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metallurgy
W. Frazier
K. Kulkarni, FAPMI
K.S. Kumar
T.F. Murphy
J.W. Newkirk
P.D. Nurthen
J.H. Perepezko
P.K. Samal
H.I. Sanderow
D.W. Smith, FAPMI
R. Tandon
T.A. Tomlin
D.T. Whychell, Sr., FAPMI
Contents 44/1 January/February 2008
M. Wright, PMT
A. Zavaliangos
2 Editor's Note
INTERNATIONAL LIAISON COMMITTEE 5 PM Industry News in Review
D. Whittaker (UK) Chairman 7 PMT Spotlight On … David Rector
V. Arnhold (Germany)
E.C. Barba (Mexico) 9 Consultants’ Corner James G. Marsden, FAPMI
P. Beiss (Germany)
C. Blais (Canada) GLOBAL REVIEW
P. Blanchard (France)
G.F. Bocchini (Italy)
15 Powder Metallurgy in Italy
F. Chagnon (Canada) O. Morandi and E. Mosca
C-L Chu (Taiwan)
H. Danninger (Austria) RESEARCH & DEVELOPMENT
U. Engström (Sweden)
N.O. Grinder (Sweden) 22 Effect of Die Filling on Powder Compaction
S. Guo (China) D. Korachkin, D.T. Gethin, R.W. Lewis and J.H. Tweed
F-L Han (China)
K.S. Hwang (Taiwan) 35 High-Density Inconel 718: Three-Dimensional Printing
Y.D. Kim (Korea) Coupled with Hot Isostatic Pressing
G. Kneringer (Austria)
G. L’Espérance, FAPMI (Canada)
J. Sicre-Artalejo, F. Petzoldt, M. Campos and J.M. Torralba
H. Miura (Japan)
C.B. Molins (Spain) ENGINEERING & TECHNOLOGY
R.L. Orban (Romania) 44 Economics of Processing Nanoscale Powders
T.L. Pecanha (Brazil)
F. Petzoldt (Germany) J.L. Johnson
S. Saritas (Turkey)
G.B. Schaffer (Australia) OUTSTANDING TECHNICAL PAPER FROM POWDERMET2007
Y. Takeda (Japan)
G.S. Upadhyaya (India) 55 Close-Coupled Gas Atomization: High-Frame-Rate
Analysis of Spray-Cone Geometry
Publisher
C. James Trombino, CAE A.M. Mullis, N.J.E. Adkins, Z. Aslam, I. McCarthy and R.F. Cochrane
jtrombino@mpif.org
Editor-in-Chief DEPARTMENTS
Alan Lawley, FAPMI 65 Web Site Directory
alan.lawley@drexel.edu
Managing Editor
78 Meetings and Conferences
Peter K. Johnson 79 APMI Membership Application
pjohnson@mpif.org 80 Advertisers’ Index
Advertising Manager
Jessica S. Tamasi Cover: Award of Distinction–winning parts from MPIF’s 2007 Design
jtamasi@mpif.org Excellence Awards Competition
Copy Editor
Donni Magid The International Journal of Powder Metallurgy (ISSN No. 0888-7462) is a professional publication serving the scientific and tech-
dmagid@mpif.org nological needs and interests of the powder metallurgist and the metal powder producing and consuming industries. Advertising
carried in the Journal is selected so as to meet these needs and interests. Unrelated advertising cannot be accepted.
Production Assistant Published bimonthly by APMI International, 105 College Road East, Princeton, N.J. 08540-6692 USA. Telephone (609) 452-
Dora Schember 7700. Periodical postage paid at Princeton, New Jersey, and at additional mailing offices. Copyright © 2008 by APMI International.
dschember@mpif.org Subscription rates to non-members; USA, Canada and Mexico: $95.00 individuals, $220.00 institutions; overseas: additional
$40.00 postage; single issues $50.00. Printed in USA by Cadmus Communications Corporation, P.O. Box 27367, Richmond,
President of APMI International Virginia 23261-7367. Postmaster send address changes to the International Journal of Powder Metallurgy, 105 College Road East,
Nicholas T. Mares Princeton, New Jersey 08540 USA USPS#267-120
ntmares@asbury.com
ADVERTISING INFORMATION
Executive Director/CEO, APMI International Jessica Tamasi, APMI International
C. James Trombino, CAE 105 College Road East, Princeton, New Jersey 08540-6692 USA INTERNATIONAL
EDITOR’S NOTE
N
ow in its 15th year, the MPIF Outstanding Technical Paper award recognizes
excellence in scientific/technical content and written communication.
Selected from the PowderMet2007 technical program, the recipients are
from the University of Leeds and CERAM Research in the UK. Their collaborative
study of close-coupled gas atomization, utilizing high-speed digital imaging to
monitor and analyze the spray-cone geometry, establishes an improved
understanding of the complex interactions between the gas and liquid-metal
stream in atomization.
In recognition of 2008 as a “World Congress” year, the Journal will publish a
number of global PM reviews. The first of these, prepared by Morandi and Mosca,
highlights the characteristics, history, and evolution of the PM industry in Italy,
including a perspective on the future.
There are two R&D contributions to this issue of the Journal. Korachkin et al.
describe a numerical simulation study of the effect of variations in die-fill density
Alan Lawley
on the final green-density distribution in a pressed part, and the attendant effect Editor-in-Chief
on tool stresses—both of prime importance to PM parts manufacturers. In the
other study, Sicre-Artalejo et al. assess the feasibility of fabricating high-density
parts from Inconel 718 powder utilizing three-dimensional printing. It is
demonstrated that full density can be achieved by sintering and hot isostatic
pressing of the printed parts.
In the “Engineering & Technology” section, Johnson extends the sintering and
property models for nanoscale tungsten to other nanoscale metal and ceramic
powders in order to explore processing economics. His analysis, based on
cost normalizing of properties, leads to the conclusion that the incremental
improvement in performance, compared with that of conventional metal and
ceramic powders, does not compensate for their higher cost. Usage of nanoscale
powders in “press and sinter” processing mandates a lower powder cost and/or
enhanced property performance.
Returning to the “Consultants’ Corner,” Jim Marsden provides counsel on
readers’ questions on sintering practice. In particular, his responses focus on the
importance of the furnace presinter temperature profile in the delubrication of PM
parts, and on-site generation of nitrogen–hydrogen sintering atmospheres.
First published in 2001, the PM Web Site Directory continues to expand as
e-business has become integral to the industry. This year’s directory classifies
company entries by equipment manufacturers, metal powder producers,
MIM/PIM, and others which includes PM consultants.
North Carolina
Suzhou
USA
China
Manufacturing Sites
• Research Triangle Park, North Carolina USA
• Suzhou, China
Tel: 919-544-8090 • www.SCMmetals.com
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gress
rld Con
PM Wo , 2008
2
June 8-1 30
4
Booth # n D.C.
gto
Washin
www.arburg.com
ARBURG GmbH + Co KG
Postfach 11 09 · 72286 Lossburg/Germany
Tel.: +49 (0) 74 46 33-0
Fax: +49 (0) 74 46 33 33 65
e-mail: pim@arburg.com
ARBURG, Inc. · 125 Rockwell Road · Newington, CT 06111 · Tel.: +1 (860) 667 6500 · Fax: +1 (860) 667 6522 · e-mail: usa@arburg.com
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PM INDUSTRY
NEWS IN REVIEW
The following items have appeared in PM Newsbytes since the previous
issue of the Journal. To read a fuller treatment of any of these items, go
to www.apmiinternational.org, login to the “Members Only” section, and
click on “Expanded Stories from PM Newsbytes.”
H.C. Starck Signs Tantalum new award recognizing lifetime Chapter 11 bankruptcy on
Supply Contract achievements in the PM indus- December 27, 2007. The compa-
H.C. Starck GmbH, Goslar, try. The new Kempton H. Roll ny makes a wide variety of auto-
Germany, has signed a 10-year PM Lifetime Achievement Award motive products as well as PM
contract to purchase 600,000 will serve as MPIF's highest-level parts and products in plants in
pounds of tantalum raw materi- individual award, expected to be the U.S., the UK, France, and
als annually from Tantalum presented every four years to one India.
Egypt JSC, which holds the min- individual, beginning next year
ing rights for the Abu Dabbab at the PM2008 World Congress GKN Updates 2007 Results
exploration area in Egypt. The in Washington. GKN plc, London, UK, reports
contract expands Starck’s raw profits for the first 11 months of
materials base for the metal as Austrian PM Company Gains 2007 show a solid improvement
well as supporting its long-term Miba AG, Laakirchen, Austria, over the same period in 2006
involvement in the tantalum reported sales of 286.8 millions with its Driveline, Aerospace,
market. euros, a three percent gain, for and OffHighway segments all
the first three quarters of its fis- ahead. Its powder metallurgy
New MPIF Lifetime cal year. After adjusting for lost business dipped marginally
Achievement Award Honors revenues resulting from the sale below 2006 due to higher raw
Founding Executive Director of PM plants in Italy and Spain, material costs in the second half
The Board of Governors of the the increase was 14 percent. of 2007 and some operational
Metal Powder Industries disruption stemming from
Federation (MPIF) has accepted a Federal-Mogul Exits Bankruptcy restructuring. ijpm
recommendation by the MPIF Federal-Mogul Corp. (FMC),
Awards Committee to establish a Southfield, Mich., emerged from
SPOTLIGHT ON ...
DAVID RECTOR
Education: What gives you the most satisfaction in your career?
Columbia Basin Community College New projects. I enjoy the challenge of R&D.
Why did you study powder metallurgy/particulate List your MPIF/APMI activities.
materials? Unfortunately, living in the Pacific Northwest,
My great uncle, John Rector, founded Western Sintering MPIF/APMI activities are limited.
Co. (WSC), so I grew up in the PM industry. I have spent
a high percentage of my life around presses and fur- What major changes/trend(s) in the PM industry
naces. have you seen?
The biggest change I have seen is globalization. The per-
When did your interest in engineering/ centage of “American made” products that contain parts
science begin? manufactured overseas has increased
I was the kid who begged his mother to dramatically since I became familiar
buy him a 50¢ toaster at the neighbor’s with the PM industry.
garage sale, so he could take it apart
Why did you choose to pursue PMT
and figure out how it worked.
certification?
I did not finish college. PMT certification
What was your first job in PM? What
allowed me to prove that I was compe-
did you do?
tent and knowledgeable in my chosen
I remember tapping PM parts while my
field.
father worked on the furnaces during
the weekend when I was 5 or 6 years How have you benefited from PMT
old certification in your career?
I learned about several processes of
Describe your career path, companies worked for, which I previously lacked knowledge, despite growing up
and responsibilities. with iron powder behind my ears. PMT certification
I have worked at WSC most of my life. I started walking allowed me to prove my abilities in the field.
to the plant after school when I was 12 years old in
order to work in the shipping department. When I What are your current interests, hobbies, and
turned 18 I came to work full time in the shipping/ activities outside of work?
receiving department. I boxed parts, worked in the ware- I spend my summers wakeboarding and wakesurfing on
house, and set up pallets for shipment. At age 23 I the Columbia River. In winter you will find me on a
moved into the press shop, blended powder, and set up mountain snowboarding. In my free time I read vora-
tools in both mechanical and hydraulic presses. Most of ciously, play chess, shoot pool, and occasionally substi-
my time was spent as an operator. I took and passed the tute as a goalkeeper on a local recreational league
PMT I examination at age 24. I also attempted the PMT soccer team.
II examination two years later, but did not pass. I have
not retaken the test as it has not been offered since. Manager, Sintering Operations
Western Sintering Co Inc
After about five years I moved into the sintering depart- 2620 Stevens Drive
ment and have been managing the operation for over a Richland, Washington 99354-1752
year now. I am in charge of new procedures, sintering Phone: (509) 375-3096
R&D, basic maintenance, and scheduling. Fax: (509) 375-3594
Email: DRector@westernsintering.com
CONSULTANTS’
CORNER
*Consultant, Furnace & Atmosphere Service Technology, Inc. (F.A.S.T., Inc.), P.O. Box 43, Big Run, Pennsylvania 15715-0043,
USA; Phone: 814-427-2228; E-mail: jgmars@verizon.net
CONSULTANTS’ CORNER
E-Mail:
info@cmfurnaces.com FURNACES INC.
Web Site: 103 Dewey Street Bloomfield, NJ 07003-4237
http://www.cmfurnaces.com Tel: 973-338-6500 Fax: 973-338-1625
CONSULTANTS’ CORNER
minimum usage of 171 ML (6 M ft.3) per month of residential area. Any further improvement in puri-
nitrogen to be economical. The units are usually ty requires the use of hydrogen in a deoxidation
installed and maintained under a long term con- stage with subsequent drying to produce oxygen
tract (usually 15 years) with the industrial-gas levels in the range 2 to 5 ppm.
supplier. Thus, it is prudent to be cognizant of The liquid nitrogen–assist generator uses liquid
long-term projected growth, and the ability of the nitrogen supplied from an on-site vessel to provide
unit to supply projected needs in the future. refrigeration “assist” in the cryogenic separation
The PSA unit has a purity of approximately 99.9 process that separates nitrogen from the atmos-
v/o. The unit may require that it be housed in an phere. Previous cryogenic separation technology
enclosure which would require a dedicated build- for nitrogen utilized a turbine expander to provide
ing or floor space in the manufacturing facility. this refrigeration. As with the PSA, air is filtered,
The unit is comprised of two large separation ves- compressed, and further treated to remove
sels that reduce the air, under pressure, by utiliz- unwanted components (oil and water). The com-
ing a carbon molecular sieve material. In the pressed air is cooled and then enters the cryogenic
process, air is filtered, compressed, and further air separation column where it is distilled into its
treated to remove unwanted components (air and components, including nitrogen (99.999 v/o puri-
water). The compressed air then enters a vessel ty) which is removed from the cold box and deliv-
which contains the carbon molecular sieve materi- ered to the customer by pipeline. The unit
al which absorbs the oxygen and CO2 and allows a produces oxygen levels in the range 2 to 5 ppm
nitrogen-rich stream to pass through the vessel without additional accessories. It is usually located
and be delivered to the customer by pipeline. One outside of the facility, and does not need a special
vessel takes in air while the other vessel is depres- enclosure.
surizing. This switching action results in a noisy There are other smaller, lower-volume nitrogen-
system, a minor limitation unless it is located in a generation units for rent and/or sale, such as the
W !
NE F ro m B o h l e r - U d d e h o l m
V
VAA N A D
NADIS I S 4 E X T
EXTRA R
VA N A D I S 4 E X T R AA ¤¤
CONSULTANTS’ CORNER
ijpm
THIS JUNE
THE PM WORLD
CONVENES IN
WASHINGTON, D.C.
• International
Technical Program
• Worldwide Trade Exhibition
• Special Events
This global PM event is sponsored by:
In cooperation with:
GLOBAL REVIEW
This review of the status of
powder metallurgy (PM) in
Italy covers all aspects that
INTRODUCTION
In relation to structural parts, PM in Italy has a long and successful
history. Examples include innovation in the design of components
(Olivetti, split-die principle, and the development of presses to handle
special tool sets); improvement of processes to fabricate unusual
shapes with attractive properties; and the ability to cater to markets
outside the automotive sector. The novelty of the solutions included in
some of Italy’s PM products has resulted in international recognition.
Over the years Italian PM companies have won three Grand Prizes and
nine Awards of Distinction in the International Design Competition
sponsored by the Metal Powder Industries Federation (MPIF).
Today, the evolution of the Italian PM industry is oriented primarily
towards a strengthening of its traditional products, since there
remains room for growth of these markets, especially in relation to
structural components for mechanical applications. It is here that PM
is frequently gaining success at the expense of other metal-shaping
processes.
There are attendant problems since PM technology is relatively
mature, and some components that in the past made a substantial
contribution to the domestic output are now manufactured at produc-
tion sites located in countries with low-cost manpower. For example,
this is the case for PM refrigerator compressors parts, whose produc-
tion in Italy has experienced a precipitous decline, dating back to the
1990s.
In this Global Review, the primary characteristics, history, and evo-
lution of the Italian PM industry are described. The review illustrates
the development of the technology and related activities, including a
perspective on the future.
*Assinter Secretary, Casella Postale 272, 10015 Ivrea (TO) Italy; E-mail: morandi@assinter.it, **Consultant, Corso Monte Cucco 131, Torino 10141,
Italy; E-mail: en.mosca@libero.it
is attributed to the combined effects of a positive previous experience in the traditional PM field
trend in the market, the introduction of technical began to explore the pilot-scale production of MIM
improvements in operations, and investment in parts. Today five companies are active on a rela-
machinery and automation. The average size of tively small scale, as compared with what hap-
Italian PM plants is significantly smaller than pens abroad. Now production is growing at an
those in the rest of Europe; moreover, their size accelerated rate, Figure 5. Typical components
has not undergone substantial changes as a are orthodontic brackets and dental parts, and
result of acquisitions or mergers. Such events complex structural components. These compete
occurred less frequently in Italy than in the rest of with parts fabricated by investment casting.
Europe between the mid-1980s and the mid-‘90s.
The large number of PM fabricating plants in Italy POWDER PRODUCTION
(22) compares with a relatively small number in Only one Italian company is active in this field.
the other European countries. Over the last Production and export figures since 1998 are
decade, a number of new small companies came given in Table II. Powders include atomized iron
into existence. and copper, bronze, electrolytic copper, and tin.
By examining the market for sintered compo- Significant quantities of steel shot are manufac-
nents and the evolution of PM companies in Italy, tured, together with brass, magnesium, and zinc-
it is possible to draw the following conclusions: base powders.
• Taking into account the automotive sector,
Italian PM companies were not affected signif- HARDMETALS AND FERRITES
icantly by the “ups and downs” of the car For structural parts, information is available on
industry and, much more important, most of a company-by-company basis since all the Italian
the companies succeeded in breaking into PM companies send their data to ASSINTER
new, non-automotive markets. annually, covering production, turnover, and the
• Most of the Italian fabricators of PM compo- subdivision among the four major sectors. In con-
nents and bearings are well known and
respected abroad, as reflected in the export
figures. This means that the PM industry in
Italy is healthy and, for the years to come,
prospects are encouraging.
• Excluding metal injection molding (MIM),
from an industrial perspective, pressing in
rigid dies remains the only technique used for
fabricating structural components. Other
shaping methods—for example, powder forg-
ing (PF), or hot isostatic pressing (HIP)—have
not progressed beyond the laboratory stage.
trast, for hardmetals, data about this industry ing process. Steam-treating and heat-treating fur-
can only be derived from estimates. naces are also offered.
In this field 14 companies are active, with a For PM tooling and dies, several companies
turnover of about 160 M and exports of 45 M . have the requisite knowledge and are equipped to
All the powders used in cemented carbides are supply tooling as well as automation to the PM
imported. Since the value of imports of hardmetal industry. Of these companies, at least five are
products is about 90 M , the balance of payments highly specialized in this field and innovative,
is negative. being on the forefront of technological tooling and
With respect to ceramic magnetic materials, die developments.
only hard ferrite powders are produced in Italy.
Only one company is active, but its output is sig- PM ASSOCIATIONS
nificant, namely, 15,000 mt/yr, most of which is In Italy there are two organizations involved
exported within Europe. This company also pro- in the promotion of knowledge and applications
duces 8,000 mt/yr of bound ferrites for refrigera- of PM.
tor gaskets. The first association is the Centro Metallurgia
delle Polveri (CMP), a section of the Associazione
DIAMOND TOOLS Italiana di Metallurgia (AIM), founded in 1949. At
Marble and ornamental-stone quarries are that time, PM industrial activity in Italy was
found everywhere in Italy. In consequence, indus- developing to a degree that there was a need to
trial activity has allowed the country to gain a gather and disseminate technical and scientific
large share of the market for these materials. experience on the young technology. Since its
Since stones need to be cut, drilled, and polished, inception, CMP has organized a systematic activi-
a flourishing industry has developed around the ty to spread PM knowledge and to promote the
diamond tools required for these operations. More application of structural PM parts. This has been
than 170 small companies are active in this field. accomplished by organizing meetings, seminars,
Unfortunately, data covering output and turnover and refresher courses, usually oriented towards
are not available. technical people (in particular the designers of PM
parts) in end-user companies. Up to now, 10 of
PM EQUIPMENT these courses have been held, some of them in
Hydraulic compacting and sizing presses for PM cooperation with Assinter.
are available from two Italian suppliers. It is of interest to note that several seminars
Capacities are in the range 50–800 mt and the involving PM part suppliers and end users have
presses are equipped with computerized stroke been organized at major Italian PM factories.
control, force, and position. One company offers Following the lectures, all participants were
control of up to nine independent motions. Both allowed to visit the plants.
companies have established themselves in the In 1982, in cooperation with the European PM
international market and supply presses with per- Federation (at that time EPMA did not exist), AIM
formance and quality standards comparable with organized the International PM Conference in
their European competitors. Florence. In 1983 a book specifically addressing
At least six companies manufacture sintering the designers of PM parts 1 was published in
furnaces, including vacuum furnaces, offering Italian and afterwards in English.
comprehensive solutions for control of the sinter- Today CMP operates in cooperation with EPMA
RESEARCH &
DEVELOPMENT
The paper describes a
numerical simulation study
undertaken to explore the
*Research Student, **Professor of Engineering, School of Engineering, UW Swansea, Singleton Park, Swansea SA2 8PP UK; E-mail:
D.T.Gethin@swansea.ac.uk, ***Principal Consultant, AEA Technology, Harwell, Didcot Oxfordshire OX11 0QJ, UK
effect of powder characteristics and shoe motion case studies have been devised to explore the
on powder flow into a cavity were undertaken. impact of filling on the final pressed density in a
These authors then measured filling rate and the number of part geometries and powder types.
ratio of powder volume to available die-cavity vol- Although the geometries are generically similar,
ume for different configurations of die and shoe. the actual dimensions reflect parts that are made
The effect of air on die filling was explored using the respective powder types.
through additional tests in vacuum with both Powders representative of three different types
positive and negative contributions being report- were included in the case study:
ed. The concept of a critical shoe velocity as a • Hardmetal—tungsten carbide–cobalt; composi-
method of characterizing the flowability of pow- tion: 10 w/o Co-2 w/o binder PolyEthylene
ders was introduced later.6 It is defined as the Glycol (PEG)-balance WC; spherical granules
maximum shoe velocity at which the die is filled 200–500 µm.
completely and can be used for both powder char- • Ferrous—Distaloy AE; composition: 0.5 w/o
acterization and to assist in process design. graphite (C-UF4)-0.6 w/o Kenolube-balance
Work has been undertaken to explore the iron; irregular particles 25–75 µm.
impact of filling on the initial density distributions • Ceramic—zirconia; granule size 30–80 µm
within the die. While some authors were able to These powders were chosen since they differ in
determine bulk density in vertical sections of the particle size, shape, roughness, strength, and duc-
compact, detailed measurements proved to be tility. The granules are approximately spherical,
more difficult. The sintering of loose powder after but differ in size and strength, whereas the
die fill allows for the density within smaller sec- Distaloy AE is irregular and hence is likely to pro-
tions to be determined by conventional methods. mote interlocking and bridging which, together
However, handling of the die and sintering can with the ductility of the material, will result in par-
affect the density distribution. A convenient way ticle deformation at lower loads than those used to
of determining the fill-density distribution is compress hardmetal. This phenomenon is most
through the use of X-ray computerized tomogra- likely to occur at interparticle contact points and
phy (CT).7,8 Detailed information on the density will result in a reduction of the time for which
distribution throughout the compact, including rearrangement of the particles takes place. The
that at the start of compaction, can be obtained bridges vary in strength and collapse at increasing
using this technique. force levels, resulting in a phase where both parti-
Although it is acknowledged that powder-flow cle deformation and rearrangement (during the
behavior, combined with filling-system design and collapse of the bridges) occur at the same time.
process operation, can have a significant effect on The differences in particle morphology and materi-
the fill density within the die, the consequent al properties in the three powders result in differ-
effect on the final-density variation in the pressed ent extents for which these two compaction modes
powder is unknown. Only limited work has been are present. This may result in a differing sensitiv-
done to explore its impact. 9,10 The authors ity to fill density variations. Whether this is indeed
restricted their exploration to a single part shape, the case is explored in the present study.
combined with a limited number of initial density A continuum scale model was used to simulate
variations derived from visualization experiments, the compaction process; such models are now
and fill simulation using a discrete particle tech- becoming well established for powder pressing.11
nique. The present study extends this work9,10 The system used in this study was a Cam Clay
through a more-systematic exploration of part material model, chosen because it is relatively
shape; it uses fill density determined through CT easy to characterize experimentally. The equations
scans on simple and complex die shapes. used to define this model are set out in Appendix
A. Friction contact between the powder, die, and
CASE STUDIES punch surfaces was also accounted for. The mate-
Previous work11 compared experimental work rial models used in the simulation were validated
with the prediction of compact density. One find- through comparison of punch forces derived from
ing from this comparison was that agreement the simple uniaxial die-pressing test that was used
could be enhanced through an improved defini- to determine the material parameters. Material
tion of the fill density. Consequently, the following model parameters were optimized such that the
top punch stress levels from experiment and simu- for this geometry.
lation agreed within 20 MPa for ferrous and zirco- Another common subset of geometries consists
nia powders, and within 5 MPa for tungsten of flanged components with either an external or
carbide. The simulation assumed a uniform die-fill an internal flange. Thus two components, one
density; given that the dies used for material char- with an external flange13 and a second having an
acterization were simple cylinders (typically 10 internal flange,11 were considered. Because these
mm dia. × 20 mm high) this is reasonable. part geometries were explored extensively in two
The final requirement relates to part geometry European network projects, the first is referred to
and tool set kinematics. Details are summarized via the project acronym as “Dienet” and the sec-
for the respective case studies. ond as “Modnet.”
The Dienet geometry, with dimensions, is
Die-Fill-Density Distribution shown in Table II. The Modnet geometry is shown
Fill-density distribution can be affected by a in Table III. For the case-study results presented
number of parameters, including flowability of the in this work, the line designated “NP” (see Tables
powder, shape and orientation of the die and fill- I–III) represents a neutral plane and the kinemat-
ing shoe (wide or narrow die, steps in the die), ics are defined so that no powder flow occurs
method of filling (gravity or vacuum-assisted fill, across it.
height of powder in the hopper), use of shakes, Both flanged geometries consisted of a wide top
and number of passes of the fill shoe. 12 This part and a narrow lower part. Burch14 has shown,
study attempts to assess the effect of die-fill-den- via X-ray CT, that the die-fill density is likely to be
sity distribution, affected by the cited process lower in the narrow lower section of these two-
parameters, on the pressed density of the com- level components, Figure 1; the difference is typi-
pact. To this end, a comparison was made cally 10%.
between simulated compacts in which the die-fill Double-ended compaction kinematics were
density was uniform, and in which it was not. used for each geometry and the punch displace-
The study was initiated with a simple geometry. ments were selected to provide the required com-
If simple compacts are affected significantly by paction ratio. NP was at the center of the
the die-fill-density distribution, then it is expected cylindrical compact and was located on the sec-
that this will also have an effect on more complex tion change in both the Dienet and Modnet geom-
geometries. etry parts. Figure 2 depicts schematically the
A hollow cylindrical geometry was considered as kinematics used to achieve an NP at the levels
the first shape in the study. Hollow cylindrical designated. Also the punch travel was set such
components are a common powder metallurgy that the compaction ratio on each side of the NP
(PM) product. The presence of a core rod restricts remained the same. This minimizes the effect of
powder movement both via its physical presence, flow between the upper and lower sections within
and through friction between the rod and the pow- the compact, allowing fill effects to be explored
der. The inner and outer diameters of the hollow- independently and systematically. Practically,
cylinder geometry selected are given in Table I. kinematics may be chosen such that there will be
Wu and Cocks 10 have confir med that for significant flow in this region, but this also
geometries with a high aspect ratio there was a depends on the powder type that is being
risk of air entrapment and bridging of the powder. compacted.
This most likely occurs for powders with irregular
shapes and high surface roughness as such parti- Sensitivity Study—Cylindrical Compact
cles are most likely to interlock, promoting the Geometry
formation of bridges. This geometry may also be The simulation system used in this study is an
difficult to fill completely in a given time for lower- in-house code that runs on a PC platform. This
density materials, as light particles are prevented code has been validated for parts produced using
from entering the die by the flow of air escaping press kinematics. Generally it is found that, for a
from the die. However, in this study the focus was ferrous powder, the density variation can be pre-
on the variation of the die-fill density, rather than dicted to within 2%, and the tool forces to within
on whether or not the die could be filled complete- 10%.11
ly. To this end, Distaloy AE powder was selected The sensitivity study began with the cylindrical
geometry. Fill density was taken to be 3.3 g/cm3 that in the lower part. Mass balance was main-
in the case of uniform die fill with a compaction tained to keep the average fill density at 3.3
ratio of 2.0. For the case of nonuniform die fill, g/cm3, Figure 3. The compaction was then simu-
the compact was divided into two regions of equal lated for both the uniform and nonuniform die-fill
density, namely the top and bottom halves. The distributions. In each case identical double-ended
density in the top part was set 10% higher than compaction kinematics (Figure 2) were employed.
Figure 2. Compaction kinematics: (a) cylindrical compact geometry, (b) Dienet compact geometry, (c) Modnet compact geometry
Ferrous Powder
After exploring the factors affecting the die-fill-
density distribution, and having analyzed the X-
ray CT scans available for dies filled using ferrous
powder, four initial density configurations were
selected, as shown in Figure 5. First, a compact
with a uniform fill density of 3.09 g/cm 3 was
modeled as the benchmark simulation. The
remaining configurations each consisted of two
regions of different density at fill: a region of high-
er density in the upper section and a region of
lower density in the lower section, so that the
Figure 4. Compaction of ring compact (a) nonuniform, and (b) uniform fill density.
Compaction stages in 10% increments starting at 10%
density in the upper region was 10% higher than and minimum was 10.3% of the final average den-
that in the lower region (i.e., ρtop = 1.1ρbot), and sity for the compact with uniform fill density, and
the mean density remained at 3.09 g/cm3. The 35.2% for the case of nonuniform fill distribution
configuration shown in Figure 5 (b) was selected (b). For cases (c) and (d), the density range was
since it is reasonable to assume that powder flow 14.8% and 10.5%, respectively.
into the narrow lower section may be impeded by The tool forces acting on the punches are sum-
the air escaping, and by particle bridging. marized in Table IV. For case (b) there was a 10%
Configuration (c) represents a case similar to con-
figuration (b), with the assumption that a denser
state may be obtained at the top of the lower sec-
tion due to the weight of powder above it.
Configuration (d) may be produced as a result of
local densification near the top of the die, caused
by repeated passes of the feed shoe.
The compact density contour plots are shown
in Figure 6 and Figure 7. Identical levels for the
contour colors were used in all four cases.
The compact in Figure 6(a) exhibits normal
behavior for double-ended compaction. The
regions of lowest density are located along the NP
and near the die walls. Regions of higher density Figure 6. Ferrous powder Dienet geometry compact. (a) uniform die-fill density
are located at the top and bottom punch surfaces and, (b) higher initial density in top region (ρtop = 1.1ρbot )
near the die walls, where the displacement and
wall friction are maximized. The compact in
Figure 6(b) exhibits similar features. In the lower
narrow region the trends are the same, but the
density is lower. The low-density region and the
NP occupy a larger area, with the density values
being even lower than for the uniform density
case. In the upper region the density is much
higher than in the uniform case. There is a new
region of higher density at the base of the flange,
where powder was pushed along the surface of
the punch and then around the corner into the
lower narrow section. There appears to be little
powder flow from the upper section into the lower
section of the part. Compacts in Figure 7 exhibit Figure 7. Ferrous powder Dienet geometry compact. (a) higher initial density in
similar density distribution patterns to those in top region (ρtop = 1.1ρbot ) with region border in pipe section, (b) higher initial
Figure 6(b), but with slightly less pronounced density in top region (ρtop = 1.1ρbot )
regions of high and low density near the
flange–pipe interface.
In order to be able to interpret and compare the
results, a simpler density distribution diagram is
required. In order to construct such a diagram, the
density data from the simulation were interpolated
onto rectangular zones where the density in each
zone was averaged. The final diagrams are present-
ed in Figure 8. In addition to the density variation,
Figure 8 includes the punch force levels. The bal-
ance is made up from die and core rod forces that
have not been included in the tabulation. Figure 8. Block diagram illustrating density distributions: Dienet compact geome-
The density variation between the maximum try; Distaloy AE
TABLE IV. TOOL FORCES: DIENET COMPACT GEOMETRY; DISTALOY AE subjected to larger volume reduction in compari-
son with Distaloy AE and Zirconia and thus the
Uniform Two Regions– Two Regions– compaction ratio was 2.5 while retaining the NP,
Fill Two Regions Lower Border Upper Border as shown in Table V. The uniform and nominal
Top Punch (kN) 400 442 (+10%) 435 (+8.7%) 432 (+8%) die-fill density was set at 3.15 g/cm3. The result-
Lower Outer Punch (kN) -198 -248 (+25%) -240 (+21%) -236 +(19%) ant density distribution is presented in the form
Lower Inner Punch (kN) -228 -210 (-8%) -212 (-7%) -215 (-5.7%) of a contour plot in Figure 10.
Once the reference model had been analyzed,
increase in the force acting on the top punch and
a 25% increase in the force acting on the lower
outer punch. The force acting on the lower inner
punch was reduced by 8%. This is due to the
increased amount of material in the top section of
the part. For cases (c) and (d) the increases in top
punch force were 8.7% and 8%, respectively. The
increases in load on the lower outer punch were
21% and 19%, and the decreases on the lower
inner punch were 7% and 5.7%, respectively.
Hardmetal Powder Figure 9. (a) diagonal and (b) flat region configurations
Having compared the four die-fill-density con-
figurations for the irregular ferrous Distaloy AE
powder it was appropriate to test whether the
conclusions are valid for other powders. As noted
previously, and demonstrated in a material model
validation,15 the compaction behavior of the three
powders was different. Configuration (b) was
found to result in the most severe final-density
variation and was chosen, along with configura-
tion (a), to be simulated again for the tungsten
carbide powder. The generic Dienet geometry was
used but the dimensions were modified, together
with the kinematics, to reflect the axial dimen-
sions of a part that may be manufactured using
this powder, Table V. Additionally, a configuration
similar to that in Figure 2, with a diagonal inter-
face between the two regions, was explored, Figure 10. Hardmetal Dienet compact geometry. Uniform fill density
Figure 9. In compaction, hardmetal powders are (3.15 g/cm3)
two further configurations of die-fill density were minimum values are now increased significantly in
simulated, Figure 11. In each case the die-fill den- comparison with the behavior of the ferrous pow-
sity in the upper region was 110% of the fill densi- der, achieving 15.9% of the final density for uni-
ty in the lower region, with the average density form fill, 34.1% for the diagonal border case, and
remaining at 3.15 g/cm3. The results are shown 34.2% for the horizontal border case. There is an
in Figures 11 and 12. increase in the force acting on the top punch of
In comparing the results it is clear that the 29% for the diagonal region case and 36% for the
pressed-density distribution was significantly horizontal region case. For the lower outer punch
more uniform for the compact with uniform fill. the increases in force are 57% and 64%, respec-
Regions of lower density near the NP and higher tively. The forces acting on the lower inner punch
density near the punches are more prominent for are reduced by 9% and 1.5%, respectively.
nonuniform die fill. There is also a region of high- Although the patterns of density distribution
er density immediately above the pipe–flange are similar for the ferrous and the hardmetal pow-
interface. The resulting block densities and tool ders, the percentage increase in the values of the
forces are shown in Figure 13, and the attendant tool forces are different. Consistently, there is an
tool forces are summarized in Table VI. increase in the loads on the punches; however,
The density variation between the maximum and these are proportionally much larger for the hard-
metal powder than for the ferrous powder. This is
due to the higher friction coefficient between the
die wall and powder and the larger mass of mate-
rial within the flange part of the die for the hard-
metal powder, as reflected in the significant
increase in load on the outer lower punch.
Ceramic Powder
Again, the Dienet compact geometry was used
Figure 13. Density distribution block diagram. (a) uniform fill density, (b) two
regions with diagonal border (Figure 9 (a)), and (c) two regions with horizontal
border. (Figure 9 (b))
with fill heights identical to those used for the fer- TABLE VII. TOOL FORCES ON PUNCHES: CERAMIC POWDER; DIENET
rous powder. As before, two compacts, one with a COMPACT GEOMETRY
uniform die-fill density (configuration Figure 5(a))
and the other with two regions of different die fill Uniform Fill Two Regions
density (configuration Figure 5(b)), were considered. Top Punch (kN) 699 805 (+15%)
In both cases the mass of powder was the same. Lower Outer Punch (kN) -359 -488 (+36%)
Double-ended compaction was used with a com- Lower Inner Punch (kN) -366 -332 (-9%)
paction ratio of 2.2. The density contour plots for
both simulations are presented in Figure 14 and Similar behavior to the other powders is
the corresponding block diagrams in Figure 15. observed for this geometry. For the nonuniform-
fill part the lower section density is lower overall.
The region of low density near the NP is higher,
with a lower minimum density. There is a general
increase in density in the flange region and an
area of high density immediately above the
flange–pipe interface. The variation between the
maximum and minimum densities in the compact
is 8.3% of the final density for the compact with
uniform fill density, and 28.9% for the multi-
region case.
The tool forces acting on the punches are sum-
marized in Table VII. There is a 15% increase in
the force acting on the top punch, and a 36%
increase in the forces on the lower outer punch.
The force acting on the lower inner punch are
reduced by 9%, due to the increased amount of
material in the top section of the part, consistent
with the trends reflected in the other powder
types.
Modnet Geometry
The Modnet stepped geometry differed from the
Figure 14. Ceramic powder Dienet geometry compact. (a) uniform fill density, and Dienet geometry in that the lower section was on
(b) higher initial density in top region the outside of the part, rather than on the inside.
This is significant since more volume is occupied
by the lower section of the Modnet part than that
of the Dienet part. As the upper section of the die
is expected to have a higher density, some of the
powder from the top section is transferred to the
lower section. Thus, in the case of the Modnet
geometry there is more capacity to accommodate
powder transfer than in the Dienet geometry, as
illustrated in Figure 16.
Similar fill configurations were used for the
Modnet geometry, namely, uniform die-fill density
for the first model and the second model, with two
regions of differing fill density, balanced to pro-
duce the same mass compact as in the uniform-
fill case. Again, the difference between the density
in the upper and lower parts was taken to be
Figure 15. Block diagram of density distribution in ceramic powder; Dienet com- 10%. The border between the regions and the NP
pact geometry. (a) uniform fill density, (b) higher initial density in top region
was along the top surface of the inner lower
Figure 18. Ferrous powder Modnet geometry compact. (a) uniform fill density, (b)
higher initial density in top region (ρtop = 1.1ρbot )
Figure 16. Possible powder transfer direction in Dienet and Modnet compact
geometries
Figure 19. Block diagram of density distribution: ferrous powder Modnet geome-
try compact. (a) uniform fill density, (b) higher initial density in top region (ρtop =
Figure 17. Modnet geometry fill conditions; ferrous powder 1.1ρbot )
multilevel geometries, the differences in both the friction between the tools and the powder. This is
final-density distribution and tool forces are sig- a feature commonly seen in compacts. At the
nificant. Typically, the range of densities in the lower end of area “2,” marked “4,” there is a local
final compact are higher, with more extreme max- region of high density which is again common to
imum and minimum densities. This has implica- all three compacts. The high-density area marked
tions in relation to sintering shrinkage in “5” is a common feature in all three compacts
hardmetal and ceramic parts, and the mechanical and, like feature “3,” correlates well with predic-
performance of ferrous parts. tions from experience.
Where die-fill densities are higher in the upper The features cited are also present in the densi-
region, forces on the top and the lower outer ty distribution of the Modnet geometry compact,
punch of the Dienet geometry part are also found Figure 21. The region of lower density “1” is locat-
to increase significantly. This may lead to a ed immediately below the level of the lower inner
reduced lifespan of the punch or, in extreme cases, punch. There is a band of higher density, desig-
failure. The percentage increase varies for different nated “2,” which connects the inside top of the
powders and is most significant for tungsten car- compact with the tip of the lower inner punch.
bide, because the latter powder is the most com- However, there is not a prominent region of high
pressible and exhibits a rapid build-up of stress density around point “4,” unlike the compacts
towards the end of the compaction process. When with the Dienet geometry. This is expected
combined with the larger displacement required to because the top part of the Modnet geometry com-
compress this powder, it leads to a significant pact is bulkier. The difference between the initial
increase in stress levels on the tool set. density in the top section and the mean fill densi-
The different density levels achieved in each ty is smaller for the Modnet geometry compact
powder prohibit direct comparisons. However, than for the Dienet geometry compact, in order to
some common features are observed in all three maintain the 10% top-to-bottom variation
compacts. There is an area of low density, desig- because of the relative volumes occupied by the
nated “1” in Figure 20, just below the level of the top and bottom sections in each compact. The
lower outer punch. This is the area most distant size of the top section of the Modnet geometry
from the top and bottom punches; the presence of compact also results in a smaller distribution as
a low density area in this location agrees well with the powder is less constrained. The high-density
predictions. There is a region of higher density areas “3” and “5” are also less pronounced. The
common to all three compacts, designated “2,” former because the fill density is low in the lower
which connects the tip of the lower outer punch section, and the latter because the powder in the
to the top right corner of the compact. It is diffi- top section is less constrained, allowing for a
cult to compare the intensity of zone “2” between more uniform density distribution than in the
the different compacts because of the varying Dienet geometry compact.
densities and contour color indexing. Section “3”
is a region of higher density which is caused by
Figure 20. Comparison of density distributions. (a) ceramic, (b) ferrous, (c) hard-
metal powders (nonuniform fill condition, border region at the level of the lower Figure 21. Density distribution in green Modnet geometry compacts; ferrous
outer punch) powder. (a) uniform fill, (b) nonuniform fill
ACKNOWLEDGEMENTS 3 (Pd)2 Qd
This work was funded by AEA Technology as —
Q0 =
2 2
Qd + —————— (A.8)
part of the "Minimizing Density Variations in 2Pd + —2 Qd
Powder Compacts" project for DTI’s Materials 3
Metrology program.
Therefore, for known values of and, Pd and Qd
Appendix A: Definition of Material Model can be calculated. Subsequently P0 and Q0 can be
The material model was defined using an obtained and curve fitted as functions of the den-
instrumented-die test in which a cylindrical pow- sity field. The functions are chosen to fit the form
der compact is pressed, and for which the stress of the experimental data and to satisfy limiting
state is axisymmetric. The hydrostatic and devia- conditions. There are four unknowns K1 to K3
toric stresses defined as P and Q are given by: and Qmax:
ρ – ρ0 K
P = (σz + 2σr)/3 (A.1)
( (
P0 – K1 ln – ————
ρ – ρmax )) 2
(A.9)
Q = σz – σr (A.2)
K3P0
For a Cam-Clay material model:
Q0 = Qmax tanh ———
Qmax ( ) (A.10)
Zirconia Powder
Qmax K1 K2 K3 ρ0 ρ^ E ν µ
18000.0 150.0 1.5 3.37 1.2 g/cm3 3.6 g/cm3 8.0E + 04N/mm2 0.3 Variable1
1. Friction varied from 0.12 at zero normal stress to 0.05 at 250 MPa as a quadratic function
Powder Flow”, AEA Technology Report, 2003, Atomic Exhibition PM2004, edited by H. Danninger and R. Ratzi,
Energy Authority, Harwell, Didcot Oxfordshire, UK, 2003. European Powder Metallurgy Association, Shrewsbury,
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Particulate Materials, compiled by J.J. Oakes and H.H. Numerical Study of Die Filling, Powder Transfer and Die
Reinshagen, Metal Powder Industries Federation, Compaction”, Powder Metallurgy, 2005, vol. 48, no. 1, pp.
Princeton, NJ, 1998, vol. 1, part 4, pp. 107–127. 68–76.
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Variations in Metal Powder”, Powder Metallurgy, 2002, vol. During Die Filling”, Powder Metallurgy, 2004, vol. 47, No.
45, no. 2, pp. 146–153. 2, pp. 127–136.
5. A.C.F. Cocks, L. Dihoru and T. Lawrence, “A Fundamental 11. PM Modnet Computer Modelling Group, “Comparison of
Study of Die Filling”, EURO PM2001: 2001 European Computer Models Representing the Powder Compaction
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Flow of Powder into Simple and Stepped Dies”, Powder “Comparison of Filling Behaviour of Metallic, Ceramic,
Technology, 2003, vol. 134, pp. 24–39. Hardmetal and Magnetic Powders”, Powder Metallurgy,
7. J. Haskins and W. Jandeska, “Powder Flow and Die 2005, vol. 48, no. 1, pp. 77–84.
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in Powder Metallurgy and Particulate Materials, compiled Achievements”, Powder Metallurgy, 2006, vol. 49, no. 1,
by J.J. Oakes and H.H. Reinshagen, Metal Powder pp. 8–10.
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10, pp. 77–87. ect, AEA Technology, 2004.
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Tomography”, Powder Metallurgy World Congress &
RESEARCH &
DEVELOPMENT
The feasibility of fabricating
high-density parts from
Inconel 718 powder using
EXPERIMENTAL PROCEDURE
Gas-atomized Inconel 718 powder of two different sizes was used
(Table I and the scanning electron microscope (SEM) images in Figure
1). The nominal composition of the alloy is listed in Table II.
To enhance the 3DP process, coarse and fine powders were blended
to increase both the apparent density and tap density. The coarse pow-
der was blended with different amounts of fine powder ranging from 10
w/o to 100 w/o of fine powder. Application of the 3DP process with
powder blends exhibiting a high tap density was expected to enhance
the sintered part density. The powders were blended in a Turbula™
*PhD Student, ***Lecturer, ****Professor, Universidad Carlos III de Madrid, Department of Materials Science and Engineering, Avda. Universidad
30, E-28911 Leganés, Madrid, Spain; E-mail: jsicre@ing.uc3m.es, **Head of Department of Powder Metallurgy, Fraunhofer IFAM, Wiener Strasse
12, D-28359 Bremen, Germany
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
TABLE I. PARTICLE-SIZE DISTRIBUTION OF POWDER TABLE II. CHEMICAL COMPOSITION OF POWDER (w/o)
Fine Powder (F) Coarse Powder (C) * Ni Cr Fe Nb(+Ta) Mo Ti Mn Al Si Other Elements (Max)
10 w/o -6.1 µm 1.8 w/o +53 µm 52.6 18.8 Bal. 5.3 3.2 0.93 0.12 0.49 0.28 0.08 C, 0.006 B, 0.015 S,
50 w/o -12.8 µm 98.2 w/o -53 µm 0.015 P, 0.30 Cu
90 w/o -21.8 µm
* Based on ASTM B 214
Figure 1. As-received superalloy powders: (a) coarse powder, (b) fine powder. SEM/secondary electron images
model T 2F mixer at a moderate speed for 45 min. from the reservoir to the build box creating a layer
Thermomechanical analysis (TMA) was utilized of powder with the desired thickness.
to monitor the changes in volume expansion of the Subsequently, the nozzles in 3DP-1 or inkjets in
alloy, as affected by the proportions of coarse and 3DP-2 deposited the binder, as dictated by the
fine powder in the blends. TMA analyses were con- CAD model. In both 3DP processes, the thickness
ducted in the expansion mode on a Perkin-Elmer of the powder layer was ~125 µm.4 Once the pow-
TMA thermomechanical analyzer under an atmos- der layer was printed, it was dried for 20 s in the
phere of flowing argon. Powder samples (5 mm in 3DP-1 device, and for 50 s in the 3DP-2 device.
height) were heated from 303K (30°C) to 1,598K Each 3DP device used a specific polymeric com-
(1,325°C) at 10 K min-1 with a dwell time of 1 h mercial binder, namely Primal WS-24E and PM-B-
and then cooled to 303K (30°C) at 10 K min-1. The SRX for 3DP-1 and 3DP-2, respectively. The
experiment was performed without the application difference in the two binders arises from the depo-
of force to monitor changes in length due to the sition mechanism(s) operative in each device. The
thermal cycle. This resulted in a similar response amount of binder in the final material was ~10
to that observed utilizing dilatometry. v/o; it was deposited at a rate of 2 layers per min
After characterization of the powders, the 3DP for the prototype geometry selected.
process was initiated. Two different 3D-printing The resulting 3DP green parts were sintered
devices were used, namely Prometal™RTS-300 under a high vacuum of 4.05 x 10-10 MPa (4 x 10-
and Prometal™RX-1 (hereafter referred to as 3DP- 6 mbar) at 1,563K (1,290°C) or at 1,573K
1 and 3DP-2, respectively). The two devices are (1,300°C) for 2 h in a single-step sintering
based on the same functional principle, but a dif- process. Two different heating rates were exam-
ferent binder was used in each process. The print- ined, namely 5 K/min and 10 K/min, to monitor
ing device consisted of two boxes, the reservoir the possible influence of debinding on sintered
box and the build box. The powder was spread properties.
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
Characterization of the printed parts included rial is necessary (in this case ~100 µm). When
an evaluation of the shrinkage after sintering and considering the particle size of the powders, opti-
the density, as determined by the Archimedes’ mization of the particle-size distribution is also
immersion (ethanol) method. Microstructures necessary. This was accomplished by evaluating
were analyzed by means of light optical blends of the fine and coarse powders from 100
microscopy (OM) and SEM. Samples for metallo- w/o coarse (C) to 100 w/o fine (F). As seen in
graphic analysis were prepared following standard Figure 2, the size distribution shifts slightly to
techniques: progressive silicon carbide grinding, smaller sizes when the level of fine powder added
surface polishing (3 µm diamond paste), and elec- increases from 0 w/o to 30 w/o.
trolytic etching in 5 w/o oxalic acid. Figure 3 shows the influence of particle-size
Sintered parts were HIPed in a model AIP6-30H distribution on apparent density and tap density.
press (American Isostatic Presses, Inc.). The first Since the powder is spread over the preceding
HIPing cycle was 1,473K (1,200°C) under 146 powder layer during the 3DP process, it is impor-
MPa for 3 h, as previously reported.10 Both heat- tant to know how much material was deposited.
ing and cooling rates were 10K/min. The To this end, tap density was monitored as a func-
microstructures of the HIPed parts were analyzed tion of the particle-size distribution of the powder
using LOM and SEM. The final density was meas- blends, since apparent density is strongly affected
ured by means of a helium pycnometer. After ana- by particle size; it decreases as the particle size of
lyzing the density and microstructure, a second the blend decreases.6 In contrast, a convincing
HIPing cycle was imposed, which consisted of explanation cannot be provided for the changes in
heating to 1,483K (1,210°C) under 206 MPa for 3 tap density that result from adding fine powder to
h in argon, using the same heating and cooling coarse powder. Since the 30F70C and 20F80C
rates as in the initial cycle. Samples for metallo- powder blends exhibited the highest tap densities
graphic analysis were prepared using the follow- of all the samples, they were printed along with
ing standard techniques: progressive silicon 100C powder as a reference.
carbide grinding, surface polishing (3 µm dia- Another criterion for selection of the powder
mond paste), and etching in Kalling’s reagent.5 blends to be printed is based on thermal analysis.
Powder blends with lower amounts of fine powder
RESULTS AND DISCUSSION exhibited between 13% and 16% unidirectional
Optimization of Powder Mixtures shrinkage, as shown in Figure 4. In addition to
To optimize the 3DP process, a particle size apparent density and shrinkage, it is also neces-
similar to the layer thickness of the printed mate- sary to recognize that powder blends with higher
levels of fine powder (80F20C and 90F10C powder
blends) are not suitable for 3DP.7,8
Figure 2. Effect of addition of fine powder to coarse powder on particle-size Figure 3. Effect of increasing the level of fine powder in blends of coarse and fine
distribution powder on apparent density and tap density
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
Figure 5. Photographs of 3DP process utilizing Prometal™RTS-300. (a) 100C powder, (b) and (c) 20F80C powder blend, (d) 30F70C powder blend
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
Figure 7. Effect of heating rate, sintering temperature, and binder type on relative density and shrinkage of powder blends. (a) 3DP-1 mode,
(b) 3DP-2 mode, (c) 3DP-1 mode, and (d) 3DP-2 mode
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
face:volume ratio, which increases the driving number of scattered γ’ precipitates (circled in
force for sintering. A high density was obtained Figure 8). At 1,573K (1,300°C), micrographs
and complete densification appears to be a viable exhibit large pores which appear to be the result
target for this powder blend. Nonetheless, porosity of overheating during sintering. This reflects an
is still evident, but is less for 3DP-2 than for 3DP- excessive presence of liquid phase during sinter-
1, as seen by comparing Figure 8 and Figure 9. ing, which could not rediffuse into the solid parti-
Characterization of the microstructures of the cles. Literature on the sintering of Inconel
3DP-1 parts shows that the phases present vary includes evidence of a liquid phase >1,463K
with the sintering temperature. The heating rate, (1,190°C).9,10 Thus, there will always be a small
or the proportions in the powder blends, do not amount of liquid present which favors mass
influence the resulting microstructures. transport mechanisms leading to higher densifica-
Notwithstanding discrepancies in the literature tion, at the chosen sintering temperatures.
concerning the precipitation kinetics in Inconel However, if the amount of liquid formed is exces-
718, the primary microstructural effects on sive, it could be detrimental to properties because
mechanical properties in this alloy system are of rediffusion.
attributed to the presence of γ’ (intermetallic Based on the microstructures of the sintered
Ni3TiAl) precipitates, and to γ" (intermetallic Ni3Nb) 3DP-2 parts major changes are observed com-
precipitates which are unstable >923K (650°C) pared with 3DP-1. First, the expected quantities
and are associated with the presence of iron. of γ’ and γ" precipitates (circled in Figure 9) appear
Parts sintered at 1,563K (1,290°C) exhibit a at 1,563K (1,290°C).11 Second, sintering tempera-
high density of small γ" precipitates, and a smaller ture does not affect the final microstructure sig-
Figure 8. Representative microstructures of 20F80C powder blend: (a) and (b) sintered at 1,563K, (c) sintered at 1,573K with heating rate 5 K/min and 3DP-1 mode. OM
Figure 9. Representative microstructures of 100C powder (a) sintered at 1,563K, heating rate 5K/min, (b) sintered at 1,573K and 5K/min, and (c) sintered at 1,563K,
heating rate 10 K/min and 3DP-2 mode. OM
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
nificantly. As with 3DP-1, the sintering tempera- decreases significantly as the proportion of fine
ture does not change the number of precipitates, powder in the powder blend increases.
only their size and amount. The level of porosity Specifically, with 20 w/o and 30 w/o of fine pow-
der, pores and grains are round, which suggests
that sintering occurred during the final stage.
CONCLUSIONS
1. The binder used in the 3DP process, and the
binder deposition device, influence the final
density, microstructure and the shape profile
Figure 11. Representative micrograph of HIPed sample 20F80C (1,473K and of the sintered parts.
146 MPa for 3 h) showing porosity. SEM/backscattered electron image 2. Comparing the two processes, 3DP-1 resulted
in printed parts with superior shape stability
and a higher final sintered density than 3DP-2,
but with different microstructures. The latter
mode resulted in excellent microstructures and
properties, but inferior shape stability.
3. Sintering temperature had a significant effect
on the final microstructure in the 3DP-1 mode,
but had little effect in the 3DP-2 mode.
4. The optimal sintering parameters were 1,563K
(1,290°C) for 2 h in vacuum with a heating rate
of 5 K/min; this resulted in sintered density
levels ~97% of the pore-free value.
5. No differences were found in the size or the
Figure 12. Density of sintered 3DP parts for two powder blends after HIPing at distribution of γ’ precipitates after sintering or
1,483K and 206 MPa for 3 h
HIPing. However, the homogeneity in the distri-
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
Figure 13. Representative micrographs illustrating fully dense printed and sintered parts. (a) and (c) 3DP-1 mode of 100C , (b) and (d) 3DP-2
mode of powder blend 30F70C. SEM/backscattered electron images
HIGH-DENSITY INCONEL 718: THREE-DIMENSIONAL PRINTING COUPLED WITH HOT ISOSTATIC PRESSING
6. ASM Handbook, Powder Metal Technologies and 9. K. Hajmrle and R. Angers, “Sintering of Inconel 718”, Int.
Applications, vol. 7, Ninth Edition, 1998, ASM J. Powder Metall. & Powder Tech., 1980, vol. 16, no. 3, pp.
International, Materials Park, OH. 255–266.
7. M. Turker, D. Godlinski, H. Pohl and F. Petzoldt, “Rapid 10. G. Appa Rao, M. Srinivas and D.S. Sarma, “Effect of
Prototyping of Inconel Alloys by Direct Metal Laser Solution Treatment Temperature on Microstructure and
Sintering and Three Dimensional Printing”, ibid reference Mechanical Properties of Hot Isostatically Pressed
no. 4, vol. 3, pp. 93–98. Superalloy Inconel 718”, Mater. Sci. Tech., 2004, vol. 20,
8. D. Godlinski and S. Morvan, “Steel Parts with Tailored pp. 1,161–1,170.
Materials Gradients by 3D-Printing Using Nano- 11. S. Azadian, “Aspects of Precipitation in Alloy Inconel 718”,
Particulate Ink”, Mater. Sci. Forum, 2005, vols. 492–493, 2004 PhD Thesis, Luleå University of Technology,
pp. 679–684. Sweden. ijpm
ENGINEERING &
TECHNOLOGY
Nanoscale powders can
enhance densification and
enable sintering of compo-
SINTERING MODEL
Following the approach of German and Olevsky,1,2 a sintering model
was constructed to calculate the apparent density, green density, sin-
tered density, and grain size as functions of particle size. The sintered
density and grain size are then used to predict properties.
Apparent Density
The high surface area and interparticle friction of nanoscale pow- Presented at PowderMet2007
ders result in agglomeration and low packing densities.3 The depend- and published in Advances
ence of the fractional apparent density ρA on the particle size can be in Powder Metallurgy &
expressed by the relation: Particulate Materials—2007,
log ρA = log ρ0 + a log D (1) Proceedings of the 2007
International Conference on
where ρ0 is the fractional packing density of a 1 µm powder, a is a con- Powder Metallurgy &
stant, and D is the median particle size in µm. Particle shape and sur- Particulate Materials, which
face condition impact the packing behavior, so each powder is are available from the
different. In this analysis, values of 0.143 for ρ0 and 0.21 for a were Publications Department of
used, based on values derived from tungsten particle-packing data.1,2 MPIF (www.mpif.org).
*R&D Director, ATI Alldyne, 7300 Highway 20 West, Huntsville, Alabama 35806, USA; E-mail: jjohnson@alldyne.com
( ( 1.545 P
ρg = 1 + ρA 1-exp ——— -—
D1/7 C )) (2) formity with the relation:5
ρg 1/2
where ρA is the fractional apparent density, D is
the median particle size in µm, P is the com-
G = D + Kt1/3 ———
( ) ( )
1- ρs
-QG
exp ———
T
(6)
paction pressure in MPa, and C is a function of where D is the initial particle size, K is a collection
material strength. In this paper, C is estimated as of material constants, t is the isothermal time at
nine times the annealed hardness H0 of the pore- absolute temperature T, ρg is the fractional green
free material. density, ρS is the fractional sintered density, and
QG is the activation energy for grain growth.* For
Sintered Density tungsten, K = 23.5 µm/s 1/3 and Q G = 11,430
The sintered density ρs depends on the green when time is in s, temperature is in K, and grain
density ρ g and the linear sintering shrinkage size is in µm. In this paper, the grain size for other
∆L/Lg in conformity with the relation: materials was predicted by substituting an appro-
priate activation energy, but leaving K constant.
ρg
ρs = ————— (3) As an example of the model predictions, the
( )
3
∆L green density, sintered density, and grain size are
1- —— plotted in Figure 1 as functions of particle size for
Lg
two different cases. In the first case, the tungsten
The sintering shrinkage displays an asymptotic powder is pressed at 250 MPa and sintered at
characteristic as the compact nears full density. 2,000°C for 60 min. The low apparent density of
Following the master sintering curve treatment of nanoscale powders results in a low green density,
Su and Johnson,4 this behavior can be represent- which cannot be sintered to high density. The
ed by a sigmoid function as given by the relation: density also decreases with large particles due to
their slower sintering kinetics, leaving an optimal
∆L f2 particle-size range of 1 to 3 µm for near-full den-
—— = f1 + ———————— (4)
Lg
( )
f3 - Y
1 + exp ———
f4
sity. The grain size of nanoscale powders sintered
at 2,000°C is substantially larger than the initial
particle size. In the second case, a pressure of
where f1 = 0.01, f2 = 0.165, f3 = 0.104, f4 = 0.015, 1,280 MPa is used to compact the tungsten pow-
and Y is a densification factor that can be calcu- der. A much higher green density is attained and
lated from an Arrhenius-type equation, namely: nanoscale powders are predicted to sinter to near-
full density at only 1,000°C, while preserving a
1
Y = ——
Dv
exp
( Q
Bstw - ——
T ) (5)
refined grain structure. In both cases, once the
particle size becomes too large to press and sinter
to full density at the specified conditions, grain
where D is the particle size, w and v depend on growth becomes negligible and the grain size is
the diffusion mechanism, Bs is a material param- determined by the initial particle size.
eter, t is the sintering time, Q is the activation In general, the properties of refractory metals,
energy for diffusion,* and T is the sintering tem- such as tungsten and molybdenum, are much
perature. For tungsten, BS = 0.0054, Q = 3652, v
*As defined in equations (5) and (6), Q and QG are normal-
= 0.44, and w = 0.33 when the particle size D is in ized to the gas constant (or Boltzmann’s constant). Thus, the
µm, temperature T is in K, and time t is in min- units of the two activation energies are K.
Figure 1. Two examples of model predictions for the effects of tungsten particle size on green density, sintered density, and grain size
more sensitive to particle size than other metals. hardness of the annealed pore-free material, θ is a
The properties of ceramics are even more sensitive material constant, and G is the grain size in µm.
to particle size since they cannot be pressed to The abrasive-wear loss of hard materials is
high green densities due to their high hardness linked to hardness and can be estimated from the
and brittle nature. relation:1,2
E = E0ρs3.4 (7)
σ = ρs
( θ
σ0 + ——
G ) (11)
ε0ρs3/2
H = ρs
( θ
H0 + ——
G ) (8) εmax = ————————
1+160 (1-ρs)2
(12)
where ρS is the fractional sintered density, H0 is the where ρS is the fractional sintered density and ε0
is the ductility of the pore-free material. This conductivity can be calculated directly from the
same relation is used for ceramics but with frac- Koh and Fortini relationship:
ture toughness in place of ductility.
ρs
λ = λ0 —————— (15)
Electrical Resistivity 1+11(1-ρs)2
Electrical resistivity R increases with porosity
and generally follows the structure-independent where λ0 is the thermal conductivity of the pore-
semi-empirical relationship obtained by Koh and free material.
Fortini:8 Baseline properties of pore-free materials are
summarized in Tables I and II. The values are
1+11(1-ρs)2 based on material properties given by the CES
R = R0 —————— (13)
ρs Selector Version 4.5 software (Granta Design
Limited).
where ρs is the fractional sintered density and R0 As examples of the property model predictions,
is the electrical resistivity of the pore-free material. the properties of tungsten are plotted in Figure 2
as functions of particle size for the two cases
Thermal Conductivity shown in Figure 1. For tungsten powder pressed
The thermal conductivity λ of metals can be at 250 MPa and sintered at 2,000°C, the proper-
calculated from the electrical resistivity R using ties follow density and peak at approximately 1 to
the Wiedemann–Franz relationship:9 3 µm. Higher strengths and hardnesses are possi-
ble with nanoscale powders and ultrahigh com-
LT paction pressures.
λ = —— (14)
R Property maps can be constructed by plotting the
properties as functions of each other. Utilizing this
where L is the Lorenz number and T is the method, it is possible to identify unique property
absolute temperature in K. For ceramics, thermal combinations. Plots of modulus, hardness, ductility,
Figure 2. Two examples of model predictions for the effect of tungsten particle size on various properties
Figure 3. Property maps for metals of modulus, hardness, wear resistance, ductility, electrical resistivity, and thermal conductivity as functions of
strength
electrical resistivity, thermal conductivity, and wear other. For example, modulus, hardness, and abra-
resistance as functions of strength are given in sion resistance correlate directly with strength,
Figure 3 for ten different metals. Most properties while ductility is inversely related. Interesting com-
either correlate or inversely correlate with each binations can be identified for electrical resistivity or
Figure 4. Property maps for ceramics of modulus, hardness, wear resistance, fracture toughness, electrical resistivity, and thermal conductivity as
functions of strength
thermal conductivity and strength. Lower-strength dicted properties can be divided by the powder
copper and aluminum tend to be the best electrical prices to normalize them.
and thermal conductors. The unique combination The cost of powders over a wide range of parti-
of high strength and high conductivity of tungsten cle sizes was analyzed. Differences in impurity
is evident from Figure 3. levels can have a large effect on powder costs.
Plots of modulus, hardness, fracture tough- Powder costs also vary due to fluctuations in
ness, electrical conductivity, thermal conductivity, material prices, especially metal prices (in recent
and wear resistance as functions of strength are years), but in general they follow a power law rela-
given in Figure 4 for eight different ceramics. The tionship with particle size. Plots are shown in
properties of ceramics show similar correlations Figure 5 for metals and ceramics. This is mostly
with each other as metals. In general, ceramics related to the greater cost of creating higher sur-
provide high modulus, high hardness, good wear face area. Some exceptions exist if a low-cost
resistance, and a wide range of electrical and chemical process route is feasible. For example,
thermal conductivities, but poor fracture tough- coarse tungsten powder (>10 µm) is not lower in
ness. The high strength of tungsten carbide sets it cost than 1 µm powder and can even be more
apart from the other ceramics. expensive because of longer processing times or
additives to grow the particles. The cost of refrac-
COST-NORMALIZED PROPERTY MAPS tory metal powders produced via chemical
The range of properties of the different materi- processes generally does not decrease as the par-
als shown in Figures 3 and 4 results from the ticle size increases above a few micrometers. In
range of sintered densities achieved of the differ- contrast, metals such as copper, iron, and titani-
ent particle sizes. While some applications require um continue to decrease in cost until they
maximum values for certain properties and will approach the cost of wrought metal. On the other
pay a premium for them, the most common appli- end, making nanoscale powders generally
cations will only pay for materials that provide the requires alternative techniques such as gas-phase
optimal price/performance value. As a first esti- synthesis or exploding wires and these processes
mate of the value for nanoscale powders, the pre- are generally much more costly. Some of the cost
Figure 5. Power law relationships between powder cost and particle size: (a) metals and (b) ceramics
Figure 6. Cost-normalized properties of tungsten. Pressures and temperatures refer to compaction and sintering parameters
is related to the lower volumes of powder pro- µm, their value drops. This finding is in agree-
duced and the inefficiencies of new processes, but ment with the current market structure in which
nanoscale powders are unlikely to match the cost the most commonly used powders have particles
of conventional powders. sizes of 0.8 µm to 3 µm. The higher strength and
Dividing the predicted properties by the powder hardness levels possible with nanoscale powders
cost enables plotting of cost-normalized proper- compacted at ultrahigh pressures are offset by
ties. Examples are shown for tungsten in Figure 6 the higher powder cost. For tungsten nanoscale
for the two cases given in Figure 2. For powders powders to be economically useful on a large
pressed at 250 MPa and sintered at 2,000°C, peak scale, they will need to be produced at lower cost,
values occur at ~1 µm for strength, ductility, and or provide a much larger improvement in property
thermal conductivity, indicating the optimal value performance than is predicted from the models
proposition. As the particle size decreases below 1 used in this study.
Figure 7. Cost-normalized properties of iron. Pressures and temperatures refer to compaction and sintering parameters
As another example, the cost-normalized prop- sures provide a negligible incremental value in
erties of iron are shown in Figure 7. Unlike tung- comparison to a coarser particle size. This simple
sten, no peaks are seen, thus coarse powders economic analysis shows why conventional press-
provide the best value proposition. Even property and-sinter ferrous PM uses coarse powders and
improvements with ultrahigh compaction pres- exposes the hurdles that nanoscale powders must
overcome to provide superior value. tion. To fully analyze the costs of processing
As with the absolute properties, cost-normal- nanoscale powders, a cost model was constructed
ized property maps can be produced by plotting based on the approach developed by German10–13
the cost-normalized properties as functions of for powder injection molding (PIM).
each other. The plots in Figure 8 show the high- German’s cost model for PIM was modified for
strength-per-cost ratio of iron and why it is so die compaction. The model contains over 150
widely used for structural applications. The value variables, so realistic assumptions were made in
of copper for thermal conductivity is also obvious. relation to overhead costs such as rent, mainte-
From the plots in Figure 9 for ceramics, tungsten nance, interest rate, facility use, electric rate,
carbide and alumina provide the optimal value for depreciation, and load balance. Ranges for these
high-volume, cost-sensitive applications. Other variables were evaluated where appropriate. Input
metals and ceramics have niche applications only values for the various models were obtained from
where high absolute performance is required at current databases and supplemented, as needed,
premium cost. from external sources. Each unit operation was
independently audited for costing rates and sensi-
COST MODELS tivity analyses were conducted to determine the
Powder costs are only a portion of the cost of most significant factors. The part geometry is a
producing PM parts. Compaction and sintering key attribute that affects cost in several ways. To
costs must also be considered. The use of ultra- illustrate the cost model concepts, a ring geome-
high compaction pressures to consolidate try with a 2.54 mm OD, 1.27 mm ID, and a height
nanoscale powders requires large presses with of 0.85 mm was assumed.
high tonnage, which results in high compaction Compaction costs are calculated as a function
costs. The low apparent density of nanoscale pow- of material, particle size, compaction pressure,
ders also results in a long stroke, which slows and part size. A press was selected from a data-
down production rates. Nanoscale powders have base of six presses, based on the tonnage
the potential to sinter at lower-than-conventional required to achieve desired pressures. The hourly
temperatures, reducing energy consumption and operating cost was calculated based on the capital
possibly allowing for lower-cost furnace construc- cost, floor space, utility costs, maintenance costs,
and labor costs. The cycle time was calculated Sintering costs were calculated based on the
based on the stroke rate and the stroke distance, sintering temperature required to achieve a densi-
which depends on the apparent density of the ty of 96% of the pore-free level. The sintering tem-
powder and the compaction pressure. The green perature depends on material, particle size, and
density was calculated as an output variable for green density. A furnace was selected from a
input into the sintering cost model. database of nine furnaces, based on the required
A plot of compaction cost as a function of parti- sintering temperature. Sintering costs were nor-
cle size for different compaction pressures for the malized per unit volume and the number of ring
ring geometry is shown in Figure 10. This plot is parts that could be sintered per unit volume was
not material specific, but the resulting green den- calculated. The hourly operating cost was calcu-
sity for a given combination of particle size and lated from the capital cost, floor space, utility
compaction pressure depends on material hard- costs, maintenance, and labor costs. A 12 h sin-
ness. The compaction cost is dependent on parti- tering cycle was assumed.
cle size only at ultrahigh pressures. Ultrahigh The sintering temperature required to achieve
pressures provide little benefit for ceramics, full density increases with coarser powders and
which cannot be pressed to high densities due to lower compaction pressures. Sintering costs dras-
their lack of ductility. The cost of compaction of tically increase at particle sizes which cannot be
metals and ceramics is small compared to the raw sintered in conventional furnaces. In some cases,
material cost. a lower green density requires slightly smaller
particle sizes to enable the use of conventional
furnaces. The effect of particle size on sintered
part cost for various metals is shown in Figure
11. Powder costs dominate sintered part costs.
Lower sintering temperatures due to finer pow-
ders do not offset higher powder costs except in
special cases.
CONCLUSIONS
Powder costs generally follow a power law rela-
tionship with particle size. Ultrahigh pressure
compaction and low-temperature sintering of
nanoscale powders provide a means of producing
refined microstructures that result in improved
hardness and strength. Ultrahigh compaction
Figure 10. Effect of particle size and compaction pressure on compaction cost pressures are more costly than conventional pres-
sures, but the compaction cost is small relative to
powder cost. A reduction in sintering cost due to
lower sintering temperatures of nanoscale pow-
ders does not offset their higher powder cost.
Analysis of the value proposition of nanoscale
powders by cost normalizing their properties
shows that the incremental improvement they
provide in performance does not compensate for
their higher cost. For nanoscale powders to be
useful for press-and-sinter PM, they will need to
be produced at much lower cost, or provide a
much larger improvement in property perform-
ance than predicted by conventional models.
ACKNOWLEDGEMENTS
The author gratefully acknowledges Randall M.
Figure 11. Effect of particle size and material on sintered part cost
German for sharing his spreadsheet models and
Harald Lemke for insightful discussions and guid- ness of Ultrafine and Nanocrystalline Hard Materials”, Int.
ance on the economic analysis. J. Refract. Met. Hard Mater., 1999, vol. 17, pp. 141–152.
8. J.C.Y. Koh and A. Fortini, Inter. J. Heat Mass Transfer,
1973, vol. 16, pp. 2,013–2,021.
REFERENCES 9. J.E. Parrot and A.D. Stuckes, Thermal Conductivity of
1. R.M. German and E. Olevsky, “Mapping the Compaction Solids, 1975, Pion, London.
and Sintering Response of Tungsten-Based Materials into 10. R.M. German, “The Impact of Economic Batch Size on the
the Nanoscale Size Range”, Int. J. of Refract. Met. Hard Cost of Powder Injection Molded (PIM) Products”,
Mater., 2005, vol. 23, pp. 294–300. Advances in Powder Metallurgy and Particulate Materials—
2. R.M. German and E. Olevsky, “Strength Predictions for 2003, edited by R. Lawcock and M. Wright, Metal Powder
Bulk Structures Fabricated from Nanoscale Tungsten Industries Federation, Princeton, NJ, 2003, part 8, pp.
Powders”, Int. J. of Refract. Met. Hard Mater., 2005, vol. 146–159.
23, pp. 77–84. 11. R.M. Ger man, “Engineering Economics of Powder
3. R.M. German, Particle Packing Characteristics, 1989, Injection Molding Component Production: Part II,
Metal Powder Industries Federation, Princeton, NJ. Feedstock Costs”, P/M Science and Technology Briefs,
4. H. Su and D.L. Johnson, “Master Sintering Curve: A 2003, vol. 5, no. 3, pp. 11–16.
Practical Approach to Sintering”, J. Am. Ceram. Soc., 12. R.M. Ger man, “Engineering Economics of Powder
1996, vol. 79, pp. 3,211–3,217. Injection Molding Component Production: Part III,
5. R.M. German, Sintering Theory and Practice, 1996, John Production Costs”, P/M Science and Technology Briefs,
Wiley and Sons, New York. 2003, vol. 5, no. 4, pp. 14–22
6. R.M. German, Powder Metallurgy and Particulate Materials 13. R.M. Ger man, “Engineering Economics of Powder
Processing, 2005, Metal Powder Industries Federation, Injection Molding Component Production: Part IV, Price
Princeton, NJ. Sensitivity”, P/M Science and Technology Briefs, 2004, vol.
7. V. Richter and M.V. Ruthendorf, “On Hardness and Tough- 6, no. 1, pp. 5–10. ijpm
OUTSTANDING
TECHNICAL PAPER:
POWDERMET2007
The geometry of the spray
cone during atomization of
Ni31.5Al68.5 in a close-
*Reader in Solidification Processing, ***Research Fellow, ****Research Student, *****Senior Lecturer, University of Leeds, Institute for Materials
Research, Clarendon Road, Leeds, LS2 9JT UK; E-mail: a.m.mullis@leeds.ac.uk, **Technology Manager, CERAM Research, Queens Road, Penkhull,
Stoke-on-Trent ST4 7LQ UK
ciently low to be detectable by the human eye, a to use this geometry for this experimental study for
phenomenon reported in the literature6 and observ- a number of reasons. Firstly, the simple jet geome-
able during our atomization experiments. This is try means that the gas flow is amenable to relative-
attributed to fluctuations in the aspiration pressure ly straightforward numerical modeling. Secondly,
that result from the impinging gas jets. Specifically, unlike the convergent–divergent jets used to pro-
it has been suggested that it may be related to an duce supersonic gas flow, the simple cylindrical jet
oscillation between an open and closed wake down- can be operated over a wide range of pressures
stream of the focus of the gas jets.6,7 allowing us to investigate characteristics of the
Recently, significant progress has been made atomization process as a function of pressure.
towards understanding close-coupled gas atom- The melt was superheated by 200 K, giving a
ization utilizing high-speed imaging techniques.6,8 melt temperature prior to ejection of 1,813 K. At
These have proved to be particularly fruitful when this temperature the melt stream is sufficiently
combined with Fourier analysis of the resulting bright that filming can take place using the radi-
images.6 In particular, it has been reported that, ant light from the melt, even at high frame rates.
in addition to the low-frequency pulsing of the Consequently, no external light sources were
melt, a much higher-frequency oscillation6 or pre- used. The melt was ejected from the guide tube
cession9 of the jet is also observed. It has been under a constant overpressure of 40,000 Pa,
suggested that this may be a direct consequence while the gas-jet pressure was maintained at a
of irregular wetting of the melt-delivery nozzle, constant pressure of 3.5 MPa with pure argon.
producing a filament of melt that rotates around These operating conditions gave a melt-flow rate
the tip of the nozzle in a regular manner.10 If pre- of 15.75 × 10 -3 kg s -1 and a gas-flow rate of
cession is indeed due to the presence of an irregu- 48.65 × 10-3 kg s-1 at a GMR of 0.324.
lar rotating filament, this would suggest that Imaging of the melt spray cone was performed
instantaneously the metal sees only a small frac- using a Kodak Ektapro 4540mx high-speed digital
tion of the available gas jets, thereby dramatically motion analyzer, operating at a frame rate of
decreasing the GMR and potentially reducing the 18,000 frames/s. The motion analyzer was fitted
efficiency of the atomization process. As such, an with high-magnification optics which allowed full
understanding of the physical processes leading frame images (covering a distance ~5 cm from the
to this effect is important in order to optimize the die) to be imaged at a working distance of 25 cm.
spray atomization process, Each frame was 256 ¥ 64 pixels in size, with an
In this study, we describe high-speed digital eight-bit grayscale depth per pixel. Frames were
imaging experiments performed during the atom- stored separately as high-quality TIFF images
ization of Ni31.5Al68.5 (Ni-50 w/o Al, an industrial without interlacing in 1 Gb of fast memory, giving
catalyst, hereafter referred to as Raney-nickel), a total storage of 64,000 frames, which corre-
and the subsequent Fourier analysis of the image sponded to a total recording time of 3.64 s.
sequences. These were then compared with A typical sequence of five consecutive frames
images produced in a laboratory-scale analogue from the imaging is shown in Figure 2. Here,
atomizer that atomizes a water jet. because the imaging is performed using radiant
light from the hot melt, the spray cone appears light
METAL ATOMIZATION AND IMAGING METHODS
Atomization experiments were conducted at
CERAM Research on 6 kg batches of Raney-nickel.
A simple model die of the discreet jet type with 18
cylindrical jets arranged around a tapered melt-
delivery nozzle at an apex angle of 45° was used in
these experiments. The design, shown schematical-
ly in Figure 1, is similar to the USAG11 and Ames
HPGA-I4 designs that have been widely discussed
in the literature. Although this design is known to
be inefficient in atomizing the melt stream, as the
cylindrical jets produce choked flow and limit the
velocity of the gas jets to Mach 1, we have chosen Figure 1. Close-coupled atomization die and nozzle—schematic
spray cone, calculated from a weighted average of much lower frequency variation. The high-fre-
all the intensities in the image. For a symmetrical quency oscillation is shown on an expanded scale
spray cone in which the center of the spray is ver- in Figure 4(b), although this sequence covers only
tically below the nozzle, this procedure gives a 0.05 s of filming. In addition, on Figure 4(b), indi-
value for -j of 32. vidual mean intensities from consecutive frames
-
Both statistics, I and -j, have been calculated for are shown in order to demonstrate that the high-
the entire 3.64 s of filming using an automated frequency oscillation is unrelated to the frame
batch image processing system programmed in rate at which the camera is operating.
MATLAB,12 giving two time sequences each of which Figures 5(a) and 5(b) show the equivalent time
is 65,536 elements long. In addition, each time sequence for the weighted mean center position, -j.
sequence has been subjected to Fourier analysis. This shows a similar high-frequency oscillation
(again not resolved in Figure 5(a)), although in this
RESULTS: METAL ATOMIZATION EXPERIMENTS case there is little evidence of the low-frequency
-
An overview of the time sequence for the mean variation evident in the I data. The Fast Fourier
intensity is shown in Figure 4(a). This shows that Transforms (FFTs) of the time sequences for -I and
there is a high-frequency oscillation, which on - are given in Figures 6(a) and 6(b). Both show a
j
this scale is not resolved, superimposed upon a high spectral power with a sharp peak in the
Figure 4. Time-series of gray level intensity (a) over entire 3.64 s of a filming run and (b) in more detail over 0.05 s showing that the oscillation is
unrelated to the camera frame rate
Figure 5. Time-series of melt center position (a) over entire 3.64 s of filming run, (b) in more detail over 0.05 s showing that the oscillation is
unrelated to the camera frame rate
Figure 6. Fourier spectra of time-series corresponding to (a) gray level intensity and (b) position of center of jet
vacinity of a frequency ~360 Hz, which in the case lation is mirrored in the intensity, we believe that
of -j corresponds to the regular oscillation of the we are observing a steady rotation of the jet
spray about the vertical direction. The other fea- around the vertical direction, as previously
-
ture noted regarding the FFT analysis is that I has reported by Anderson.10 Periods of high intensity
considerable spectral power at low frequencies in the radiant light are attributed to the jet being
which is not apparent in the sequence for -j, which directed towards the viewing window in the atom-
corresponds to the irregular pulsing in the amount izer (along the viewing angle), while periods of low
of material at the die nozzle previously reported. intensity correspond to the jet being directed
This low-frequency spectral power is shown in away from the viewing window (180° from the
more detail in Figure 7; it is evident that the main viewing angle). Moreover, if this model is correct
-
power occurs at frequencies of 2.2 Hz, 2.7 Hz, 4.1 we would expect the time sequences for I and -j to
Hz, 5.5 Hz, 8.8 Hz, and 15.1 Hz, although be shifted in phase relative to each other, with the
numerous other frequencies are also present sug- peaks and troughs in -j occuring at 90° and 270°
gesting that the oscillation may be chaotic. from the viewing angle, Figure 8.
With regard to the apparent oscillation of the
spray about the vertical position, it is not possible
to determine whether this is due to a lateral oscil-
lation in the jet position or a rotation of the jet by
eye. However, because the frequency of the oscil-
uid-metal atomization. The pressure used in this l-1. Figure 12 shows a sequence of consecutive
run was 2.0 MPa, as opposed to 35 MPa during frames from the high-speed camera resulting from
atomization of Raney-nickel. Due to the lower this addition. All other parameters were held
density of water, the mass ratio of gas to atomized identical between the runs depicted in Figures 11
fluid is actually higher by a factor of 2.25. It is & 12. It is clear from these images that wetting of
clear, even from the raw images, that in this case the nozzle tip was achieved.
the fluid is non-wetting as it emerges directly from The corresponding Fourier analysis of the time-
the 2 mm dia. aperture in the nozzle. Moreover, series data from the entire image sequence is
when subject to Fourier analysis the images shown in Figures 13(a) and 13(b). Note also that
reveal no precession and indeed very little pulsing in this and all the Fourier analyses of the ana-
of the material delivered to the nozzle tip. logue atomizer there is an artifact at 100 Hz,
To determine whether this behavior, which is which is due to flicker in the illumination at a fre-
significantly different from the behavior of the quency of 2 x UK mains AC. Although some differ-
Raney-nickel when atomized, was due to the ences can be observed between these traces and
nature of the fluid or to the reduced operating the traces for Raney-nickel atomization, notably
pressure, we subsequently added a powerful sur- that the peak spectral power is (a) moved to a
factant (sodium dodecyl sulphate) to the sys- higher frequency and (b) is more diffuse, it is clear
tem’s water reservoir at a concentration of 0.1 g that there is now definite evidence of both preces-
sion and low-frequency pulsing. Consequently we
may conclude that precession of the spray jet
appears to be a direct consequence of the wetting
of the nozzle tip. In the absence of wetting, a
steady vertical jet breaking up into droplets is
observed.
Having demonstrated that the precession of the
spray cone can be recreated in the analogue atom-
izer, we have attempted to understand the factors
that influence the observed precessional motion.
Our first series of experiments was designed to
elucidate the dependence of the observed frequen-
cy of rotation on the gas pressure used for atom-
ization. To this end, high-speed video was taken of
the analogue atomizer running at pressures from
Figure 12. Sequence of images of atomization of water with 0.5 MPa to 4.0 MPa at intervals of 0.25 MPa.
surfactant to aid tip wetting. Each frame is separated by 1/18,000 s
Two of the resulting Fourier analyses characteris-
Figure 13. Fourier spectra of time-series corresponding to (a) gray-level intensity and (b) position of center of jet, for water atomized with surfactant
Figure 14. Fourier spectra of time-series corresponding to melt-center position (a) 7.5 bar and (b) 20 bar, showing virtually no dependence of fre-
quency of precession on operating pressure
tic of these experiments are shown in Figure 14(a) in the resulting flow dynamics. In particular, for
and 14(b). The two frequency spectra are virtually drilled holes we note a considerable eccentricity
identical and, indeed, over the pressure range con- on some of the holes (e = 0.92 is typical, corre-
sidered, we believe that to within experimental sponding to a variation in the hole diameter of 40
error there is no variation of precessional frequen- mm) whereas for the spark eroded holes this fig-
cy with atomization gas pressure. ure was significantly closer to 1 (e = 0.97), which
One variable that we have identified that does presumably, in part, reflects the fact that no
appear to have an effect on the nature of the pre- torque is imparted to the work piece during cut-
cession is the engineering tolerance applied dur- ting. Figure 15(a) and 15(b) show the Fourier
ing the die-manufacturing process. Two dies were spectra resulting from high-speed imaging experi-
manufactured to the same engineering drawings. ments on the analogue atomizer using these two
In one, the holes were produced by conventional dies, with all other parameters held constant. The
drilling, and in the other by spark erosion. atomizing-gas pressure in both cases was 4.0
Although notionally identical, the method of pro- MPa. The die produced by spark erosion produced
ducing the holes, which are close to the minimum spectra with (a) a much more tightly focused peak
diameter that can be produced by conventional at around 1,000 Hz than the die produced by
drilling, appears to make a significant difference drilling, and (b) the low-frequency components,
Figure 15. Fourier spectra of time-series corresponding to gray-level intensity for dies fabricated by (a) drilling and (b) spark erosion
Figure 17. Fourier spectra in gray level corresponding to atomization with different nozzle geometries: (a) Type 1, (b) Type 2, (c) Type 3, and (d)
Type 4
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specializes in production of high- steel, iron, low-alloy steel, copper, Low-volume, high-density, com-
performance bearings, structural brass, bronze, aluminum, nickel plex parts producer of ferrous-
and gear components using iron, silver, tungsten, 50/nickel/50 based components including soft
iron alloys, soft magnetic alloys, iron, copper-infiltrated steels and magnetics. Presses range from
stainless steel, bronze, brass and many specialty alloys. 65T to 1,000T, ISO 9001 certified.
custom materials. Types of parts include gears, In-house CNC equipment
magnetic pole pieces, cams, includes turning, boring, drilling,
thrust bearings, bushings, com- tapping, broaching. Also coining,
sizing, deburring, tool design, offering complete customer- room environments. Visit our Web
with CAD/CAM and Pro-E. Full focused solutions for high-per- site www.mottcorp.com for our
range of gauging inspection formance automotive complete line of porous metal
equipment, gear-inspection components. Extensive engineer- capabilities and products.
equipment including CMM. Fully ing research and development
automated from press to sinter. stands behind each and every NETSHAPE TECHNOLOGIES, INC.
Parts include stators, rotors, product. Metaldyne is the largest www.netshapetech.com
gears, counterweights, rings, etc. powder forged connecting rod A manufacture of engineered,
Aspect ratios reaching 10:1. provider in the world, manufac- complex, high-strength compo-
turing more than 50 million per nents using powder metallurgy
METALPÓ IND. E COM. LTDA. year. Metaldyne also designs and and metal injection molding!
www.metalpo.com.br manufacturers a variety of other NetShape is a Lean-focused,
Since its opening, in 1967, powder metal products for auto- global supplier with 5 PM and 1
Metalpó has had its activities motive manufacturers around the MIM operations worldwide,
pointed to powder metallurgy as a world. including a facility in Suzhou,
nonferrous powders and sintered China. Industry-leading technolo-
parts producer. Typical Metalpó METCO INDUSTRIES gies include high-performance
powder metallurgy products are www.metcopm.com materials, unmatched shape com-
self-lubricating bearings (bronze Metco Industries, Inc., has mold- plexity, tolerances and part size.
and iron), structural parts (iron, ing capabilities up to 400 ton Our innovative Conversioneeing®
stainless steel, bronze and brass) including multi-action for ferrous process and strong engineering
and metal powders (copper, and nonferrous applications. support offer unmatched value
bronze premix, prealloyed bronze Advanced secondary machining and support for converting parts
and tin). Using modern methods facility on site for quicker response to PM.
and quality management systems to customer demands. Celebrating
Metalpó has had since its early 25 years of PM excellence in the NOVAMET SPECIALTY
years the acknowledgment for automotive, lawn & garden, recre- PRODUCTS CORPORATION
highest level of quality. This has ational vehicle, healthcare and www.novametcorp.com
earned the Metalpó quality man- commercial markets. Novamet Specialty Products
agement system the ISO Corporation, a CVRD Inco
9001/2000 and ISO TS 16949 MI-TECH METALS, INC. Company, is a producer of spe-
assessments. www.mi-techmetals.com cialty metal and metal oxide pow-
Mi-Tech Metals, Inc., located in ders. Carbonyl nickel powders are
METAL POWDER PRODUCTS Indianapolis, Indiana, produces classified to narrow size ranges
COMPANY tungsten heavy alloy and copper for a variety of applications,
www.metalpowderproducts.com and silver tungsten composite including metal injection molding.
Metal Powder Products Company materials. Additional materials The Novamet family of Type 4SP
is an international provider of include tungsten carbide and nickel powders is the preferred
custom-engineered powder metal- pure molybdenum and tungsten. MIM industry choice. Four size
lurgy product solutions to cus- Mi-Tech maintains inventory to ranges are available, -400 mesh, -
tomers in a variety of industries. meet immediate requirements and 20 micron, -20 + 10 micron and -
MPP has developed a number of our extensive machine shop man- 10 micron.
innovations in material formula- ufactures parts to p????
tion, sintering, densification, pow- PHILIPS ADVANCED METAL
der metallurgy joining techniques, MOTT CORPORATION SOLUTIONS
and value-added secondary oper- www.mottcorp.com www.philips.com/ams
ations. MPP is the largest manu- Mott Corporation has been pro- Philips Advanced Metal Solutions,
facturer of powder metal viding unique solutions in the global development center for
aluminum structural parts in development and application of Philips Lighting, is a specialist
North America. porous metal media since 1959. producer of tungsten and molyb-
Mott partners with customers in denum components serving many
METALDYNE SINTERERED many industries to engineer and applications in various industries.
COMPONENTS design porous metal products We combine our technical expert-
www.metaldynepowdermetal.com with very specific tolerances and ise in alloying, material engineer-
Metaldyne, An Asahi Tec compa- attributes. Mott is ISO 9001:2000 ing and shaping technologies like
ny, is a world leader in the Certified and also maintains lasering & MIM with our underly-
Powder Metallurgy (PM) industry, Class 100 and Class 10,000 clean ing philosophy—“designed around
you.” This enables us to deliver steels, high-shape-complexity turer of highly engineered techno-
the refractory metal products that MIM and PM, steel-bonded car- logically differentiated powertrain
you need in a reliable and cost- bides, tungsten carbides, high- components, systems, and
effective way. Please visit conductivity copper, and a wide assemblies.
www.philips.com/ams variety of other specialties. Come
visit our Web site at www.psmin- STERLING SINTERED
PLANSEE USA dustries.com. TECHNOLOGIES
www.plansee-usa.com www.sterlingsintered.com
Schwarzkopf Technologies is now SCHWARZKOPF Sterling Sintered Technologies, an
PLANSEE USA and continues to TECHNOLOGIES LLC ISO 9001-2000 company, is an
deliver the world’s best furnace www.plansee-usa.com innovative leader in the manufac-
solutions. Schwarzkopf Technologies is now ture of powdered metal compo-
Schwarzkopf Technologies is PLANSEE USA and continues to nents. The Sterling team works
known within the U.S. and deliver the world’s best furnace with customers to concurrently
Canada as the industry leader in solutions. design parts and processes for
developing, designing, and manu- Schwarzkopf Technologies is them. This approach has allowed
facturing high-temperature fur- known within the U.S. and Sterling Sintered and its cus-
nace products to perform better Canada as the industry leader in tomers to develop new applica-
and last longer. developing, designing, and manu- tions and push PM technology to
As an independent subsidiary facturing high-temperature fur- the forefront of our industry. Let
we have contributed to the suc- nace products to perform better Sterling Sintered do this for you.
cess of the PLANSEE Group— and last longer. For additional information explore
going forward we will be operating As an independent subsidiary our Web site at www.sterlingsin-
jointly under one name. we have contributed to the suc- tered.com
Our customers will be able to cess of the PLANSEE Group—
benefit even more from synergies going forward we will be operating VOLUNTEER SINTERED
generated within the Group, jointly under one name. PRODUCTS, INC.
demonstrating our uncompromis- Our customers will be able to
www.volunteersintered.com
ing commitment to delivering the benefit even more from synergies
generated within the Group, Established 1981, family
highest-quality products. owned/operated
demonstrating our uncompromis-
ing commitment to delivering the Press Range 20–200 Ton
PLANSEE SE Materials include iron, prealloyed
highest-quality products.
www.plansee-group.com steels, brass, bronze, stainless
The Plansee Group is one of the SMC POWDER METALLURGY Parts include gears, bearings,
world’s leading suppliers of pow- www.smcpowdermetallurgy.com structurals, cams, etc.
der metallurgical products and Secondary operations – copper
components. The industrial port- SMC Powder Metallurgy is a 57- infiltrating, brazing, coining, bur-
folio of Plansee Group is struc- year young PM manufacturer, nishing, drilling, tapping, turning,
tured into three divisions: diverse in the materials supplied, oil impregnation, deburring
PLANSEE High Performance the business markets served, and Inspections/QC ISO 9001 certi-
Materials, CERATIZIT Hardmetals the parts manufactured. SMC fied, Rockwell hardness, gear
& Tools and PMG PM–Products. Powder Metallurgy manufactures tester, optical comparator, surface
Ignoring differing shares of the in a modern 112,000 sq. ft. facili- finish, crush tester
ownership, the Group achieved ty located in Galeton, Specialties complex, close-toler-
worldwide sales of over 1.4 billion Pennsylvania, dedicated solely to ance parts, short lead times for
euros in the 2006/07 fiscal year, the manufacturing of powder tooling and production
and employed a total of 8,800 metal components. SMC Powder
people. www.plansee-group.com Metallurgy is TS-16949 certified WESTERN SINTERING CO. INC.
company. For additional detail,
www.westernsintering.com
PSM INDUSTRIES, INC. please visit our Web site at
www.smcpowdermetallurgy.com. Manufacturer of custom powder
www.psmindustries.com metal parts. Presses to 300 tons.
A symphony of PM solutions. Our STACKPOLE LIMITED Steel, stainless steel, and copper-
6 manufacturing divisions will www.stackpole.com base materials.
find an answer to your most Complete secondary facilities and
pressing PM problem. Specialties Our mission is to be recognized heat treat in-house.
include high-dense high-speed as the world's premier manufac-
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