, primarily the use of carbon,
were identified to increase the strength of the steel produced. Knowledge was also accumulated on the effect of microstructure on
properties (2). An important paradigm shift was stimulated by the occurrence of brittle fractures in welded structures of transport
ships built during the Second World War (Liberty ships) (3). As a result, in the late 1940s, the concept of toughness was introduced as
a requirement for shipbuilding and other structural steels. Ferrite grain refinement was established as a mechanism to increase both
strength and toughness (4,5). Thus, by the 1950s, steelmakers sought ways to incorporate grain refining methods into their rolling
practices, that is, to thermomechanically process the steel to control its microstructure (6). Normal rolling practices at that time
consisted of reheating the steel slab to about 1250 * C before rolling it in multiple passes to a prescribed thickness using a reversing
mill. The rolling was usually carried out above 1000 * C, and subsequent air cooling resulted in a rather coarse grain size. To improve
the steel’s properties, additional heat treatments (e.g., normalization, quenching, and tempering) were frequently carried out after
rolling. For example, during normalization, the steel is reheated into the austenite phase field at relatively low reheat temperatures
(e.g., 900 * C) and then cooled. However, as early as 1925, it was discovered that low-temperature rolling practices could lead to finer
grain structures without normalization (2). In the 1950s, controlled rolling was introduced for C–Mn steels whereby the hot rolling
process is interrupted at an intermediate stage and resumed after the steel has cooled to a lower temperature, for example, 900 * C,
but finished in the austenite region (e.g., above 800 * C) (6–9).
Another landmark for TMP was the introduction of Nb as a microalloying element in 1958 by the Great Lakes Steel Corporation,
a division of the National Steel Corporation of the United States (10). They added up to 0.03 wt.% Nb to an ordinary semikilled
C–Mn steel, thereby achieving a remarkable increase of yield stress from 300 to 415 MPa. Early research in 1959 and 1960 established
a basic understanding of the effects of Nb on microstructure and mechanical properties in C–Mn steels (11,12). In particular, it was
recognized that adding Nb leads to ferrite grain refinement. In the mid-1960s, it was discovered that Nb greatly reduces the recrys-
tallization rates of deformed austenite (13–15). As a result, successful thermomechanical-controlled rolling practices were designed
by executing the last rolling passes at lower temperatures (e.g., 850 * C) than in conventional rolling schedules. In controlled rolling,
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Thermomechanical Processed Steels 193
the Nb-microalloyed steel is finished rolled under the so-called nonrecrystallization condition, and this processing scheme was
a breakthrough in developing modern TMP steels. In particular, controlling the rolling temperatures enabled avoidance of the region
of sluggish recrystallization that had led to variable results in the early development of Nb-treated steels (16).
These achievements paved the way for the development of microalloyed steels in the 1960s and 1970s for a wide range of
applications. In addition to Nb, V and Ti became widely used microalloying elements. These three elements are strong carbide and
nitride formers in steels and thus have potential as precipitation strengtheners, but in practice, they act differently. For example, the
effects of V or Ti in delaying recrystallization are rather modest as compared to that of Nb; that is, the controlled rolling practice of
nonrecrystallization generally requires microalloying with Nb. Microalloying enables the development of high-strength low-alloy
(HSLA) steels where the carbon content could be reduced, compared to mild steels for a given strength. The decrease in carbon
content had immediate beneficial effects on the weldability of these microalloyed grades. As a result, it was possible to develop
microalloyed linepipe steels with higher strength levels, for example, which had an enormous impact on the oil and gas industry, as
it made it economical to work on oil and gas fields in some very remote and inhospitable areas of the world. Figure 2 provides an
overview on the evolution of linepipe grades over the past 50 years. Until about 1980, these microalloyed steels, both linepipe and
HSLA, had yield stress levels of up to 420 MPa. These steels typically have a ferrite-pearlite microstructure that can be obtained by air
cooling after controlled rolling.
Around 1980, both the pipeline and the automotive industries increasingly demanded steels with yield stress levels in excess of
420 MPa. This desired increase in strength could readily be achieved by refining the ferrite-pearlite microstructure through water spray
rather than air cooling. Water cooling was first introduced as a commercial quenching method in the normalization treatment of
plates; that is, the plates were reheated into the austenite region before quenching. This process of ‘reheat quenching’ was practiced in
the manufacturing of steel plates as early as 1935 as so-called Platen-quenching (17). The first online quenching of hot-rolled plates
was reported in 1956 in Japan (18). Starting in the 1960s, hot strip mills were equipped with run-out table water spray cooling,
primarily as a method of reducing cooling times to reach the coiling temperature rather than as a microstructure control tool. It was
well established, however, that increasing the cooling rate shifts the austenite decomposition to lower temperatures, which leads to
higher strength by ferrite grain refinement and/or the formation of nonequilibrium transformation products, such as bainite and
martensite. Thus, in the early 1980s, TMCP was introduced in the production of steel plates by combining controlled rolling with
ACC, as illustrated in Figure 3, where the fundamental metallurgical phenomena of grain growth, recrystallization, work hardening,
and phase transformation are also indicated (19). The first commercial ACC facility, OLAC" (OnLine Accelerated Cooling), was
installed in 1980 by NKK (now JFE) in their plate mill in Fukuyama, Japan (20). Since then, the production of TMCP steel plates has
increasingly become the method of choice for manufacturing high-quality steel plates. Similarly, run-out table cooling in hot strip
mills was increasingly developed as a microstructure control tool through the 1980s. Since the 1980s, the steel industry has moved
into the modern era of TMP steels, which will be reviewed in this chapter, along with an emphasis on TMCP plate and strip steels.
1.10.1.3 Key Aspects of TMCP

Figure 4 schematically compares the conventional normalizing treatment of steel plates with the TMCP manufacturing path. In the
normalizing treatment, the previously hot-rolled steel is subjected to an offline heat treatment cycle with a reaustenitizing treatment at
900 * C. This low austenitizing temperature leads to a fine-grained austenite microstructure, such that upon cooling to ambient
temperature, a refined transformation microstructure can be obtained. In TMCP, on the other hand, no offline heat treatment is
required. The steel is controlled-rolled, which leaves a fine-grained and/or nonrecrystallized austenite microstructure at the exit of
finish rolling that facilitates ferrite grain refinement. Microstructure refinement is further promoted by combining controlled rolling
with ACC. Thus, TMCP enables cost-effective and energy-efficient production of steels with desirable property combinations of, for
example, high-strength, large-fracture toughness, and excellent weldability. These are the key properties required for advanced linepipe
grades, which are in ever-increasing demand. Examination of the trends shown in Figure 2 confirms TMCP as the enabling technology
to produce linepipe steels with yield stress levels of 480 MPa and higher, which are now essential for any new pipeline project.
700 Grain refinement API-X100

2000
Bainite+Martensite
Yield stress, MPa
API-X90
Bainite 1990
600 Increased
API-X80 Cooling
Year
Ferrite+Bainite 1980
500 API-X70 TMCP
Ferrite+Pearlite
1970
API-X60
400 Ferrite+Pearlite
API-X52 Hot rolled and normalized 1960
Ferrite+Pearlite
300
Toughness
Figure 2 Evolution of linepipe steels (API-Grades, API: American Petroleum Institute).
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Figure 3 Schematic of TMCP plate steel rolling. Reproduced from Yoshie, A.; Fujioka, M.; Watanabe, Y.; Nishioka, K.; Morikawa, H. Modelling of
Microstructural Evolution and Mechanical Properties of Steel Plates Produced by Thermo-Mechanical Control Process. ISIJ Int. 1992, 32 (3), 395–404.
Figure 4 Comparison of (a) conventional rolling including normalizing with (b) TMCP.
Figure 5 provides an overview of the key metallurgical features in manufacturing TMCP steel plates. The steel slabs are placed
into a reheat furnace where they are heated into the austenite temperature region. A soaking time of up to 3 hours is required to
ensure that all parts of the slab with a typical thickness of 25 cm are properly reheated at the designated reheat temperature that is
usually in the range of 1200–1300 * C. During reheating, austenite forms from the ferritic microstructure of the as-cast slabs. Further,
carbide and nitride precipitates of microalloying elements will completely dissolve, except for TiN. In particular, all Nb will be
brought into solution. While it would be attractive to lower reheat temperatures to reduce energy consumption, it is important that
these temperatures are sufficiently high to allow for the proper conditioning of austenite after reheating. This will result in
a homogeneous austenite microstructure with all microalloying additions in solution, except for the Ti, which appears in the form
of TiN. Subsequently, the steel is rolled in several passes at temperatures (usually above 1100 * C) where austenite recrystallization
can readily take place during the rolling process. This process generally leads to a substantial refinement of the austenite grain size
from the coarse-grained structure that results from substantial grain growth during reheating. Then, the rolling process is interrupted
such that the steel cools down to lower temperatures (typically below 1000 * C) before executing several passes of controlled rolling
under conditions of nonrecrystallization. This finish rolling is usually carried out in the austenite region, so that finish exit
temperatures are typically above 800 * C. The details of rolling temperature selection depend on the steel chemistry. For example,
increasing the alloy content (e.g., with Mn and Mo) frequently reduces austenite decomposition temperatures, which potentially
increases the window for controlled rolling. In some special cases, rolling may be extended into the intercritical region, where
a mixture of austenite and ferrite is present. However, intercritical rolling is a practice that is only employed to a limited extent, and
so it will not be further discussed here.
As in any conventional rolling process, an essential goal of controlled rolling is to produce a steel plate with the required
dimensions, particularly a prescribed thickness that may fall into the general range of 10–100 mm, depending on the application.
The microstructure after controlled rolling is that of nonrecrystallized austenite with a pancaked (i.e., elongated and work-
hardened) grain structure. Further, in typical plate-rolling conditions, strain-induced precipitates form; some of the Nb will form
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Figure 5 Schematic of microstructure evolution in TMCP steels (Tnr: nonrecrystallization temperature, Ar3: transformation start temperature, BS: bainite
start temperature, MS: martensite start temperature).
carbides, nitrides, and/or carbonitrides, but a significant amount of Nb will remain usually in solution. The conditioning of
austenite is controlled, as it determines the initial microstructure for austenite decomposition during ACC. Pancaked austenite
provides additional nucleation sites for ferrite, thereby promoting ferrite grain refinement. ACC is usually employed until a pre-
selected cooling stop temperature. Employed cooling rates and cooling stop temperature further determine the austenite decom-
position kinetics and the resulting transformation microstructures, for example, ferrite-pearlite, ferrite-bainite, martensite, and
others. This offers tremendous opportunities to design the final microstructure by employing different controlled cooling scenarios,
thereby tailoring the properties of the TMCP steel. To exploit this metallurgical feature, further sophisticated modifications of the
cooling process have been introduced in some plate mills by combining ACC with an inline tempering step, for example (21). ACC
has become the key technology in manufacturing high-quality TMCP steel plates. A significant challenge when applying these higher
cooling rates is to maintain a rather homogeneous cooling of the entire plate to avoid excessive thermal stresses that otherwise
would adversely affect the flatness of the plate, for example.
The previously described key metallurgical features for TMCP steel plates apply in a similar way to the rolling of steel strips with
a final thickness in the range of 1–10 mm. In a hot strip mill, steel slabs are reheated and rough rolled, in a fashion that is similar to
what happens in a plate mill. Finish rolling, however, is executed for strips in a tandem mill of six or seven consecutive roll stands.
Thus, the finish rolling time is typically about 10 s, that is significantly shorter than in plate rolling. An important consequence of
these reduced processing times is that very little, if any, strain-induced precipitation takes place during rolling; all microalloying
elements brought into solution during reheating tend to remain in solution at the exit of finish rolling. Strips are coiled products,
and the coiling temperature is the equivalent of the cooling stop temperature for plates. Controlling the coiling temperature in strip
rolling is an important metallurgical feature. In addition to the transformed microstructure resulting from run-out table cooling and
coiling, possible precipitation strengthening, due to the formation of fine carbides and/or nitrides with microalloying elements (Nb,
V, excess Ti), depends critically on the coiling temperature (22,23). Coiled products can also be produced in a Steckel mill, which
can be viewed as a hybrid of plate and strip rolling. In a Steckel mill, finish rolling takes place similarly to plate rolling in a reversing
mill, except that the strip is coiled in between individual roll passes. Rolling times are comparable to those in a plate mill. After the
completion of Steckel rolling, the strip is cooled on a run-out table and coiled similar to the procedures employed in a strip mill.
An increasing number of steel strips are now being produced through the compact strip processing (CSP) route in minimills. In
1989, Nucor Steel was the first steelmaker to start operating a CSP plant in Crawfordsville, Indiana (24). Since then, the CSP route
has been successfully adapted to routinely produce microalloyed steels using the TMCP concept. The CSP route is a major advance
to further increase the efficiency of the production of hot-rolled steel strips. Figure 6 provides an outline of a CSP mill where the
casting of thin slabs with a thickness in the range of 50–70 mm is directly combined with hot rolling. The energy savings of this
process are obvious when compared to processing steel in a conventional hot strip mill of integrated steelmakers. The reheating step
of the latter is eliminated in CSP mills. Here, the reheat furnace is replaced by a tunnel furnace that usually operates at 1150 * C to
conduct an equilibration treatment of the as-cast thin slab before hot rolling. Subsequent rolling, cooling, and coiling steps are
similar to that of a conventional hot strip mill. A major difference, however, is that less reduction is required from a thin slab to
obtain a specified final strip thickness. This reduces the window of controlled rolling, which was initially one of the challenges
to produce high-end steel strips. Meanwhile, it has been demonstrated that TMCP routes can be developed for most hot-rolled
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Figure 6 Schematic of compact strip processing (CSP) mill.
CSP steel products, including microalloyed grades with a 550 MPa yield stress. Even so, conventional hot strip mills with their less
condensed processing path offer essential advantages in manufacturing a number of advanced steel strip products, including
interstitial free steels for automotive applications and ultrahigh-strength steels with strength levels in excess of 550 MPa.
A common aspect of all TMCP practices is that they require a tight control of the processing parameters. As a result, modern mills
are high-tech facilities with a high degree of automatization, computer control, and a multiplicity of sensors to continuously
monitor the rolling process. The process parameters that are monitored and controlled include dimensions of strip or plate, rolling
speed, reduction schedule, and temperatures at selected process positions, such as reheat furnace, rough and finish rolling, coiling,
or cooling stop. Temperature control is paramount in indirectly controlling the evolution of microstructures. A wealth of micro-
structure process models has been developed since the pioneering work of Sellars et al. (25,26) in the late 1970s. Yoshie et al. (19)
were the first to develop a complete microstructure process model for TMCP plate rolling. Meanwhile, virtually all advanced
steelmakers use microstructure process models, and a recent review of these models can be found in (27). These microstructure
models are usually run offline to underpin robust processing routes and target temperatures at the various process stages.
Linepipe steels are key TCMP products that can be made as either plates or strips, depending on their required thickness. The
diversity and performance requirements for linepipe steels are ever increasing, as advances in drilling and long-distance transportation
technologies have made it possible to develop oil and gas fields in Arctic regions and deep-sea areas. Thus, there is a trend toward
long-distance pipelines, and the fluids to be transported have become more diverse. Depending on the pipeline project, the property
requirements for linepipe steels go beyond yield stress, fracture toughness, and weldability. In cases where fluids contain H2S, sour
service properties, such as resistance to hydrogen-induced cracking and sulphide stress corrosion cracking, are essential. For pipelines
in the Arctic, a paradigm shift has taken place from a stress- to a strain-based design since pipelines may traverse unstable permafrost
territory and must withstand frost heaves. Thus, linepipe steels for the Arctic must also display sufficient uniform elongation.
In this chapter, linepipe steels are selected as a primary example to describe the fundamentals of TMP of steels in more detail in
the following sections. Before describing TMCP in detail, it is useful to provide an overview on the properties and chemical
composition of TMCP steels. Then, the austenite conditioning during reheating and rolling will be discussed before analyzing phase
transformation during ACC. Finally, state-of-the-art developments in TMCP steels will be reviewed, and an outlook on future trends
will be presented.
1.10.2 Properties and Composition of TMCP Steels

1.10.2.1 Properties of TMCP Steels
The goal of TMCP is to cost-efficiently produce steel strips and plates with the properties required for a specific application. In
addition to strength and toughness, these properties may include weldability and corrosion resistance. The yield stress (and
similarly the ultimate tensile strength) depends on five factors, that is,
s ¼ so þ sss þ sprec þ sgs þ strans [1]
where so represents the intrinsic strength of the iron lattice, sss is the solid solution strengthening of alloying elements, sprec is the
contribution from precipitation strengthening, sgs describes the effect of grain size on strength, and strans accounts for the role of
transformation hardening due to the formation of pearlite, bainite, and/or martensite.
Common alloying elements added as solid solution strengtheners include Mn, Cu, Ni, Si, and P. Pickering quantified their solute
solution strength (in MPa) as follows (28):
sss ¼ 678P þ 123Sn þ 83Si þ 32Mn þ 39Cu þ 11Mo ' 31Cr [2]
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where the alloy concentrations are given in wt.%. Depending on the steel composition, the solid solution strength contribution falls
typically into the range of 100–150 MPa. It must be noted that interstitial C and N would be extremely efficient solute solution
strengtheners (5000 MPa per wt.%), provided that they remain in solid solution (29). However, the solubility of C and N in Fe is
very low and is further reduced in steels that are microalloyed with strong carbide and nitride formers. Thus, solute solution
strengthening of these interstitials is greatly reduced in practice. Instead, precipitation hardening due to fine carbides and nitrides is
utilized in TMCP steels. Precipitation strengthening depends on the volume fraction, f, and size, r, of precipitates and, at least for
practical purposes, the strength increase by precipitates is approximately related to these two factors by (29)
f 1=2
sprec f [3]
r
That is, a dense population of fine particles provides optimum precipitation strength that typically falls into the range of
50–200 MPa for TMCP steels (30).
The effect of ferrite grain size, d, on strength is given by the Hall–Petch relationship (31,32)
K
sgs ¼ F [4]
d1=2
where F is the ferrite fraction and K is approximately 22 MPa mm1/2 when the grain size is quantified from micrographs as
equivalent area diameter (in mm) (29). The effect of grain size on yield stress is remarkable in ferritic steels (F z 1). For a grain size
of 20 mm, the strength contribution is about 150 MPa and increases to 300 MPa for a grain size of 5 mm, which is thought to be the
smallest grain size that can be attained in plain carbon–manganese steels, using current processing conditions. In microalloyed
steels, further refining of the ferrite structure can be obtained, and the associated strength increases are 400 and 500 MPa for grain
sizes of 3 and 2 mm, respectively. The Hall–Petch relationship is applicable to polygonal ferrite, but the very fine ferrite micro-
structures are frequently associated with a more irregular ferrite. Irregular ferrite has a higher dislocation density and may be viewed
as a precursor to nonequilibrium transformation products, that is, bainite.
The effect of highly dislocated ferrite and/or other transformation products (i.e., pearlite, bainite, and martensite) on strength is
represented by the fifth term in eqn [1], strans. Here it must be noted that the proposed linear addition law of different strengthening
mechanisms is an oversimplification. In particular, combined strengthening due to precipitates and dislocations (sdis) is more
accurately described by a nonlinear addition law of the form (33)
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Ds ¼ s2prec þ s2dis [5]
suggesting that for highly dislocated ferrite precipitation, strengthening becomes increasingly inefficient. The hardening term due to
other transformation products depends on the volume fraction of these constituents and their characteristic feature size (e.g., sheaf
size in bainite as the equivalent of grain size and interlamellar spacing in pearlite). In principle, there is an enormous potential for
transformation strengthening. For example, in pearlitic steels (with a carbon content of approximately 0.8 wt.%) the interlamellar
spacing can be refined to the nanometer scale, such that strength levels approaching 6000 MPa can be attained in steel wires, which
constitute the strongest currently available bulk materials (34,35). These excessive strength levels cannot, however, be obtained in
the low-carbon steels that are of relevance for the TMCP steel plates and strips discussed here where yield stress requirements are
typically in the 350–800 MPa range, and in very few cases, about 1000 MPa.
For these steels, however, toughness is a property that is of equal importance as strength for many applications; the steel must be
tough at the operating temperatures to guarantee the safety of the structure where it is used. An important measure to evaluate in-
service toughness is the ductile–brittle transition temperature (DBTT, in * C) that for low-carbon structural steels is given by (36)
1=2
DBTT ¼ 19 þ 44Si þ 20Cu þ 136Sn þ 450P þ 700Nf þ 2Pe ' 12:9d'1=2 [6]
where the alloy content is in wt.%, Nf is the amount of free nitrogen (i.e., nitrogen in solution in wt.%), Pe is the pearlite fraction in
%, and d is the ferrite grain size (equivalent area diameter in mm). From eqns [4] and [6], it is evident that ferrite grain refinement
increases both strength and toughness, while pearlite decreases toughness. The most detrimental effect on toughness is associated
with free nitrogen that can be eliminated by adding strong nitride formers (most notably Ti). The effect that precipitates may have
on toughness is still somewhat controversial; some authors claim no effect in Nb steels, whereas others report an increase in the
transition temperature by approximately 0.5 * C MPa'1 precipitation strength (36,37).
Weldability is another critical aspect for TMCP steels. Good weldability requires that the fusion of base and weld metal occur
without the formation of cracks and other imperfections, such that postheat treatments of the weld can be eliminated. Here, the
chemical composition is seen to be the key parameter in a first approximation, and the carbon equivalent has been introduced to
assess weldability. For carbon contents below 0.18 wt.%, the carbon equivalent (in wt.%) is given by (38)
Si Cr þ Cu þ Mn Ni Mo V
CE ¼ C þ þ þ þ þ þ 5B [7]
30 20 60 15 10
where the alloy concentration is given in wt.%. Steels with a CE below 0.4 wt.% are considered to have good weldability. Most
notably, the effect of Nb on weldability is not included in the carbon equivalent equation. The effect of Nb on weldability was
sometimes controversially discussed, but there is now a general consensus that TMCP steels can be produced without any
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detrimental effects of Nb microalloying on weldability (39). However, the dominant factor for weldability is the carbon content of
the steel. For example, advanced linepipe steels should have carbon concentrations of 0.03–0.06 wt.% to attain excellent
weldability.
Improving steel’s corrosion resistance is another concern for steelmakers, as this would enable the building of structures without
the need to use additional corrosion-preventing techniques (e.g., coating or painting). For example, adding small amounts of Cu, P,
Si, or Cr can improve the corrosion resistance of structural steels by forming a protective rust layer that minimizes further corrosion
attack (37). In a number of applications, however, coated products remain essential, such as in the automotive industry.
1.10.2.2 Chemical Composition of TMCP Steels

As is evident from the previous description, steel properties depend on both chemistry and processing (e.g., to achieve grain
refinement), and can be controlled by an appropriate design of these two essential components for TMCP steels. These steels
are low-carbon steels with carbon levels at least below 0.25 wt %, but in modern TMCP steels, the carbon content is usually below
0.1wt% for improved weldability. The strength loss due to these lower carbon levels is mitigated by adding suitable alloying
elements. In addition to C, Mn is another base alloying element that is present in virtually any steel. In TMCP steels, the three
microalloying elements Nb, V, and Ti are the key additions to the steel chemistry. Further, Mo, B, Si, Al, Cu, Ni, and Cr are frequently
used alloying elements, whereas other elements (including N) are present as residuals resulting from the steelmaking process.
Table 1 provides an overview on the role of these alloying elements in TMCP steels.
State-of-the-art TMCP steels may have Mn contents of up to 2 wt.% to exploit the role of Mn in delaying the austenite-to-ferrite
transformation and the resulting microstructure refinement. The three microalloying additions (Nb, Ti, and V) are all strong carbide
and nitride formers, but play different roles during TMP. The thermodynamics for the tendency to form precipitates is described by
the solubility product, that is,
log½M(½X( ¼ A ' B=T [8]
where [M] is the microalloying element and [X] is the interstitial content (in wt.%) that for equilibrium conditions remain in
solution at the temperature T (in Kelvin); A and B are parameters that depend on the precipitate type (40–45). Figure 7 compares the
solubility products of the different basic carbides and nitrides that the three microalloying elements form. Here, the first observation
is that solubility limits are usually much lower in ferrite than in austenite; virtually all microalloying elements are precipitated
within the ferrite matrix in equilibrium. In austenite, TiN has an extremely low solubility, such that TiN precipitates are very stable
and will not dissolve during reheating (i.e., Ti removes N from solid solution). On the other hand, VC has the highest solubility in
austenite, and as a result, V hardly precipitates during rolling in austenite and remains fully available as a precipitation strengthener
in ferrite (i.e., V is primarily added to provide precipitation strength). The solubility limits for Nb precipitates fall into an inter-
mediate region. As a result, Nb(C,N) can form both in austenite and in ferrite depending on the processing conditions.
Formation of fine Nb(C,N) precipitates in ferrite can lead to significant precipitation strength. Further, as already noted, Nb is
unique, and its use as a microalloying addition has facilitated a paradigm shift: the production of low-carbon, high-strength TMCP
steels. Nb strongly retards static recrystallization and grain growth in hot-rolled austenite, thereby enabling rolling practices in the
nonrecrystallization regime. Further, Nb in solution also drastically delays austenite decomposition. Both of these aspects lead to
a tremendous refinement of the ferrite microstructure. In modern TMCP steels, Ti is often added as a second microalloying element.
The comparatively coarse and stable TiN precipitates limit austenite grain growth, which is particularly important in the weld heat-
affected zone (HAZ) close to the fusion line. Further, Ti is an efficient precipitation strengthener when added in excess to the N
content (in at%), such that Ti carbides and/or carbosulphides can form in ferrite.
Molybdenum, chromium, copper, and nickel are now frequently added to modern TMCP steels to augment their properties even
further. Molybdenum has similar to boron (an element used in some specific steel grades but not in linepipe steels) tremendous
Table 1 Role of alloying elements typically used in TMCP steels
Element Typical amount, wt.% Influence
C <0.25 Strengthener
Mn 0.3–2.0 Delays austenite decomposition, solute solution strengthener
Si 0.1–0.5 Deoxidizer, solute solution strengthener
Al <0.02 Deoxidizer, limits grain growth (AlN)
Nb 0.02–0.10 Very strong ferrite strengthener, strongly delays austenite recrystallization, delays austenite decomposition
Ti 0–0.15 Strong ferrite strengthener, austenite grain–size control
V 0–0.10 Precipitation strengthener
Mo 0–0.6 Delays austenite decomposition to promote bainite formation
B <0.001 Strongly delays austenite decomposition to promote bainite formation
N <0.012 Forms TiN, AlN, VN, Nb(CN)
Cr 0–1.25 Delays austenite decomposition, improves corrosion resistance
Cu 0–1.5 Precipitation strengthener, improves corrosion resistance
Ni 0–0.5 Increases toughness, improves corrosion resistance, mitigates potential hot shortness due to Cu alloying
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Figure 7 Solubility products of main microalloy precipitate species in austenite (g) and ferrite (a). Reproduced from Irvine, K. J.; Pickering, F. B.; Gladman, T.
Grain-Refined C-Mn Steels. J. Iron Steel Inst. 1967, 205 (2), 161–182; Hudd, R. C.; Jones, A.; Kale, M. N. Method for Calculating Solubility and Composition
of Carbonitride Precipitates in Steel with Particular Reference to Niobium Carbonitride. J. Iron Steel Inst. 1971, 209 (2), 121–125; Narita, K. Physical-Chemistry
of Group-IVA (Ti, Zr), Group-VA (V, Nb, Ta) and Rare-Earth Elements in Steel. Trans. Iron Steel Inst. Jpn. 1975, 15 (3), 145–152; Taylor, K. A. Solubility Products
for Titanium-Carbide, Vanadium-Carbide, and Niobium-Carbide in Ferrite. Scr. Metall. Mater. 1995, 32 (1), 7–12; Akamatsu, S.; Hasebe, M.; Senuma, T.;
Matsumura, Y.; Akisue, O. Thermodynamic Calculation of Solute Carbon and Nitrogen in Nb and Ti Added Extra-Low Carbon Steels. ISIJ Int. 1994, 34 (1), 9–16
and Fountain, R. W.; Chipman, J. Solubility and Precipitation of Vanadium Nitride in Alpha and Gamma Iron. Metall. Soc. AIME 1958, 212 (6), 737–748.
effects on delaying the austenite decomposition, and thus can improve the hardenability of the steel (46–48). For example, Mo is very
effective in delaying the formation of ferrite and can essentially prevent formation of pearlite during industrial cooling conditions
(47,49,50). Thus, adding Mo in modest amounts (0.1–0.4 wt.%) is increasingly used to produce steels with ferrite-bainite or bainite
microstructures, such as 550 MPa linepipe steels. Synergistic effects are found with Mo and Nb microalloying (47,48,51). In
particular, the addition of Mo reduces the rate of Nb(CN) precipitation in austenite so that more Nb remains in solution at the exit of
the finishing mill, thereby magnifying the benefits of Nb on grain refinement and precipitation strengthening. Further, the formation
of (NbMo)4C3 rather than NbC increases the volume fraction of precipitates that augment their strengthening role. The combined
effects of Nb and Mo on processing and resulting properties in TMCP steels were recently reviewed by Mohrbacher (47). Figure 8
provides an overview of strengthening contributions in modern TMCP steels that indicates the significance of Nb and Mo additions.
Some steelmakers have developed alloying concepts for multiphase steels by using Cr and increased Si additions in modest levels
(<1wt% for both elements) (52). This alloy design also leads to delays in the austenite decomposition that can be used to obtain
ferrite-bainite or ferrite-martensite microstructures. However, a concern with increased Si additions (i.e., in excess of 0.5 wt.%) is
that they can lead to a number of detrimental effects on properties and processing, particularly reduced surface quality.
Copper is an alloying element that has received renewed attention as a precipitation strengthener, in particular for novel
structural steels with improved fire resistance. During industrial processing, Cu can be retained in solid solution, even for slow air-
cooling conditions. But reheating to about 500–600 * C leads to significant precipitation strength (up to 200 MPa for a Cu content of
1000
Dislocation strengthening due to Mo, B, Cr

800
Mo domain
Nb precipitate size control and coprecipitation
Yield stress, MPa
600
Precipitation strengthening due to Nb, Ti, V
400 Nb domain Refining of grain size due to TMCP + Nb, Ti
Solute solution hardening due to Mn and Si

200
Yield stress of mild steel
Figure 8 Strengthening components in TMCP steels. After Mohrbacher, H. Mo and Nb Alloying in Plate Steels for High-Performance Applications.
In The International Symposium on the Recent Developments in Plate Steels; AIST: Warrendale, PA, 2011; pp 169–179.
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1.6 wt.% (53)), and this is thought to provide temporary strengthening of reinforcing beams in buildings in the event of a fire.
Conventionally, Cu is added to a number of steels to provide improved corrosion resistance. A challenge of Cu alloying is that it
may lead to hot shortness (i.e., embrittlement during reheating) that can, however, be mitigated by coalloying with Ni (usually in
similar amounts as Cu). Nickel also improves corrosion resistance and delays the austenite decomposition, with associated benefits
in terms of strength and toughness.
1.10.3 Austenite Conditioning during Thermomechanical Treatment

1.10.3.1 Austenite Formation and Dissolution of Precipitates during Reheating
The first step in TMCP steel plate rolling is reheating the slabs, so that the as-cast ferritic microstructure can transform to austenite.
This is followed by austenite grain growth. The extent of austenite grain growth for a given steel chemistry depends on the selected
soaking temperature. Figure 9 shows a recent laboratory study on austenite grain growth in a state-of-the-art 550 MPa linepipe steel
containing Nb, Ti, and Mo (54). Here, grain growth was measured continuously in situ using a novel laser ultrasonic technique. The
symbols indicate conventional metallographic measurements of the grain size that benchmark the laser ultrasonic data. The
observed grain growth behavior is a representative example for austenite grain growth in low-carbon steels. Grain growth rates
increase with reheat temperature. At each individual temperature, an initial period of comparatively rapid growth precedes a second
stage where the grain size changes very little, and a limiting grain size is eventually reached. The limiting grain size significantly
increases with temperature. Examining Figure 9 in more detail reveals that reheat temperatures can be grouped into three regions
regarding grain growth. For sufficiently low-reheat temperatures (here below 1000 * C), very little grain growth takes place and a fine
austenite microstructure forms (here with grain sizes below 20 mm). Conventional normalizing treatments essentially take
advantage of this limited grain growth. Then, there is an intermediate temperature region where significant grain growth takes place.
The onset of this temperature region is commonly referred to as the grain-coarsening temperature (1050 * C in the present example).
For even higher temperatures, much grain growth has already taken place during heating (here at 10 * C s'1) before reaching the
soaking temperature, where further grain growth results in coarse-grained austenite with average grain sizes larger than 50 mm in the
present case. These general trends of austenite grain growth can be rationalized when considering the role of precipitates and their
gradual dissolution during reheating. Four precipitate types were found in the investigated steel before conducting the grain growth
tests: Mo2C, small Nb(CN) with sizes <5 nm, large Nb(CN) with sizes >10 nm, and some coarser TiN (55). Further, it was found
that during reheating, the Mo and Nb precipitates dissolve such that only TiN remains precipitated for reheat temperatures of
1200 * C and higher. Mo2C essentially dissolves before the completion of austenite formation and, thus, has no effect on austenite
grain growth. For the lower reheat temperatures (<1000 * C), Nb(CN) remains precipitated and provides strong pinning opposing
grain boundary motion, such that only limited grain growth can take place. The onset of grain coarsening and the intermediate grain
growth temperature range coincides with the dissolution of Nb(CN). The dissolution of these precipitates leads to a rapid decrease
in pinning forces such that abnormal grain growth stages can result. During abnormal growth, a bimodal grain structure forms that
consists of a few large grains and many small grains. Once surpassing these abnormal growth stages, normal growth of the coarse
grain structure resumes at higher reheat temperatures.
The presence of a heterogeneous microstructure must be avoided as a result of reheating the steel during TMCP plate or strip
rolling; heterogeneous microstructures could lead to unacceptable property variations throughout the plate or strip. Thus, in practice,
sufficiently high reheat temperatures are selected to eliminate any possible remnants of potential abnormal growth. After reheating,
Figure 9 Austenite grain growth in a 0.06 wt.% C–1.65 wt.% Mn–0.034 wt.% Nb–0.012 wt.% Ti–0.24 wt.% Mo 550 MPa steel measured by laser
ultrasonics (lines) and metallographically (symbols). Reproduced from Maalekian, M.; Radis, R.; Militzer, M.; Moreau, A.; Poole, W. J. In Situ Measurement
and Modelling of Austenite Grain Growth in a Ti/Nb Microalloyed Steel. Acta Mater. 2012, 60 (3), 1015–1026.
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Figure 10 Austenite grain growth during reheating in low-carbon steels. Reproduced from Yoshie, A.; Fujioka, M.; Watanabe, Y.; Nishioka, K.; Morikawa,
H. Modelling of Microstructural Evolution and Mechanical Properties of Steel Plates Produced by Thermo-Mechanical Control Process. ISIJ Int. 1992,
32 (3), 395–404.
the steel will have a coarse-grained austenite microstructure with all microalloying elements in solution, except for the amount of Ti
that is precipitated as TiN. The actual amount of Ti in solution will depend on the steel chemistry, in particular the Ti N ratio and
reheat temperature. As a rule of thumb, all excess Ti (i.e., when there are more Ti atoms than N atoms in the steel) will be in solution.
In detail, the grain growth kinetics depends on steel chemistry, as shown in Figure 10 (19). Here, grain growth behavior is shown
for four classes of steels: (1) plain C–Mn steel, (2) Al-killed C–Mn steel, (3) Nb-microalloyed steel, and (4) Ti-microalloyed steel.
The plain C–Mn steel provides an idealized upper limit for grain growth that is unaffected by any precipitates: That is, unpinned
grain growth occurs with no apparent grain size limit. In the Al-killed steel, AlN precipitates are initially present and dissolve
gradually during reheating, affecting grain growth in a similar way, as discussed above for the Nb(CN) dissolution. When
comparing grain growth in the Al-killed steel with the Nb-microalloyed steel that otherwise has the same base composition, it is
apparent that grain growth rates are generally lower in the Nb-treated steel, even after all precipitates are dissolved at higher
temperatures. This behavior is consistent with a solute drag effect of Nb on grain boundary motion that slows grain growth rates
(56). Finally, in the Ti-microalloyed steels, grain growth is further reduced. The case shown in Figure 10 displays a situation where Ti
microalloying leads to an apparent grain size limit (here about 50 mm) even for reheat temperatures as high as 1300 * C. Whether or
not such a grain size limit is observed depends in detail on the Ti and N content of the steel and the casting conditions. The resulting
TiN particle size distribution determines the pinning pressure for grain growth. In detail, the pinning pressure, P, is related to the
volume fraction, f, and size, r, of the precipitates by
f
P¼k g [9]
r
where g is the grain boundary energy and k is a constant that has been estimated based on experimental observations of limiting
grain sizes in steels and other polycrystalline materials (57). The pinning pressure increases with the density of the precipitates, such
as when decreasing the particle size for a given volume fraction. For steels with similar Ti and N compositions, one would expect the
same volume fraction, but the particle sizes could be quite different as a function of the processing conditions – most notably also
those found during casting, as TiN may already start to form in the molten steel.
The lines in Figure 10 show predictions of a grain growth model that incorporates a pinning pressure, as proposed in (19,54).
" #
d 4g
dg ¼ M 'P [10]
dt dg
Here, dg represents the average austenite grain size, and M is the grain boundary mobility; M is a steel-specific parameter that
depends on temperature and is usually determined by fitting to experimental grain growth kinetics (55). The pinning pressure can
be determined from the observed limiting grain size and decreases with increasing temperature, clearly indicating the dissolution
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regions, such as the dissolution of small and large Nb(CN) in the 550 MPa linepipe steel. In a more rigorous way, the changes in
P during reheating can be tracked by modeling the dissolution of precipitates that is controlled by diffusion of the microalloying
element (e.g., Nb) that forms the carbide or nitride (55).
In CSP, the reheat practices are quite different. The slab comes directly from the continuous caster and is at elevated temperatures
(typically above the austenite decomposition temperature) before entering the tunnel furnace that is the equivalent of the reheat
furnace in conventional mills. In the tunnel furnace, the steel is equilibrated by reheating at temperatures of approximately 1150 * C,
that is, a much lower temperature than in conventional reheating.
The challenge here is to control precipitation in microalloyed steels. It has been demonstrated that processing conditions can be
established such that TiN and perhaps more complex precipitates (Ti,Nb)(C,N) form in the as-cast slab before entering the tunnel
furnace where these precipitates change little, but some of the complex precipitates (Ti,Nb)(C,N) may dissolve, bringing more Nb
and Ti in solution (24). At the exit of the tunnel furnace, the situation is very similar to that of conventional reheating: Most of the Ti
is precipitated as TiN, and remaining microalloying elements are mostly in solution, perhaps with the exception of some Nb that
may coprecipitate with Ti. The difference with the CSP route, as compared to conventional reheat practices, is that an as-cast
austenite microstructure is present rather than the coarse-grained austenite that results from grain growth. In subsequent pro-
cessing, this appears to be of little consequence. In the first stands of a CSP mill, the austenite microstructure experiences dramatic
changes similar to that during rough rolling in a conventional hot strip mill and the as-cast initial structure is broken down through
recrystallization.
1.10.3.2 Recrystallization, Grain Growth, and Strain-Induced Precipitation during Rolling

The main metallurgical phenomena present during rolling the steel are work hardening, recovery, recrystallization, and grain growth
of austenite. The extent to which recrystallization and grain growth can occur depends in detail on steel chemistry and rolling
conditions that are, therefore, precisely controlled in TMCP. The important parameters for hot rolling are the rolling temperatures,
rolling speeds, roll forces, and reduction in thickness per pass. The reduction, rt, can be translated into a true strain, ε,
1
ε ¼ ln [11]
1 ' rt
and, by using the rolling speed, into a strain rate, ε_ , to quantify the work hardening. Roll forces are limited by the rolling power of
individual roll stands. The required roll force to execute a particular thickness reduction increases with reduction, plate or strip
width, and the flow stress (the resistance of the steel to deformation). Typical stress–strain curves for hot rolling conditions are
shown in Figure 11. The stress increases with applied strain and reaches a plateau for sufficiently large strains, which is the so-called
mean flow stress, sflow, commonly used to estimate roll forces. The flow stress decreases with increasing temperature (i.e., it is easier
to deform a material at higher than at lower temperature) and decreasing strain rate. Thus, frequently a temperature corrected strain
rate, that is, the Zener–Hollomon parameter
" #
Q
Z ¼ ε_ exp [12]
RT
is introduced to characterize the flow stress behavior. Here, Q is an effective activation energy, R is the ideal gas constant, and T is the
absolute temperature (in Kelvin). Further, the flow stress depends on steel chemistry and increases usually with alloying content.
Because flow stresses are lower at higher temperatures, rolling schedules are commonly designed to have higher reductions per pass
at higher than at lower temperatures. From a roll force perspective, rolling should be conducted at temperatures as high as possible,
Figure 11 Typical flow stress curves for different temperatures and strain rates in advanced low-carbon steels.
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and this is essentially done in conventional rolling. In TMCP, however, this paradigm is revisited as rolling temperatures are selected
to control microstructure.
The mean flow stress curves provide important information on the deformed microstructure. During deformation, austenite
grains are elongated in the rolling direction (the grains are pancaked), and dislocations are generated (the steel is work hardened).
During deformation, two competing processes determine the dislocation density. Dislocations are created due to the deformation
work, but dynamic recovery simultaneously occurs (i.e., the annihilation and rearrangement of dislocations). The balance between
these two processes leads to the emergence of the plateau in the flow stress curves (see Figure 11). Recovery during hot working
involves diffusional processes (i.e., dislocation climb), and thus the extent of recovery increases with temperature (higher diffusion
rates) and decreasing strain rate (longer deformation times), whereas the dislocation generation rate scales with strain rate. The flow
stress curves provide a measure of the stored energy in terms of the average dislocation density:
rfs2flow [13]
The dislocation density, and thus the stored energy, may vary throughout the deformed microstructure.
Controlled rolling is conducted in two stages: rough rolling at higher temperatures and finish rolling at lower temperatures.
Rough rolling is executed at temperatures (>1100 * C) where recrystallization can readily take place. Recrystallization during hot
working is classified into three categories: (1) static recrystallization, (2) dynamic recrystallization, and (3) metadynamic recrys-
tallization. Static recrystallization occurs after deformation in the interpass time between subsequent roll passes. In contrast,
dynamic recrystallization takes place during deformation (such as in the roll-bite), and metadynamic recrystallization depicts
a situation where recrystallization is initiated in the roll-bite but is completed in the interpass region. For TMCP practices, static
recrystallization is the dominant mechanism, as rolling temperatures and strains per pass are sufficiently low and roll speeds
sufficiently high (19,22). Dynamic recrystallization can only take place provided the steel has been deformed above a critical strain,
which increases with decreasing temperature and increasing strain rate (58). There may be some potential for dynamic recrystal-
lization in the initial passes of rough rolling where temperatures and reductions are high. In subsequent passes, however, static
recrystallization takes place and determines the austenite microstructure at the exit of rough rolling.
Austenite grains can be refined during rough rolling in the recrystallization range. The recrystallized grain size, drex, depends
primarily on strain (i.e., reduction) and initial grain size in the case of static recrystallization (19,29). Microalloying additions, strain
rate, and temperature have a comparatively minor effect on drex. In a multipass rolling operation, successive grain refinement is
observed from pass to pass, as shown in Figure 12 for hot strip rolling of plain low-carbon steels. The coarse-grained austenite
present after reheating is quickly broken down by recrystallization. During the interpass time of rough rolling, significant grain
growth may occur. However, during finish rolling, a limiting recrystallized grain size is attained that typically falls into the range of
10–30 mm, and interpass times are too short and temperatures are too low for substantial grain growth to occur after the completion
of such recrystallization. The situation in Nb-microalloyed steels is similar, as indicated by the solid line in Figure 12. For Nb-treated
steels, however, recrystallization cannot take place anymore in the final passes of finish rolling and work hardening of austenite
occurs. Further, as Nb also delays grain growth, the magnitude of grain coarsening during rough rolling is greatly reduced.
The rate of recrystallization depends on steel chemistry, particularly the microalloying content, the temperature, and the
deformed microstructure, such as the stored energy and its spatial distribution, as well as the austenite grain size. Recrystallization is
a thermally activated process such that recrystallization rates increase with temperature. Further, recrystallization rates increase with
driving pressure due to the stored energy that scales with the flow stress (recrystallization rates increase with amount of reduction
and strain rate). An important aspect of recrystallization is its onset through the formation of small recrystallized grains. The
detailed microstructural mechanisms in these early stages of recrystallization are still debated, but it is generally accepted that
austenite grain boundaries provide suitable sites for the onset of recrystallization. Thus, in addition to steel chemistry and
250
C–Mn steel
Austenite grain size, m
200 Roughing Nb steel
150
100
Finishing
50
No recrystallization
0
R1 R2 R3 R4 R5 R6 R7 F1 F2 F3 F4 F5 F6 F7
Rolling station
Figure 12 Typical austenite grain size evolution during rough and finish rolling of low-carbon steels in a hot strip mill.
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deformation condition (temperature, reduction, and strain rate), the austenite grain size determines static recrystallization kinetics
(19,22,27). Growth of recrystallized grains is governed by the velocity of the moving grain boundary
v ¼ MðG ' PÞ [14]
where G denotes the driving pressure given by the stored energy. Similar to grain growth, a pinning pressure due to precipitates can
significantly affect recrystallization (27,59). Driving pressures for recrystallization are, however, typically at least an order of
magnitude larger than that of grain growth. All three parameters (M, G, P) that determine the growth rate depend on steel chemistry,
but the grain boundary mobility and pinning pressure are strongly affected by a number of alloying additions, in particular
microalloying with Nb (19,47).
A detailed examination of the above recrystallization behavior is used in designing controlled rolling schedules for finish rolling.
Here, an important criterion is the so-called nonrecrystallization temperature, Tnr, which is the temperature below which rolling is
conducted without complete recrystallization taking place (37). Figure 13 summarizes the effect of microalloying additions on Tnr
for typical rolling conditions (60). Nb has a dramatic effect on retarding recrystallization, whereas Ti and V only modestly retard
recrystallization. Microalloying with Nb opens a wide window for nonrecrystallization rolling: for example, for 0.05 wt.%, Nb
recrystallization cannot be completed for typical rolling conditions below 1000 * C, and for 0.1 wt.% Nb, this temperature is further
increased to approximately 1050 * C. Employing Nb microalloying at the 0.1 wt.% level has led to the benefits of thermomechanical
rolling at higher temperatures in the so-called high-temperature processing (HTP) route and, thus, lower rolling loads (51).
However, to conduct HTP in practice, the carbon content must be sufficiently low, and most of the free N must be scavenged by Ti
such that all Nb can be easily brought into solution during reheating. Further, alloying with Mo significantly retards recrystallization
(albeit to a much lesser degree than Nb), and the combined role of Nb and Mo has to be considered when designing rolling
schedules to obtain complete recrystallization in the roughing stands but work hardening during finish rolling (47).
Adding Ti has a moderate effect on recrystallization, but even microalloying with 0.1 wt.% Ti does not raise the temperature of
incomplete recrystallization much above 900 * C. Thus, controlled finish rolling below Tnr is limited to Nb-microalloyed steels in
practice. Controlled rolling practices in plain low-carbon steels and other steels not containing Nb is nevertheless an important part
of thermomechanically processing these steels. Here, finish rolling is conducted at sufficiently low temperatures (<1000 * C) to
essentially limit grain growth after completion of recrystallization (austenite grain refinement is attained through recrystallization).
This can be accomplished more easily in strip mills with interpass times typically decreasing from 5 to 0.5 s in the tandem finish
mill. In plate mills, interpass times are large enough (8–20 s) so that controlled rolling is primarily conducted using the non-
recrystallization concept, and TMCP steel plates are microalloyed with Nb. Figure 14 compares these two types of controlled finish
rolling for steels both with and without Nb microalloying, and their consequences for subsequent ferrite grain refinement.
In detail, Tnr depends not only on steel chemistry but also on the rolling schedule (reduction schedule and interpass times).
There are important differences between strip and plate rolling that involve whether or not recrystallization is affected by strain-
induced precipitation. Figure 15 summarizes the recrystallization regimes with respect to precipitation: A – recrystallization is
complete before precipitation; B – recrystallization and precipitation occur concurrently; and C – precipitation is complete before
recrystallization. Regime A is significant for strip rolling with short processing times and regime B is significant for plate rolling with
longer processing times, whereas regime C requires much longer times that are not of practical interest. In particular, recrystalli-
zation regime B, where recrystallization interacts with precipitation, is quite striking. The formation of strain-induced precipitates
(i.e., precipitation in the deformed microstructure) may bring recrystallization to a temporary halt when fine precipitates are
sufficiently densely distributed. In this situation, the pinning pressure is larger than the driving pressure, and the grain boundaries
stop migrating. When the holding (or interpass) time is increased, the precipitates start to coarsen and the particle density decreases.
Figure 13 Effect of microalloying addition on the nonrecrystallization temperature in a 0.07 wt.% C–1.4 wt.% Mn–0.25 wt.% Si steel. After Cuddy, L. J.
Effect of Microalloy Concentration on the Recrystallization of Austenite during Hot Deformation. In Thermomechanical Processing of Microalloyed
Austenite; DeArdo, J. A., Ratz, G. A., Wray, P. J., Eds.; TMS-AIME: Warrendale, PA, 1982; pp. 129–140.
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Figure 14 Comparison of controlled rolling in (a) plain-carbon and (b) Nb microalloyed steels; ferrite nuclei shown in black.
A B C
Fraction recrystallized
Time
Figure 15 Recrystallization regimes in Nb microalloyed steels: A – recrystallization complete before precipitation, B – recrystallization and precipitation
occur concurrently, and C – precipitation complete before recrystallization.
As a result, the pinning pressure decreases, and eventually the grain boundaries become unpinned again, such that recrystallization
resumes. The recrystallization stop condition shown by the plateau in regime B can be attained in plate rolling and provides a clear
definition of Tnr. In summary, two different mechanisms lead to the enormous retarding effect of Nb on recrystallization that is
utilized in controlled rolling. In plate and Steckel rolling, strain-induced precipitation is expected to occur that essentially stops
recrystallization completely. Evidence of Nb precipitation in austenite can be found in plate or Steckel rolled Nb-treated steels. For
example, the previously discussed 550 MPa linepipe steel was Steckel rolled and displayed two families of Nb(CN) precipitates
(coarse precipitates that had formed in austenite during rolling and fine precipitates formed in ferrite during coiling (54,55)). In
strip rolling, recrystallization rates are primarily reduced by the solute drag of Nb such that during the short processing times
(approximately 10 s) in the finish mill, recrystallization cannot take place. Hutchinson et al. (56) have shown that Nb in steel
provides very strong solute drag, such that the effect of solute Nb in controlling grain size and recrystallization can dominate over
the pinning arising from NbC precipitates.
Under nonrecrystallization conditions, the process of rolling leads to continuous work hardening of austenite and associated
increases in the mean flow stress. In strip mills, observations have been made by analyzing the recorded roll forces that the flow
stress drops in selected cases in the final rolling stands. This has led to the interpretation that dynamic recrystallization may occur
under these conditions (the strain accumulation due to the absence of static recrystallization exceeds the critical strain necessary for
dynamic recrystallization to occur (61,62)). This interpretation, however, requires further studies as alternative explanations, such as
extended recovery, may be possible; but at least for now, this seems to be of more academic interest. If dynamic recrystallization was
indeed to occur, it would lead to a dramatic refinement of the austenite microstructure, with benefits comparable to those of the
work-hardened austenite on phase transformation on the run-out table (63).
For sufficiently long interpass times (e.g., in plate rolling), strain-induced precipitation of Nb(CN) occurs and prevents further
recrystallization (64,65). Deformation leads to the introduction of crystalline defects in the microstructure, primarily in the form of
dislocations. Nucleation of precipitates is augmented as the high dislocation density increases the number of potential nucleation
sites. Further, Nb tends to form complexes with vacancies and may travel with excess vacancies formed as another crystalline defect
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Temperature
Deformation
Time
Figure 16 Schematic time-temperature-transformation (TTT) diagram showing the effect of deformation on precipitation kinetics of Nb(CN).
during deformation to vacancy sinks, such as dislocations and grain boundaries (66). After annihilation of these vacancies, Nb is
enriched at these sinks, thereby providing an increased local supersaturation for the formation of Nb-containing precipitates. Both
aspects (the increased density of potential nucleation sites and increased local supersaturation) lead to significantly increased
nucleation rates of Nb(C,N) as compared to those in undeformed austenite. The precipitation start times decrease with increased
strain applied, as schematically illustrated in Figure 16. The nose of the precipitation curve is around 900 * C, with precipitation start
times of approximately 10 s in work-hardened austenite, as concluded from laboratory studies (22,29).
1.10.4 Phase Transformations during Accelerated Cooling

1.10.4.1 Accelerated Cooling Practices
The austenite decomposition during cooling determines the final microstructure and, thus, the properties of the steel. Therefore, the
austenite-ferrite transformation is the key metallurgical tool to tailor properties of hot-rolled steels required for a particular
application. ACC technologies are increasingly employed to create refined microstructures with improved properties, such as higher
strength. In plate mills, the cooling concepts can be classified as follows (67):
1. ACC results in cooling where the difference of cooling rate between surface and center is kept low.
2. Heavy ACC (HACC) is a special variant of ACC, but with lower final cooling temperature and higher cooling rate.
3. Direct quenching (DQ) is the fastest possible cooling of the surface, similar to conventional quenching. The center of the plate is
also cooled to below the martensite start temperature.
4. DQ plus self-tempering means that the center heat still present is exploited after a very short cooling time to achieve self-
tempering.
These ACC methods are particularly important for linepipe and shipbuilding steel grades with increased strength, whereas the
two quench methods lead to either martensitic steels (DQ) or partially martensitic steels.
The heat transfer and boiling phenomena that occur when steel plates are water-cooled can be broadly classified into three
modes: nucleate boiling, transition boiling, and film boiling (Figure 17). At the start of plate cooling, the steel surface temperature is
high and film boiling is predominant. In this case, a film of steam forms between the steel surface and the cooling water such that
heat must be transferred through this steam film. In contrast, for sufficiently low steel surface temperatures, nucleate boiling occurs
where the cooling water is in direct contact with the steel surface and heat transfer occurs by the generation of bubbles. Therefore,
during cooling of the steel, the steam film becomes unstable as the surface temperature decreases. The cooling water starts to come
locally into direct contact with the plate, and film and nucleate boiling start to coexist. This cooling situation is the transition boiling
regime, where boiling gradually shifts from film to nucleate boiling. Unlike for the film and nucleate boiling regimes, the cooling
capacity characteristically increases in the transient boiling condition as cooling proceeds. Therefore, any temperature differences
that may exist before cooling are magnified during the cooling process.
When pushing the limits of HACC by further increasing the cooling rates with conventional ACC practices by using spray or
laminar cooling, the transition boiling regime is rapidly attained such that cooling becomes unstable and temperature deviations
increase as cooling proceeds. As a result, microstructures are nonuniform and thermal stresses build up, leading to unstable plate
quality. Thus, in state-of-the-art ACC lines, such as the Super-OLAC of JFE Steel, the goal is to achieve nucleate boiling over the entire
plate surface virtually simultaneously with the start of cooling, thereby avoiding transition boiling (17,68). Here, the top side of the
plate is subjected to corridor flow cooling, where the cooling water flows in the direction of plate movement from nozzles located in
close proximity to the plate. Induced laminar flow cooling is employed for the bottom side of the plate; that is, cooling is performed
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Advanced ACC
Nucleate boiling
Heat flux
Conventional ACC
Transition boiling Film boiling
Temperature
Figure 17 Heat flux evolution in conventional and advanced accelerated cooling.
by spraying cooling water from nozzles densely arranged in the water tank. Using this cooling method, nucleate boiling can be
realized with a high cooling capacity on both the top and bottom sides of the plate (see Advanced ACC in Figure 17). For plate
thicknesses of more than 30 mm, this method attains high cooling rates that approach the theoretical cooling limit; that is, heat
diffusion from the interior of the steel plate becomes rate limiting. This maximum cooling rate decreases with plate thickness from
about 30 * C s'1 for a thickness of 20 mm to about 5 * C s'1 for a thickness of 100 mm.
A major advantage of these advanced cooling methods is that the surface temperature distribution of the plate shows improved
uniformity. For example, with the advanced cooling system CLC-m of Nippon Steel Corporation, the surface temperature variance
across the plate width is reduced by approximately a factor of two, as compared to conventional ACC (17).
1.10.4.2 Transformation Products

Changing the cooling conditions not only refines the microstructure resulting from the phase transformation, but also leads to
different transformation products. In low-carbon steels, there are three types of microstructures, broadly speaking: (1) ferrite-
pearlite, (2) bainite, and (3) martensite. Figure 5 shows typical micrographs of these three transformation products. The ferrite-
pearlite microstructure results from slow cooling (e.g., air cooling) and represents lower strength levels. Increasing the cooling
rate will lead to bainitic microstructures with higher strength, whereas quenching (i.e., sufficiently fast cooling) enables the
formation of martensite, which has the highest strength. The general trend of microstructures required for linepipe steels with
increasing strength and toughness are shown in Figure 2. Here, ferrite-pearlite microstructures are sufficient up to API-X70 grades
with a minimum yield stress of 480 MPa. For ferrite-pearlite steels, the strength is a function of ferrite grain size and pearlite fraction,
as described in Section 2.1.
For higher strength linepipe steels, increasingly bainitic microstructures are required. The above discussed 550 MPa linepipe
grade for Arctic applications is a typical example of API-X80 steel with a ferrite-bainite microstructure. In detail, the microstructure is
even more complex, as it also contains martensite/austenite (MA) constituents. The MA constituents (their fraction, size, and
morphology) critically determine the fracture toughness of the steel (69). Increasing the strength level above 550 MPa will require
the steel to have a completely bainitic microstructure. Examining bainitic microstructures in more detail reveals different variants of
bainite. In order of decreasing transformation temperature and increasing strength, these bainite variants are classified as granular
bainite, upper bainite, and lower bainite (70). Figure 18 shows the typical micrographs of these different bainitic microstructures
that are increasingly required for higher strength TMCP steels.
A multiphase concept is becoming more common in advanced high-strength steels to tailor their properties for specific appli-
cations. API-X80 steels represent an example of this concept, with a microstructure that consists of ferrite, bainite, and MA. The
multiphase microstructure approach has been employed since the turn of the century, particularly in automotive steel sheets. Dual-
phase steels with a ferrite-martensite microstructure have become a material of choice for car makers (71–73). In these cases, hard
martensite is embedded in a soft ferrite matrix, creating a composite structure that combines high strength with good ductility and
enables more complex forming operations than in conventional high-strength steel sheets. Other members of the multiphase steel
family for automotive applications are complex phase steels with a ferrite-bainite-martensite microstructure and transformation-
induced plasticity (TRIP) steels that contain 5–20% retained austenite in addition to ferrite, bainite, and martensite. The
retained austenite transforms, at least in part, to martensite during a forming operation, which leads to even better forming
characteristics than that of dual-phase steels. However, the consistent industrial creation of these complex microstructures remains
a challenge, such that TRIP steels have remained a niche product. While all these multiphase steels can be produced as hot-rolled
coils – hot-rolled dual-phase steels have been fabricated since about 1980 for wheel rims and discs – these steels are primarily
produced by cold-rolling and subsequent intercritical annealing in the austenite-ferrite two phase field. This particular TMP route is
beyond the scope of this chapter.
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Figure 18 Different variants of bainite in low-carbon steels: (a) granular bainite; (b) upper bainite; and (c) lower bainite. Reproduced from Schwinn, V.;
Bauer, J.; Flüss, P.; Kirsch, H. J.; Amoris, E. Recent Developments and Application of TMCP Steel Plates. In The International Symposium on the
Recent Developments in Plate Steels, AIST, Warrendale, PA, 2011; pp. 1–11.
1.10.4.3 Transformation Kinetics

During thermomechanical control processes, it is paramount to develop cooling strategies after finish rolling that will produce
transformation products that are required for the properties sought. The transformation kinetics depend on the steel chemistry and
the cooling path, that is, primarily the cooling rate employed, but also on the austenite conditioning, such as the grain size, degree of
pancaking, and microalloying elements (e.g., Nb) present in solution.
Because of its technological relevance, the decomposition of austenite in steels has been extensively investigated for many
decades. In particular, the continuous cooling transformation (CCT) behavior is a critical piece of information for steelmakers to
select steel chemistry and processing conditions. In CCT tests, steel samples are reheated to a predetermined austenitizing
temperature to produce a suitable austenite grain size and then cooled at different rates to room temperature. The transformation
kinetics can be monitored with a dilatometer, for example, that records the volume increase due to the FCC–BCC transformation
(FCC is a closed-packed crystal structure, whereas BCC is a less closely packed structure with a molar volume that is about 1%
larger). The resulting microstructure can be analyzed with metallographic techniques to determine the fraction of transformation
products. It can usually be assumed that there is a sequential formation of different transformation products, starting with ferrite
followed by pearlite, bainite, and martensite (22,27). Figure 19 shows a schematic CCT diagram. Here, it is evident that slow
cooling (such as air cooling of a steel plate) will result in a ferrite-pearlite microstructure, whereas faster cooling lowers the
transformation temperature, thereby encouraging the formation of bainite and martensite. In detail, the transformation temper-
atures and cooling rates required to form bainitic and martensitic microstructures depend on steel chemistry, as will be discussed in
more detail later in this section.
Figure 19 Schematic CCT diagram; dashed lines indicate cooling paths; the solid lines indicate transformation start and finish; the numerals are a formal
labeling for the four different cooling paths that are shown schematically in the figure.
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Figure 20 Final microstructure (F ¼ ferrite, P ¼ pearlite, and B ¼ bainite) for different cooling rates in 0.06 wt.% C–1.49 wt.% Mn–0.047 wt.% Nb steel
with an initial austenite grain size of 40 mm.
The other aspect of increased cooling rates is refining the microstructure. Figure 20 shows a sequence of micrographs from CCT
tests for a Nb-microalloyed low-carbon steel where a ferrite-pearlite/bainite microstructure forms. Increasing the cooling rate from
0.5 to 10 * C s'1 leads to a dramatic grain refinement and an increased fraction of bainite. For modest cooling rates (here 0.5 and
1 * C s'1), mostly polygonal ferrite forms, whereas an increase of the cooling rate to 10 * C s'1 leads in the present steel to the
formation of nonpolygonal microstructures that consist mostly of bainitic transformation products. These transformation trends
illustrate the conceptual idea of ACC; that is, increasing the cooling rate leads to a refined microstructure and eventually to the
formation of bainite.
These general trends should be discussed in more detail to better appreciate the design of TMCP plate and strip rolling practices.
During finish rolling, austenite will be conditioned to provide a suitable initial microstructure for austenite decomposition. Two
important factors of the prior austenite microstructure affect the transformation behavior: (1) the grain size and (2) the degree of
pancaking, as schematically illustrated in Figure 14. The primary motivation for controlled rolling is refining the austenite
microstructure by either grain refinement or work hardening as it translates into a finer ferrite grain size. The key here is that ferrite
nucleates primarily at austenite grain boundaries: that is, decreasing the grain size leads to a larger grain boundary area per unit
volume and results in an increased density of ferrite nuclei. Additional sites for ferrite nucleation are introduced in work-hardened
austenite due to the presence of the deformation substructure, for example, shear bands, subgrain boundaries, and others. The
higher nuclei density and associated shorter growth distances to complete the transformation lead to higher transformation
temperatures, as compared to coarser prior austenite microstructures.
Adding alloying elements such as Mn, Mo, Nb, B, and others makes the steel more hardenable by shifting the transformation to
lower temperatures, so that slower cooling rates are sufficient to produce fine-grained ferrite, bainite, and/or martensite (19,46–48).
For example, Nb in solution is quite efficient in delaying the austenite decomposition. As illustrated in Figure 21, the trans-
formation temperature in the 550 MPa linepipe steel can be substantially reduced (by up to 100 * C) when Nb is in solution. Mo is
another element with a major effect on the austenite decomposition kinetics. There is a large body of work on the effect of Mo on the
transformation kinetics that shows how Mo can delay the ferrite formation and can lead to incomplete transformation, thereby
affecting the separation of the ferrite and bainite portions in the overall transformation through the emergence of the bainite bay in
the time-temperature-transformation diagrams with increasing Mo content (46–50). Thus, adding Mo is an efficient strategy that
can be used to tailor the phase transformation such that under the constraints of an industrial processing line, the desired
multiphase microstructures form. The synergistic effects of Nb and Mo on the phase transformation are less well characterized.
The addition of these alloying elements is limited for a variety of reasons, including cost, but also process limitations (such as in
terms of casting) and inherent metallurgical factors (no added benefits are obtained in the final properties when increasing Nb
microalloying above 0.1 wt.% in TMCP steels). Thus, cooling stop and coiling temperatures in plate and strip mills must be lowered
below 500 * C to promote bainite formation. Otherwise, slow air cooling of a plate or slow coil cooling following ACC would
encourage formation of ferrite-pearlite microstructures.
Much attention has been paid to developing phase transformation models applicable to industrial cooling conditions. These
models typically assume a sequential formation of the different transformation products: (1) ferrite, (2) pearlite, (3) bainite, and
(4) martensite. The Johnson-Mehl-Avrami-Kolmogorov (JMAK) model is commonly employed to describe ferrite, pearlite, and
bainite formation kinetics, as seen in (74–76)
& '
X ¼ 1 ' exp 'bt k [15]
in the case of isothermal transformation where X represents the fraction transformed, t is time, b is a rate parameter, and k the JMAK
exponent. Usually, k can be taken as independent of temperature. Tamura et al. (3) proposed the following nominal values: k ¼ 1 for
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Figure 21 Effect of Nb in solution on austenite decomposition in a 0.06 wt.% C–1.65 wt.% Mn–0.034 wt.% Nb–0.012 wt.% Ti–0.24 wt.% Mo 550 MPa
steel cooled at 5 * C s'1 from a prior austenite grain size of 5 mm.
ferrite, k ¼ 4 for pearlite, and k ¼ 4 for bainite. Because of the wide range of different bainitic transformation products, different
k-values for bainite have been reported ranging from 1 to 7 (27). The parameter b can be written as (3,27)
b0 ðTÞ
b¼ [16]
dm
eff
where b0 is a function of temperature, deff is the effective austenite grain size, and m the grain size exponent. The effective grain size is
introduced to account for the effect of work-hardened austenite on transformation, that is, deff ¼ dg exp('εa), where εa is the strain
accumulated due to partial or no recrystallization in the finishing stands (77). Here, m and the function b0 depend on steel chemistry
and are usually determined from transformation experiments. In practice, austenite decomposition occurs during cooling, and the
JMAK theory is combined with the additivity principle to account for these nonisothermal conditions; this approach is valid as long
as the JMAK exponent, k, is a constant. Then, the fraction transformed during continuous cooling can be obtained from (3)
8 0 T 1k 9
< Zs
1 @ b0 ðTÞ1=k A =
X ¼ 1 ' exp ' m dt [17]
: deff fðTÞ ;
T
where f ¼ dT/dt is the instantaneous cooling rate and Ts is the transformation start temperature.
To describe the beginning of the transformation, classical nucleation theory can be employed. However, the lack of detailed
nucleation information, as well as the realization that a measurable transformation start (e.g., 5% transformed) requires some
initial growth of the ferrite nuclei, has led to an alternative transformation start model that considers carbon diffusion-controlled
early growth of ferrite nucleated at temperature TN on grain corners to describe the ferrite transformation start temperature, Ts (78).
Measurable transformation start is assumed to coincide with nucleation site saturation, that is, the formation of a ferrite film along
prior austenite grain boundaries. In the model, this situation is depicted by carbon enrichment at the austenite boundaries that
attains a critical level, c*, above which ferrite nucleation is inhibited. This approach provides a satisfactory description of the
transformation start during continuous cooling by using TN and c* as adjustable parameters. This model has recently been extended
to include the effect of Nb in solution on delaying ferrite start by introducing a suitable solute drag term with another adjustable
parameter (79). The transformation start model is a crucial component of transformation models since the ferrite grain size is
essentially determined by Ts, that is, (22)
da ¼ ðF expðB ' E=Ts ÞÞ1=3 [18]

where F is the ferrite fraction and B and E are steel-specific parameters. An important practical implication of this finding is that to
maximize ferrite grain refinement in ferrite-pearlite steels, ACC has to be employed to decrease Ts as much as possible. The
remaining transformation may subsequently occur during slower cooling, and this will also ensure that a ferrite-pearlite micro-
structure is formed.
The cessation of ferrite formation can be related to a sufficiently slow-moving austenite-ferrite interface such that pearlite
nucleation becomes possible at this interface. In the case of ferrite-bainite steels, attaining a critical driving pressure (free energy
difference between ferrite and remaining austenite) provides the condition for bainite start (and thus ferrite stop) (80). Finally,
upon reaching the martensite start temperature, MS, the remaining austenite transforms to martensite. The martensite start
temperature is typically expressed as a function of steel chemistry, but it is important to note that it is the composition of the
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reaming austenite that determines MS, and that the carbon enrichment of austenite due to the preceding ferrite formation must be
accounted for. Other factors, such as the size of the remaining austenite grains, may also affect the stability of austenite against the
martensite transformation (81).
The above delineated model approach is semiempirical in nature and requires the determination of a number of parameters
from CCT tests. As a result, there are challenges in developing transformation models with predictive capabilities for a wide range of
steel chemistries, in particular to accurately quantify the role of substitutional alloying elements (such as Nb, V, Ti, Mo, Si, and Cr)
and their potential combinations, which are increasingly being considered in TMCP steels. These alloying elements delay the
austenite decomposition primarily by a solute drag mechanism on the moving austenite–ferrite interface.
Fundamental transformation models have been developed for low-carbon steels. During the formation of ferrite, interstitial
carbon is rejected from ferrite and enriched in remaining austenite, whereas during industrial cooling conditions, there is no long-
range redistribution of substitutional alloying elements because of their comparatively slow diffusion. In Fe–C alloys with a higher
carbon content (>0.2 wt.%), ferrite formation is controlled by carbon diffusion in austenite and can be predicted by diffusion
models (82–84). When the carbon content is lowered below 0.2 wt.%, the transformation increasingly assumes a mixed-mode
character (85) (the reaction is determined by both long-range carbon diffusion and the interface reaction that is described with
an interface mobility according to eqn [14] introduced above for grain boundary motion during recrystallization). There is a great
deal of uncertainty regarding the value of this mobility, as even in model Fe–C alloys residual solutes may affect the apparent
interface mobility. In low-carbon steels, the mobility is indeed an effective quantity that is affected by solute drag of the alloying
elements. The quantification of the role of alloying elements on migrating interfaces is currently subject to extensive dedicated
studies combining experimental and modeling approaches, including advanced experimental tools with atomistic resolution (i.e.,
atom probe tomography) and atomistic simulations (86).
1.10.4.4 Precipitation Strengthening

Microalloying additions can provide substantial precipitation strength in classical HSLA steels with ferrite-pearlite microstructures
(22,23,30). This strength component is typically realized when the precipitates form in ferrite during coiling or, in the case of plates
during slow cooling, below the cooling stop temperature. As the solubility of the microalloying elements is extremely low in ferrite
(on the order of a few ppm or even less), the precipitation strength potential becomes independent of temperature and is deter-
mined by the amounts of these elements that remain in solution in the ferrite matrix, that is, all V added to the steel, Nb that is not
consumed by strain-induced precipitation in austenite, and excess Ti that is not precipitated in form of TiN. Coiling and cooling stop
temperatures, respectively, must be carefully selected to fully realize the precipitation potential by forming a dense population of
carbides (or carbonitrides in steels that are either not microalloyed with Ti or contain an insufficient amount Ti to scavenge all N)
(22,23,29). The diffusion of the microalloying elements that form the precipitates is the rate-controlling step.
The situation is comparatively straightforward when the precipitation process is dominated by a single microalloying element.
V(C,N), Nb(C,N), or TiC provide precipitation strength in singly microalloyed steels. In multimicroalloyed steels, more complex
precipitates, such as (Ti,Nb)(C,N), can form, and may modify the precipitation kinetics in detail. Overall, however, robust pro-
cessing windows can be designed to attain precipitation strength in all HSLA steels. Figure 22 provides an example for the prediction
Figure 22 Calculated normalized precipitation strength as a function of coiling temperature assuming coil cooling at 30 * C h'1. Reproduced from
Militzer, M.; Hawbolt, E. B.; Meadowcroft, T. R. Microstructural Model for Hot Strip Rolling of High-Strength Low-Alloy Steels. Metall. Mater. Trans. 2000,
31A (4), 1247–1259.
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of relative precipitation strength as a function of coiling temperature in Nb- and V-microalloyed steels, respectively. To attain at least
90% of the maximum precipitation strength, coiling temperatures between 550 and 650 * C can be employed for Nb steels, and this
range is about 600–700 * C for V steels. The absolute amount of precipitation strength increases with microalloying content, but
saturation limits have been observed for Nb in particular. That is, an addition above about 0.06 wt.% Nb does not lead to further
increases in precipitation strength.
The role of precipitation strength is reduced in steels with highly dislocated irregular ferrite and/or bainitic ferrite (87). Because of
the nonlinear addition law of precipitation and dislocation strengthening (see eqn [5]), the effect of precipitates on strength can be
greatly reduced when dislocation strength becomes larger than the contribution from precipitates. Then, the role of Nb, for example,
is to facilitate increased strength due to microstructure refinement and dislocation strengthening (i.e., transformation hardening).
Precipitation can also occur during the austenite-to-ferrite transformation when cooling conditions are carefully controlled and
steel chemistries are tailored such that the noses of the precipitation and austenite-ferrite transformation curves almost overlap
(53,88). Reactions of this type are known as interphase precipitation where the precipitates nucleate on the moving austenite-ferrite
interface. The possibility to use this strengthening approach industrially had been demonstrated for TiC precipitation in steels
containing 0.07 wt.% C and 0.05–0.12 wt.% Ti, for example, in (89). In this scenario, almost all C is consumed by the precipitation
reaction such that no C enrichment of austenite occurs, thereby preventing the formation of pearlite, bainite, and martensite. In this
way, a precipitation-hardened ferrite microstructure can be obtained. By refining the interphase precipitation approach, a yield stress
of up to 780 MPa has been achieved in Ti- and Mo-bearing HSLA sheet steels with nanometer-sized complex (Ti,Mo)C precipitates
in the ferritic matrix (89). These steels are known by the trade name Nanohiten.
1.10.5 Summary and Outlook

1.10.5.1 Summary on the Role of Nb Microalloying
It is of interest to investigate why Nb, but not other typical alloying elements, shows this extraordinary behavior in iron and steel
that is at the core of TMCP steels. Niobium was discovered in 1801 by Charles Hatchett (90), a Fellow of the Royal Society, who
named it columbium, a name that some steelmakers occasionally still use today. It was not until 1844 that Nb could be clearly
distinguished from tantalum (Ta), when the German chemist Heinrich Rose identified subtle differences in the valence states of
both elements. Rose changed the element’s name appropriately to niobium (91). According to Greek mythology, Niobe was
a daughter of Tantalus, king of Sipylus. The beneficial role that Nb played in C–Mn steels was found as early as the late 1930s; two
decades before its first commercial use as a microalloying element (92). Meanwhile, advanced experimental and modeling tech-
niques have been employed to investigate and quantify the role of Nb in steel from a fundamental perspective. In general, Nb has
a strong tendency to be associated with defects like vacancies, dislocations, and grain boundaries. By using the Vienna Ab initio
Simulation Package (VASP) (93,94) and density functional theory (DFT), calculations have recently been performed to determine
the binding energies of commonly employed alloying elements to vacancies and a S5 grain boundary in BCC–Fe. These calculations
confirm the strong interaction of Nb with these crystalline defects in iron. The binding energies are approximately 0.4 eV (1 eV per
atom ¼ 96.5 kJ mol'1) with vacancies and the S5 grain boundary, respectively. There are three different boundary sites in this
special boundary, and Figure 23 depicts the average binding energy for a given solute as a function of its atomic volume in the bulk
Fe matrix. The binding energies increase with atomic volume. Out of the considered elements, Nb has the largest atomic volume
when as a solute atom on a regular lattice site in BCC–Fe, and this translates into the largest binding energy to the grain boundary by
far (0.4 eV as compared to 0.3 eV for Ti and Mo). These quantum-mechanical calculations are consistent with the enormous effect of
Nb in delaying recrystallization. The strong grain boundary segregation of Nb significantly reduces boundary migration rates due to
solute drag.
0.5
Nb
0.4
Binding energy, eV
Mo
0.3 Ti
Ni Cu
0.2
Mn Cr
V
0.1 Si
Co
0.0
7.4 7.6 7.8 8.0 8.2 8.4 8.6 8.8
–30 3
Solute volume, 10 m
Figure 23 Binding energies of solutes to the S5 grain boundary in BCC–Fe as obtained from DFT simulations.
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Further, the comparatively large binding energy of Nb with a vacancy – only boron is known to have a stronger binding energy
with vacancies in iron (95) – provides evidence to rationalize its potential for strain-induced precipitation. Nb-vacancy complexes
form, and because of excess vacancies generated by deformation, there are also excess Nb-vacancy complexes. These complexes
travel to vacancy sinks (dislocations and grain boundaries) where the excess vacancy is annihilated, leaving the solute Nb in its
vicinity. This is thought to promote strain-induced precipitation in a plate or Steckel mill.
1.10.5.2 Recent Developments in TMCP Steels and Future Trends

TMCP steels are well established as cost-effective, high-quality steel products. There will be increased demand for these steels in the
future, including further improved property requirements. For example, world energy consumption is projected to increase by 50%
in 2035 from current consumption levels (96). A major contribution of this increase will come from natural gas. Further, alternative
energy supplies, such as wind energy, are expected to see significant growth over the next two decades. Advanced steel plates that are
technically feasible and economically viable are required to complete the necessary energy infrastructure expansion (such as natural
gas pipeline projects). Similarly, there will be an increased demand for TMCP plates in other structural applications, including high-
rise buildings and bridges, as well as shipbuilding (17). The design yield stress specifications are expected to increase from the
current 400–500 MPa range to at least 700 MPa for the most advanced steels (with good toughness and weldability) used in
building structures. For example, new bridge high-performance steels were recently specified in Japan, with a minimum yield stress
of 500 and 700 MPa, respectively. It is important to note that, in addition to yield stress, improved fracture toughness is increasingly
becoming a critical design criterion in building constructions that are safe and reliable, particularly in seismically active areas. There
are also new challenges associated with supplying steel plates for shipbuilding. To build the next generation of mega-container
ships, high-strength steel plates are needed with increased plate thickness and excellent brittle-crack arrestability.
Welding is a critical aspect of the construction of pipelines, ships, bridges, buildings, and other civil engineering applications.
New high-productivity welding procedures are currently being introduced (including dual-torch and laser-hybrid welding).
Ultrahigh-heat input (up to 1300 kJ cm'1) welding technologies have been increasingly employed to reduce the construction costs
of steel structures. Thus, it is crucial that new steels be developed that maintain the required HAZ fracture toughness when using
advanced welding techniques. Here, TMCP steels have a clear advantage over conventional steels with the same strength levels. The
lower carbon content of these TMCP steels leads to better weldability.
A major concern in welding is the coarse-grained HAZ immediately at the fusion line. There are two metallurgical approaches to
control the microstructure: (1) limit austenite grain growth and (2) introduce intragranular ferrite nucleation sites. So far, TiN has
been used primarily for limiting austenite grain growth. New concepts, however, have to be introduced to control the HAZ
microstructure for high and ultrahigh-heat input welding as TiN particles will coarsen under these conditions, thereby reducing their
pinning efficiency on grain growth. The oxide metallurgy may provide attractive alternatives (97). For example, it has been
established for some time that Ti oxides and other large precipitates (including coarse TiN) facilitate intragranular ferrite nucleation
to form acicular ferrite. The oxides may not provide the nucleation sites per se, but coprecipitation with MnS and TiN, for example,
has been reported to lead to ferrite nucleation. More recently, it has been found that a number of oxides and sulphides containing
Ca, Mg, and/or rare earths not only provide suitable ferrite nucleation sites, but are also thermally more stable than TiN to efficiently
pin austenite grain boundaries (97). Thus, it has been possible to develop a new class of supertough steels by combining austenite
grain growth control with intragranular ferrite formation in the HAZ, that is, the so-called HTUFF steels (17). The absorbed energy in
Charpy fracture tests of these steels is about a factor of two larger than that in TiN steels and exceeds 70 J (in the 0–40 * C temperature
range), which is the new standard for building construction in seismic active areas, as concluded by analyzing data from the
catastrophic Hanshin-Awaji Earthquake (1995) in Japan (98).
Other advances in TMCP steels include the combination of ACC with a subsequent online heat-treatment step. This technology
was introduced by JFE Steel in 2004 by installing an online induction heating facility, HOP" (Heat treatment Online Process) in
their Fukuyama plate mill (21). As a result, the so-called direct quenching and HOP process (DQ-HOP) was introduced as an
alternative to the conventional direct quenching and tempering (DQ-T) to manufacture high-strength steels. Both processes are
compared in Figure 24. In the conventional DQ-T process, the steel is rapidly cooled (quenched) in the mill to ambient
temperatures and then heat-treated (tempered) offline. In the DQ-HOP process, quenching and tempering are conducted online in
the rolling mill. The combination with the Super-OLAC cooling system enables accurate control of the stop-cooling temperature
before tempering. As a result, this processing route offers tremendous opportunities for microstructure control that are unachievable
with either the conventional DQ-T or conventional TMCP processes. The DQ-HOP process has already been demonstrated to
control the size and morphology of cementite precipitates and martensite-austenite constituents such that, for example, TMCP steels
can be manufactured that combine high strength with superior toughness.
Significant research efforts have recently been made to develop processing routes for ultrafine-grained steels, in which the use of
costly alloying elements is dramatically reduced (63,99,100). A number of processing routes were evaluated for this purpose,
primarily by using laboratory simulations. For example, the novel technique of deformation-induced ferrite transformation (DIFT)
(also known as strain-induced transformation or SIT), dynamic strain-induced transformation, strain-induced dynamic trans-
formation, and strain-assisted transformation, provide the potential to produce an ultrafine ferrite (UFF) structure with grain sizes
that typically fall into the 1 mm range. The DIFT processing is based on quickly cooling austenite just above the transformation start
temperature that would be associated with this cooling condition. Heavy deformation of the severely undercooled, metastable
austenite leads to the formation of UFF. An important advantage of this technique is that it can, at least in principle, be applied to
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Figure 24 Comparison of (a) conventional direct quenching and tempering (DQ-T) with (b) direct quenching (DQ) and HOP (Heat treatment Online
Process).
sheet steel production. Yada et al. (101) had already claimed in the 1980s to have used this technique to produce hot-rolled coils
with a ferrite grain size of approximately 1 mm. Recently, Morimoto et al. (102) reported industrial production of fine-grained plain-
carbon steel strips with ferrite grain sizes of 2–5 mm that can be attributed to DIFT, which was initiated in the final stands of a seven-
stand finish mill by a combination of asymmetric rolling and proper interstand cooling.
Another intriguing example where TMCP may lead to breakthroughs is related to high-quality electrical steels. This example is
selected here to illustrate the potential breadth of the TMCP concept. The primary goal in the production of electrical steels is an
improvement in the magnetic properties (i.e., magnetostriction and hysteresis losses) rather than the mechanical properties, which
were the focus of the TMCP steels discussed in this chapter. As a matter of fact, low-carbon steels can be processed as low-cost
electrical steel grades. However, high-end electrical steels, such as those used for transformer sheets, are a separate steel family that is
based on a Fe-3 wt.% Si alloying concept with ultralow-carbon levels. These steels are ferritic at all processing temperatures in the
solid state (i.e., the austenite-ferrite transformation is absent to potentially manipulate properties) and can be thermomechanically
controlled-rolled, even though the presence of Si leads to significant challenges (such as the formation of an oxide layer prior to hot
rolling). The magnetic properties of these steels could be further improved if it were feasible to increase the Si alloying level;
magnetostriction becomes zero for 6.5 wt.% Si. However, when the Si content is increased, the material becomes extremely brittle,
making it virtually impossible to produce it by rolling. Nevertheless, laboratory investigations have recently been reported that
indicate that the development of new rolling procedures may be possible in order to mitigate these problems (103,104).
The above examples illustrate the potential and viability of the TMCP approach as a cost-effective processing route to fabricate
advanced steel products for a wide range of applications. Further advances in TMCP technology are imminent and will lead to
improved steel products that will be critical for sustainable economic growth worldwide in the foreseeable future.
See also: Advanced High Strength Bainitic Steels; Structure and Mechanical Properties of High-Manganese Steels; Hot Rolling and
Direct Cooling; Introduction to Steel Heat Treatment; Metallo-Thermo-Mechanical Coupling in Quenching; Austenite Formation and
Microstructural Control in Low-Alloy Steels.
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COMPREHENSIVE MATERIALS

Gilmar Ferreira Batalha

ASSESSING PROPERTIES OF CONVENTIONAL

Chester J. Van Tyne

AMSTERDAM • BOSTON • HEIDELBERG • LONDON • NEW YORK • OXFORD

British Library Cataloguing in Publication Data

Library of Congress Cataloging-in-Publication Data

For information on all Elsevier publications

Printed and bound in Italy

Project Manager: Gemma Tomalin

Joseph A. McGeough is an honorary professorial fellow in the School of Engineering at the

Syed H. Masood is professor of Mechanical and Manufacturing Engineering at Swinburne

Mustaﬁzur Rahman is currently a professor at the Department of Mechanical Engineering at

M. Vu!ceti"c M.J. Worswick

1.01 Introduction to Assessing Properties of Conventional and Specialized Materials 1

Volume 1 Assessing Properties of Conventional and Specialized Materials

Volume 2 Materials Modeling and Characterization

2.04 Ultrasonic Characterization of Anisotropic Materials

Volume 3 Advanced Forming Technologies

3.11 Improvement of Mechanical and Physical Properties in Powder Metallurgy

Volume 4 Films and Coatings: Technology and Recent Development

4.15 Advanced Carbon-Based Coatings

Volume 5 Casting, Semi-Solid Forming and Hot Metal Forming

5.14 Hot Forging

Volume 6 Welding and Bonding Technologies

6.14 Bonding Technologies in Manufacturing Engineering

Volume 7 Nano- and Microscale Processing e Modeling

Volume 8 Health, Safety and Environmental Issues

Volume 9 Laser Machining and Surface Treatment

Volume 10 Advances in Additive Manufacturing and Tooling

Volume 11 Advanced Machining Technologies

Volume 12 Thermal Engineering of Steel Alloy Systems

12.08 Residual Stresses Produced by Quenching of Martensitic Steels

Volume 13 Sensor Materials, Technologies and Applications

Comprehensive Materials Processing, Volume 1 http://dx.doi.org/10.1016/B978-0-08-096532-1.00100-X 1

Comprehensive Materials Processing, Volume 1 http://dx.doi.org/10.1016/B978-0-08-096532-1.00124-2 3

Figure 1 Classiﬁcation of advanced ceramics based on their applications.

1.02.2 Evaluation of Microstructural, Chemical, and Physical Properties

Figure 2 Different forms of advanced ceramics used in technical applications.

1.02.2.2 Crystal Structure

Figure 6 Schematic diagram of an X-ray diffraction system.

Figure 8 Schematic diagram of Raman spectroscopy system.

1.02.2.3 Chemical Composition

1.02.2.4 Size and Shape of Ceramic Powder

Valence band Valence band

Ground State Ejection of Photoelectron

Figure 12 EDX spectra of a ceramic TiAlN coating.

1.02.2.5 Density, Surface Area, and Porosity

Figure 15 A ceramic block made from compaction of ceramic powder.

1.02.2.6 Ceramic Coating Thickness

1.02.3 Evaluation of Mechanical Properties

1.02.3.1.3 Ultrasonic Measurement Technique

1.02.3.2 Fracture Toughness

Figure 20 Nanoindentation of TiAlSiN coating.

1.02.3.2.1 Crack Length Measurement Method

Figure 21 Vickers indentation with radial cracks from the corner.

1.02.3.2.2 Rockwell C and Vickers Indentations

1.02.3.3 Edge Toughness

Figure 23 Rockwell C setup for the toughness measurement of ceramic coating.

1.02.4 Evaluation of Tribological Properties

Figure 26 Arrangement of pin-on-disk for wear testing and wear proﬁle.

1.02.5 Evaluation of Thermal Properties

1.02.5.1 Thermal Expansion