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STRUCTURE AND PROPERTIES

OF ULTRAHIGH-STRENGTH
STEELS

A symposium sponsored by the


METALLURGICAL SOCIETY OF AIME and the
AMERICAN SOCIETY FOR TESTING AND MATERIALS
Cleveland, Ohio, Oct. 22, 1963

Reg. U. S. Pat. Off.

ASTM Special Technical Publication No. 370

Price $11.00; to Members $7.70

Published by the
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia 3, Pa.

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© by American Society for Testing and Materials 1965

Printed in Baltimore, Md.


March, 1965

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FOREWORD

The papers in this volume were presented at a Symposium on Steels With


Yield Strengths Over 200,000 psi sponsored by the Panel on Structural
Materials for Airframes and Missiles of the ASTM-ASME Joint Committee
on Effect of Temperature on the Properties of Metals, and the Structural
Materials Committee, Institute of Metals, Metallurgical Society of AIME.
The Symposium was held on Oct. 22, 1963, in Cleveland, Ohio.
F. M. Richmond, of Universal-Cyclops Steel Corp., and J. W. Welty, of
Solar Aircraft Co., were the chairmen of the morning session. E. E. Reyn-
olds, of Allegheny Ludlum Steel Corp., and J. J. Heger, of U. S. Steel Corp.,
presided over the afternoon session.

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iii
NOTE—The Society is not responsible, as a body, for the statements
and opinions advanced in this publication.

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CONTENTS

PAGE
Introduction 1
Relationships Between Microstructure and Toughness in Quenched and Tempered
Ultrahigh-Strength Steels—A. J. Baker, F. J. Lauta, and R. P. Wei 3
Discussion 23
Relationships Between Structure and Properties in the 9Ni-4Co Alloy System—
J. S. Pascover and S. J. Matas 30
Discussion 45
High-Strength Stainless Steels by Deformation at Room Temperature—S. Floreen
and C. R. Mayne 47
An Evaluation of the 18Ni-9Co-5Mo Maraging Steel Sheet—D. L. Corn 54
The Metallurgy and Properties of Cold-Rolled Am-350 and Am-355 Steels—T. H.
McCunn, G. N. Aggen, and R. A. Lula 78
Discussion 93
Fracture Micromechanics in High-Strength Steels—Bani R. Banerjee 94
Discussion 116
The Effect of Solidification Practice on the Properties of High-Strength Steels—
C. M. Carman, R. W. Strachan, D. F. Armiento, and H. Markus 121
Discussion 143
High-Strength Steel Forgings—H. J. Henning 147
Ausform Fabrication and Properties of High-Strength Alloy Steel—W. W. Ger-
berich, A. J. Williams, C. F. Martin, and R. E. Heise 154
Thermomechanical Treatments Applied to Ultrahigh-Strength Bainites—D. Kalish,
S. A. Kulin, and M. Cohen 172
Discussion 205
Ultrahigh-Strength Steel Fasteners—A. C. Hood and R. L. Sproat 208
Discussion 220

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V
RELATED ASTM PUBLICATIONS

Properties of Basic Oxygen and Open Hearth Steels, STP 364 (1963).
Stress Corrosion Cracking of Austenitic Chromium-Nickel Stainless Steels, STP 264 (1960).
Chemical Composition and Rupture Strengths of Super-Strength Alloys, STP 170-C
(1964).

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vi
STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

INTRODUCTION
The increasing demands of the military utilization of higher strengths that are
for improved performance of structural now obtainable.
materials for space, land, and deep ocean The papers presented at this sym-
environments has resulted in an intensive posium included descriptions of new
activity in the development, evaluation, steels (or new concepts for making
and prototype testing of a broad range steels) having yield strengths in excess
of materials including oxides, carbides, of 200,000 psi, and good ductility and
aluminum, titanium, and even gold. A toughness. Specifically mentioned are
significant portion of this activity has the new maraging steels, higher strength
been devoted to high-strength steels. and higher toughness martensitic steels,
Recognizing the scope of this activity steels strengthened by thermomechanical
and the need to assemble into one semi- treatments, and steels strengthened by
nar the more recent advances in the cryogenic treatments. Progress has been
development and application of high- made in the understanding of the illu-
strength steels, the Panel on Structural sive property known as toughness, and
Materials for Airframes and Missiles two papers are presented summarizing
of the Joint Committee of ASTM and the state of art in this area. Also the
ASME, and the Structural Materials effect of melting and processing on high
Committee of the Institute of Metals strength properties, the characteristics
Division of the Metallurgical Society of specific products—namely, forgings
of AIME, organized this Symposium and fasteners—and the fabrication of the
on Steels With Yield Strengths Over new high-strength steels are discussed
200,000 psi. in detail.
Until recently, steels having yield In reviewing the information con-
strengths in excess of 200,000 psi were tained in this Symposium, the reader
not considered suitable as materials of is reminded that steels having the high
construction, because fabrication and yield strengths discussed herein will not
inspection techniques were not suffi-
always be confined to military applica-
ciently sophisticated to permit full
tions. The American economy demands
utilization of these high strengths, which
at that time were accompanied by low that such steels eventually will be used
ductility and low toughness. Recently, for pressure vessels as well as for struc-
however, major developments have tural members in such prosaic applica-
occurred not only in alloy development, tions as buildings and bridges, and
which has permitted the achievement perhaps even for the structural members
of higher levels of ductility and tough- of the transportation vehicles that the
ness, but also in inspection and fabrica- reader will be using as a personal means
tion techniques that permit the full of conveyance within the next 10 years.

1
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RELATIONSHIPS BETWEEN MICROSTRUCTURE AND TOUGHNESS IN
QUENCHED AND TEMPERED ULTRAH1GH-STRENGTH STEELS
BY A. J. BAKER,1 F. J. LAUTA,1 AND R. P. WEI1

SYNOPSIS
An investigation was made of a number of 0.30 and 0.40 per cent carbon
alloy steels to determine the relationships between their fracture toughness
properties and their internal microstructures. The plane-strain fracture tough-
ness of the steels was measured after tempering quenched material in the tem-
perature range 300 to HOOF. A thin section transmission electron micros-
copy study was carried out on the tempered materials.
From the fracture toughness studies it was concluded that all the materials
behaved similarly and that alloying elements (carbon and silicon) had little
influence on the general relationship between tensile strength and toughness in
these fully hardenable steels. It was found that the fracture toughness remained
low at low tempering temperatures but improved rapidly once a critical tem-
pering temperature, characteristic of the particular steel, was reached.
The microscopy study showed that major microstructural changes occurred
in the tempering range where the rapid increase in toughness was observed.
At low tempering temperatures the defect structure of the as-quenched mar-
tensite remained unchanged, and continuous films of carbide were formed in
the boundaries of the martensite. In the critical tempering range the carbide
films were spheroidized and the defect structure of the matrix removed or
modified by recovery processes. On the basis of these observations, it was con-
cluded that the low fracture toughness of the steels in a lightly tempered condi-
tion was due to their high defect densities and the presence of carbide films at
boundaries. Only when these features were removed or modified did toughness
increase.

In recent years there has been a grow- loy steels with carbon contents in the
ing demand for materials of very high range of 0.3 to 0.5 per cent. Quenched
strength for aerospace applications such and tempered low-alloy steels already
as rocket motor casings. This demand has have many uses both as structural mate-
stimulated research aimed at the de- rials and, at higher strength levels, as ma-
velopment of ultrahigh-strength steels, chine parts. When their yield strengths
that is, steels with useable yield strengths are raised to . the strength level men-
of more, than 200,000 psi; and an im- tioned, there is the major problem of
portant part of this research has been the maintaining an adequate level of tough-
study of quenched and tempered low-al- ness that will meet the design require-
mentS
i Technologists, U. S. Steel Corp., Applied Pkced UP°n them'
Research Laboratory, Monroeville, Pa. The present investigation was carried
3
4 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

out to determine the fracture-toughness were hot-rolled to a 1-in. plate after be


capabilities of these steels at the ultra- being heated to 2300 F. Steel D was cast
high-strength level and to attempt to as a 300 Ib, 8 by 8-in. ingot that was sub-
relate their properties to microstructure. sequently reduced by rolling to a 1-in.
The investigation was based on three 0.40 plate.
per cent carbon steels and one 0.30 per Oversize 0.505-in.-diameter tension
cent carbon steel, and the effects of specimens were rough-machined from the
both chemical composition and temper- plate or bar materials, austenitized for
ing treatment on plane-strain fracture £ hr at 1700F and oil-quenched. The
toughness were examined. specimens were then tempered for times
To study the relationship of micro- up to 4 hr in the temperature range 400
structure to fracture toughness, a parallel to HOOF and air-cooled. After heat
metallographic investigation was made treatment, the specimens were finish-
using thin-section transmission and machined to 0.505-in.-diameter tension
replica electron-microscopy techniques. specimens.

TABLE 1—CH EMICJ*.L CO1VEPOSI TIONS OF SI^EELS INVES3TIGArFED,


PER CEN1

Steel C Mn P S Si Ni Cr Mo V Al

A, 4340 commercial 0.39 0.74 0.019 0.026 0.27 1.79 0.89 0.26 0.044
B 4340 CEVR° 0.43 0.77 0.009 0.008 0.27 1.16 0.73 0.26 0.03
C 300M CEVR 0.42 0.74 0.005 0.006 1.60 1.87 0.83 0.37 0.10 0.092
D, experimental heat 0.31 0.84 0.007 0.009 1.59 2.04 2.04 0.51 0.055 0.055

" Consumable Electrode Vacuum Remelted.

Materials and Method: Notched tension specimens were pre-


pared by rough machining 6-in.-long
The chemical composition of the four cylinders of 0.8 or 1.05-in.-diameter from
steels investigated is shown in Table 1. the plate or bar material. These speci-
The composition of steels A and B is mens were given heat treatments identi-
within the specification limits for AISI cal with those given the smooth tension
4340 steel, except that steel B is slightly specimens. After heat treatment, the
deficient in nickel. The lower phosphorus specimens were machined to either 0.750
and sulfur content of steel B, compared or 1.00-in. diameter and notched. The
to that of steel A, is probably a result of depth of the machined notch was chosen
the consumable-electrode vacuum-remelt so that after a subsequent introduction
process by which it was produced. Steel of a 0.030-in.-deep circumferential fa-
C is a high-silicon modification of AISI tigue crack, the area of the remaining
4340, with a small vanadium addition, uncracked material would be 50 per cent
and it corresponds to the material com- of the gross cross-sectional area. Fatigue
monly designated as 300M. Steel D is an precracking was accomplished in an en-
experimental laboratory-made material. gine lathe, the tailstock being offset to
Steel A was received as l^-in.-diameter introduce a bending moment.
annealed bar stock, and test specimens Specimens for transmission electron
were machined directly from this. Steels microscopy were taken from the broken
B and C were received as 7- and 5-in. tension specimens. Small pieces | by \ by
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blooms, respectively, and these blooms 0.1-in. thick were cut out and ground on
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BAKER ET AL ON MICROSTRUCTURE AND TOUGHNESS 5
TABLE 2—MECHANICAL PROPERTIES—FRACTURE TOUGHNESS
OF STEELS INVESTIGATED.

Steel A Steel B Steel C Steel D


Tempering
Tempera-
tures, F YS,a TS,a 9ic in.- YS, TS, Sic in.- YS, TS, Sic in.- YS, TS, Sic in.-
ksi ksi lb/in.2 ksi ksi lb/in.2 ks ksi lb/in.2 ksi ksi lb/in.2

400 229 301 20 214 296 /48


18 152

500 234 280 20 223 263 43 246 304 48 205 262 88


20 45 90
24
26

550 2706 18
16

600 225 261 21 222 256 (51 249 296 (52 212 262 87
23 \55 \50 91
83
700 215 242 45 212 238 129 254 297 /49 215 259 /89
39 125 \53 \84
142
139
750 2306 48 2556 (97
53 186
51

800 202 218 105 193 208 179 206 269 55


114
117
179

900 186 199 193 255 [78 179 242 87


J73
[59
975 230fr 98
121
1000 165 180 212 242 !08 184 225 151
99 122
100
1050 209 232 107 174 196
214
1100 170 193
a
YS = yield strength; TS = tensile strength.
6
Extrapolated value.

a wet belt to a thickness of about 0.020 successively in 1:10 mixture of perchloric


in. These specimens were then chemically acid and methyl alcohol and a solution of
polished in a warm solution of 50 per cent chromic acid in acetic acid to prepare
phosphoric acid (H3PO4) and 50 per cent thin foils suitable for transmission elec-
hydrogen peroxide (H202) to reduce their tron microscopy (I).2 Formvar-carbon
thickness to less than 0.005 in. This
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boldface 2015 in parentheses refer
0.005-in. material was electropolished to the list of references appended to this paper.
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6 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

FIG. 1—Effect of Tempering Temperature on Strength and Fracture Toughness of Steels A and B.

FIG. 2—Effect of Tempering Temperature on Strength and Fracture Toughness of Steels C and D.

replicas for electron microscopy were ture surfaces with electrodeposited


prepared both from heat-treated material nickel, sectioning perpendicular to the
and from the fracture profiles of the fracture surface, and polishing the profile
broken notched rounds. The fracture pro-" by standard metallographic preparation
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BAKER ET AL ON MICROSTRUCTURE AND TOUGHNESS 7

RESULTS It is important to note the effect of


notch acuity on plane-strain fracture-
Mechanical Properties: toughness evaluations. The effect of tem-
Table 2 is a compilation of the strength pering temperature on plane-strain frac-
and toughness properties of the steels ture toughness shown in Figs. 1 and 2 can
examined. The effect of tempering treat- be obtained only with fatigue-precracked
ment on yield strength, tensile strength, specimens. To emphasize this point, a
and plane-strain fracture toughness is comparison is made in Fig. 3 between the
shown in Figs. 1 and 2. By comparing the notched-tensile strengths obtained with
properties of steels A and B with those of fatigue-precracked specimens and those
steels C and D at a given tempering obtained with specimens having ma-
temperature, the influence of silicon and chined notches with a 0.0015-in. root

FIG. 3—Schematic Showing Effect of Notch Acuity on Fracture Toughness Test Results.

chromium in retarding the rate of radius. The tests were carried out on an
tempering can clearly be seen. experimental 0.40 per cent carbon, low-
All four steels show a similar type of alloy steel with a composition similar to
behavior in the effect of tempering treat- that of 300M steel. With machined
ment on plane-strain fracture toughness. notches, the variation of notched tensile
In each case, the fracture toughtness re- strength with tempering treatment fol-
mains low and almost constant at low lows a variation similar to that of yield
tempering temperatures but undergoes strength, which suggests that this type
a sharp increase in a critical tempering of behavior is controlled by the initiation
range characteristic of the particular of a crack at the root of these relatively
steel. The actual level of fracture tough- dull notches. Apparent values of Slc com-
ness at low tempering temperatures de- puted on the basis of these results would
pends on the individual steel composi- indicate a more complex variation of 9ic
tions. Those with lower phosphorus and with tempering treatment than is ac-
sulfur contents have a higher level of tually the case. Using fatigue precracked
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toughness.
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8 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

characterized by a region of almost con- the relationships exhibited by steels B


stant and low fracture toughness at low and C in Fig. 4. These steels differ in sili-
temperatures and a region of rapidly con content, having 0.25 and 1.50 per
increasing fracture toughness above a cent, respectively, but it is apparent that
critical tempering temperature. the higher silicon content of steel C has
The results shown in Figs. 1 and 2 indi- not led to any improvement in the bal-
cate that the critical tempering tempera- ance of fracture toughness to strength
tures, above which fracture toughness over that attainable in steel B.
increases rapidly, are dependent on the The systematic relationships shown in
alloy content of the steels. Silicon has a Fig. 4 created interest in the associated
particularly strong influence in that, for microstructural changes, and conse-
steels A and B, containing 0.25 per cent quently an electron metallographic study

FIG. 4—Relationship Between Plane-Strain Fracture Toughness and Tensile Strength for Four
Steels.

silicon, the critical temperature is 600 F, was made on these materials after various
whereas for steels C and D, containing tempering treatments. It was possible to
1.50 per cent silicon, the critical tempera- consider all four steels as a group despite
ture is 900 F. their varying composition, and the
So that the four steels can be compared metallographic study was further facili-
at equal strength levels, the data shown tated by the fact that each steel exhibited
in Figs. 1 and 2 are replotted in Fig. 4 two distinct levels of fracture toughness
with fracture toughness as a function of above and below the 240,000-psi strength
tensile strength. The sharp change in level. It was possible, therefore, to predict
fracture-toughness behavior is again ap- the critical tempering-tfemperature range
parent: above a tensile strength level of within which important structural
about 240,000 psi the steels have low changes were likely to occur. Thus, while
fracture toughness, whereas at lower it was still necesasry to examine the
tensile strengths the toughness increases. structures developed throughout the
A further conclusion
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BAKES ET AL ON MicsosTRuorasE AND TOUGHNESS 9

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5—Electron Micrographs of Steel D Specimens Anstenitized at 1700 F and Oil-Quenched
.XSQ.OQO).
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10 STKUCTUSE AND PKOPERTIES OF ULTRAHIGH-STKENGTH STEELS

(top) X 50,000
(bottom) XMon
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FIG. 6—Electron
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BAKER ET AL ON MICROSTRUCTURE AND TOUGHNESS 11

investigation of microstructure could be twin-boundary direction, which suggests


concentrated on the narrow range likely that they may nucleate in the twin
to be significant. boundaries. In addition, there are a num-
ber of smaller particles that lie across the
Microstructure: twins and often link together the twin-
The metallographic studies showed boundary particles. These smaller parti-
that all four steels underwent similar cles have a ragged appearance and are
microstructural changes during temper- probably nucleated on dislocations. Other
ing. To avoid unnecessary repetition, a particles are formed at the martensite
detailed discussion of the effects of tem- boundaries, and these also connect with
pering on microstructure will be given for adjacent particles in the matrix.
steel D only; discussion of the results for The precipitate particles observed are
steels A, B, and C will be restricted to a feature of the martensite produced in
those parts of the temperature sequence thick-section, oil-quenched material, and
in which important changes occurred, or they do not appear in thin-section, water-
in which their behavior differed from quenched specimens. This fact would
that of steel D. suggest that the particles are created by
The martensitic structure of steel D is auto tempering during quenching; since
shown in Fig. 5. The martensite has a the Mg temperature of steel D is rela-
predominantly plate-like morphology, tively low (about 550 F), the particles
with rrfany of the plates lying in parallel are probably e-carbides, as this is the
groups. The plates are about %n wide and carbide formed at low tempering temper-
about 4/i long. Their thickness is difficult atures (4). However, it was not possible
to estimate accurately because of the to identify them by selected-area elec-
uncertainty in knowing the angle at tron diffraction using either thin foils or
which a plate meets the foil surface; but extraction replicas; in the thin foils, the
the thinnest plates measured were about precipitate volume fraction was too small
1000 A. Two types of lattice defect are to produce an identifiable diffraction
present within the plates, namely, a high pattern, whereas with extraction replicas
dislocation density and many microtwins. the density of particles was insufficient to
The dislocation density is about 10" obtain a pattern. The difficulty experi-
lines/cm2, which is comparable with that enced in extracting these particles,
of heavily cold-worked metals (2). In coupled with the fact that they are small
many areas of the foils, the dislocation in size and general shape, suggests that
density is too high to resolve the in- they may have a high degree of coherency
dividual dislocations, and a mottled type with the matrix.
of contrast results instead. The micro- Tempering steel D at 600 F resulted in
twins are closely spaced at about 200 A the formation of further quantities of
and are as narrow as about 100 A in precipitate. The preferred sites for pre-
width. The twinned structure observed is cipitate formation were the martensite
similar to that found in high-carbon, plate boundaries and the twin bounda-
plain-carbon steels (3). ries. The structure is shown in Fig. 6
In addition to dislocations and micro- (top), where the martensite boundary pre-
twins, the martensite contains many cipitate can be seen to constitute an al-
small precipitate particles as shown in most continuous film. The precipitate at
Fig. 5 (bottom). The precipitate particles this tempering temperature had sufficient
are small rods,
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diameter, that usually
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12 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

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FIG. 7—Electron
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BAKER ET AL ON MICROSTRUCTURE AND TOUGHNESS 13

as 6-carbide. The twin-boundary precipi- terial, do not appear in the tempered


tate at this stage of tempering is about structure and must therefore dissolve as
500 A wide and must have incorporated the larger particles grow.
several twins during its sidewise growth. On tempering at higher temperatures,
At high magnification, both the martens- up to 900 F, increasing quantities of car-
ite boundary and the twin-boundary bide were formed, but above 1000 F sev-
precipitates exhibit a substructure of fine eral important changes occurred.
parallel striations (Fig. 6 (bottom)), which Figure 7 (top) shows the 1050-F tem-

FIG. 8—Electron Micrograph of a Steel D Specimen Tempered 4 hr at 1050 F (X 100,000).

may be due to fine-scale faulting within pered structure, and it can be seen that
the carbide structure. The c-carbide on the carbide precipitates are discrete
the twin boundaries probably retains spheroidized particles at the martensite
some coherency with the matrix at this boundaries, rather than continuous films.
stage of tempering, and the faulting The carbide formed at this tempering
could be ihe result of a strained mode of temperature was identified as iron car-
growth. Carbides are known to contain bide (Fe3C). The original martensite
strains when formed at low tempering boundaries can still be seen between the
temperatures (5). The small precipitate carbides, and the martensite retains its
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particles linking the twin boundaries, plate-like morphology.
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14 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

at 1050 F was that the initial, randomly planation for the spheroidal morphology
tangled dislocation mass showed evidence of the carbide precipitate formed. Since
of some recovery for the first time. In Fe3C has a lower density than iron, a
Fig. 7 (bottom), which is a higher mag- mass transfer within the matrix is neces-
nification area than that of Fig. 7 (top), sary if the Fe3C particles are to grow
groups of regular, fine-mesh, dislocation and change shape rapidly. This mass
networks can be seen within the marten- transfer requires the diffusion of iron
site. The formation of these dislocation atoms within the matrix and this, in

FIG. 9—Electron Micrograph of a Steel C Specimen Tempered 1 hr at 800 F (X 80,000).

networks indicates that dislocation climb turn, is controlled by vacancies. Hence,


and consequent recovery are occurring at major changes in carbide morphology can
this tempering temperature. Since dis- only occur at a temperature sufficiently
location climb is a vacancy-controlled high to provide a large supply of vacan-
process, the changes in dislocation ar- cies. Below this temperature, the carbides
rangement also indicate that vacancy are restricted to easy nucleation sites,
generation and migration must be rapid such as boundaries, and a slow and
at this temperature. relatively strained type of growth along
The availability of vacancies at this the boundaries results.
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tempering temperature provides an ex- The spheroidization of the martensite
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BAKER ET AL ON MICROSTRTJCTURE AND TOUGHNESS 15

boundary precipitates is accompanied by The microstructural changes in steel C


a similar spheroidization of the twin followed a similar sequence to those in
boundary precipitates, as shown in Fig. Steel D. The martensite contained all the
8. In addition, it can be seen that, as the features already discussed for steel D,
twin boundary precipitate spheroidizes and at tempering temperatures up to
and leaves a region of matrix, the traces 800 F, progressively thicker precipitates
of the twin boundaries tend to disappear of carbide were formed both at the mar-
also. This disappearance of the twin tensite boundaries (Fig. 9) andwithin the

FIG. 10—Electron Micrograph of a Steel C Specimen Tempered 1 hr at 800 F (X 140,000).

boundaries suggests that the twin bound- twins (Fig. 10). Again, as in steel D, there
ary and matrix-carbide interface are was no change in dislocation arrange-
closely coupled at this tempering tem- ment up to this temperature. At 1000 F,
perature. The coupling probably comes however, spheroidization of the Fe3C
about by the incorporation of the twin formed along the martensite boundaries
boundary into the precipitate interface and twins occurred, and dislocation re-
as the precipitate loses coherency during covery resulted in network formation.
growth. Once incorporated, the twin The spheroidization of the carbides at
boundaries disappear as the carbides the martensite boundaries is shown in
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withdraw from a region
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16 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

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FIG. 11—Electron
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BAKER ET AL ON MICROSTRUCTURE AND TOUGHNESS 17
at the twin boundaries are shown in Fig. vated dislocation climb results in the
11 (bottom). formation of networks which are, in ef-
In steels A and B, the changes in fect, low-angle boundaries. As the
microstriicture followed a similar se- networks develop, the martensitic matrix
quence to that observed in steels C and is divided into many small subgrains of
D, but the changes occurred at lower similar orientation. With further temper-
tempering temperatures. At the lowest ing, the subgrain boundaries migrate to
tempering temperature, a continuous become higher angle boundaries and, ul-
film of e-carbide was produced at the timately, a well-developed fine-grained
martensite and twin boundaries, and at structure is developed within the mar-

FIG. 12—Electron Micrograph of a Steel A Specimen Tempered 1 hr at 600 F (X50,000).

higher tempering temperatures (600 F) tensite matrix. The creation of the sub-
the e-carbide was replaced by Fe3C (Fig. grain structure shown in Fig. 13 (bottom)
12). At 800 F the boundary Fe3C began is thus the initial stage in the recrystal-
to spheroidize (Fig. 13 (top)), and the lization of the steel.
matrix showed signs of the changes re- At higher tempering temperatures, the
sulting from dislocation recovery (Fig. 13 recrystallization process proceeds more
(bottom). rapidly. Figure 14 shows the advanced
The structure shown in Fig. 13 (bot- stage reached at 1000 F.
tom) illustrates an early stage in the
microstructural changes produced in the Fracture Profile Metallography:
matrix as dislocation recovery and migra- Figure 15 shows replica micrographs
tionCopyright
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18 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

Copyright
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A Specimen EST12015
Tempered hr at 800 F.
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BAKER ET AL ON MICROSTRTJCTURE AND TOUGHNESS 19

steel C, tempered at 600 (top) and 1000 F bide. In the higher-temperature tempered
(bottom). It can be seen that, for material material the profile shows evidence of
in the 600-F tempered condition, the greater plastic deformation and tearing
fracture path tends to contain many more along the fracture path, and the fracture
flat facets than that for material tem- path shows little tendency to follow any
pered at 1000 F; and these facets are distinct microstructural feature.

FIG. 14—Electron Micrograph of a Steel A Specimen Tempered 1 hr at 1000 F (X60,000).

often oriented parallel to the carbides at DISCUSSION


the martensite boundaries or twin bound-
aries. The fracture surface of the steel The mechanical property results show
tempered at 1000 F has a more roughened that both tensile strength and fracture
appearance, and there is no obvious cor- toughness are closely related to temper-
relation between the fracture path and ing treatment. In each of the steels in-
the microstructure. It appears from the vestigated, there is a a decrease in tensile
fracture profiles that cracks propagate in strength as the tempering temperature is
the low-temperature tempered material increased, but the fracture toughness re-
along a succession of short, almost mains low until a critical temperature
straight paths and that these paths tend range is reached within which it increases
to follow suitably
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20 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

FIG. 15—Fracture Profiles of Steel C Tempered 1 hr at 600 and 1000 F (X 10,000).

B, the fracture toughness improves for The metallographic structures show


temperatures above 600 F, whereas in the that the sharp rise in fracture toughness
higher-silicon steels C and D the increase occurs at a temperature range in which
is retarded
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BAKER ET AL ON MICROSTRTJCTURE AND TOUGHNESS 21

the spheroidization of carbide precipitate ties of carbides and dislocations remain


particles, and (2) the reduction or redis- relatively high, so that the tensile
tribution of the defect structure of the strength does not fall sharply, as the
martensite. toughness increases. The phenomenon is
It is possible to correlate the changes essentially one of redistribution of micro-
in mechanical properties with the struc- structural features rather than of their
tural changes by considering qualita- complete removal.
tively the possible influences of micro- While the observations on fracture
structure on properties. In the marten- path emphasize the embrittling role of
sitic condition, the steels exhibit a type boundary carbides, the potential tough-
of microstructure in which yielding and ening influence of dislocation recovery
general ductility are likely to be very may be equally valuable. By freeing large
limited. The martensite is tetragonal be- areas of the matrix from their defect con-
cause of the carbon contained in the lat- tent and by generating a fine-grained
tice, and the transformation produces a substructure, the dislocation changes are
high dislocation density. In addition, the likely to produce some beneficial effect on
many twin boundaries present will act as toughness.
barriers to dislocation movement. It has been shown that silicon has a
On tempering at low temperatures, strong influence in retarding the major
little relief from the embrittling features tempering reactions that lead to the de-
can be obtained; the metastable martens- velopment of high fracture toughness.
ite begins to decompose and the tetra- As already discussed, the microstruc-
gonality is consequently reduced. How- tural changes observed as carbide sphe-
ever, the carbon liberated is utilized in roidization and dislocation recovery are
the formation of almost continuous films vacancy - controlled processes and can
at the martensite boundaries and twin only occur at temperatures high enough
boundaries. These films appear to act as to provide rapid vacancy formation and
preferred paths for crack propagation migration. If silicon retards tempering,
through the structure, either by provid- it would seem, at first sight, that it might
ing adjacent weak zones in the matrix or exert its influence by inhibiting the neces-
by fracturing themselves. Consequently, sary vacancy generation or mobility. A
while the tensile strength of the marten- more likely explanation is provided by
site falls, there is no accompanying in- (1) the well-known fact that silicon does
crease in fracture toughness. not form a simple carbide in steels, be-
In the critical tempering range, several cause of the instability of silicon carbide
changes occur that lead to improved with respect to iron carbides, and (2) the
toughness. First, continuous films of car- recent observation that silicon is in-
bide are no longer produced at the mar- corporated into the e-carbide formed
tensite and twin boundaries; instead, dis- during the early stages of tempering (6).
crete rounded particles are formed there. The presence of silicon in these carbides
Second, the dense dislocation array is is likely to reduce the rate at which they
modified by recovery so that larger areas can grow and hence to delay the processes
of defect-free matrix are developed. that will lead eventually to spheroidiza-
Third, the twin boundary structure dis- tion.
appears with the spheroidization of the As long as the carbide dispersion re-
twin boundary carbides. All these mains stabilized and finely dispersed, and
changes are likely
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toughness. However, the
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22 , STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

location array will have little freedom to only when certain important structural
climb and recover. Thus, the carbide dis- changes have occurred.
persion could, in effect, stabilize the dis- 4. The microstructural changes that
location arrangement and prevent any are of major importance in the improve-
general migration. ment of fracture toughness are (a) the
elimination of embrittling carbide films at
CONCLUSIONS boundaries by spheroidization, and (b)
From the investigation of the changes the redistribution and removal of the lat-
in mechanical properties that occur on tice defect structure by recovery proc-
tempering and the accompanying esses.
changes in microstructure, it is possible 5. The retarding influence on temper-
to draw the following conclusions: ing exerted by silicon delays the develop-
1. In the steels investigated, the plane- ment of good fracture toughness by in-
strain fracture toughness shows a rapid hibiting the essential microstructural
increase within a critical range of temper- changes necessary for its improvement.
ing temperatures. Below this range, the 6. Retarding the tempering process by
fracture toughness remains almost con- the addition of alloying elements does
stant. not lead to improved fracture toughness
2. There is a close relationship be- at a given strength level. While alloy addi-
tween mechanical properties and micro- tions enable higher strengths to be re-
structure; fracture toughness, in particu- tained at higher tempering temperatures,
lar, is very sensitive to structural changes. the balance between strength and tough-
3. Good fracture toughness develops ness is not improved.

REFERENCES
(1) P. M. Kelly and J. Nutting, "Techniques Cohen, "Microstructural Changes on Tem-
for the Direct Examination of Metals by pering Iron-Carbon Alloys," Transactions,
Transmission in the Electron Microscope," American Society for Metals, Vol. 46, 1954,
Journal of the Institute of Metals, Vol. 87, p. 851.
1958-59, p. 385. (5) E. V. Kurdjumov and L. Lyssak, "The
(2) A. S. Keh and S. Weissmann, "Deformation Application of Single Crystals to the Study
Substructure in Body-Centered Cubic of Tempered Martensite," Journal of the
Metals," Electron Microscopy and Strength
of Crystals, Interscience, 1963, p. 231. Iron and Steel Institute, Vol. 156, 1947, p. 29.
(3) P. M. Kelly and J. Nutting, "The Morphol- (6) B. G. Reisdorf, "The Tempering Charac-
ogy of Martensite," Journal of the Iron and teristics of Some 0.4 Percent Carbon Ulcra-
Steel Institute, Vol. 197, 1961, p. 199. high-Strength Steels," Transactions, AIME,
(4) B. S. Lenient, B. L. Averbach, and Morris Vol. 227, 1963, p. 1334.

Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
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DISCUSSION
1
B. R. BANERJEE —I am happy to these factors, a sufficient number of
have the opportunity to discuss this datum points may be critical in revealing
interesting paper. The authors are to be true trends in behavior.
commended for their fine structural Therefore, I have taken the liberty to
characterizing of the final vacancy- calculate opening-mode fracture-tough-
recovery-steps in these steels, and indeed ness values, KIC , from the authors'
they confirm our own findings in this glc data on their air-melt 4340 (Steel A)
respect. on which they present the most complete
However, the authors' conclusions— set of datum points. These calculated
based on their fracture-property data KM values are plotted in Fig. 16, along
on these steels—tend to contradict much with other recent literature data2 and
that has been firmly established on these some Crucible research data3—all ob-
steels over the past several decades. To tained on fatigue-cracked circumferen-
suggest that the toughness of 4340 or its tially notched round tension specimens
modifications remain unchanged upon of air-melted 4340. The dotted line,
tempering up to any temperature up drawn through these points, immediately
through 600 to 900 F, as the authors suggests two significant trends which run
allege (Figs. 1 and 2 in their paper), is contrary to the authors' conclusions:
contrary to the vast body of metal- 1. The toughness of air-melted 4340
lurgical literature accumulated over the increases throughout the entire temper-
years through much careful experi- ing range of 200 to 1000 F, rather than
mentation with these materials. "a region of about constant low frac-
The authors have used fatigue-cracked ture toughness at the lower tempering
circumferentially notched round tension temperatures, and a region of rapidly
specimens, and determined the critical increasing toughness," as suggested by
strain-energy release rate, or crack- the authors. A similar, continued tough-
extension force values, presumably using ness increase upon tempering air-melt
the Irwin approximation. But this 4340 was also found by plane-stress
approximation does not give the true tension tests performed with center-
g lc , but actually a lower bound of notched, fatigue-cracked sheet speci-
9ic. In order for this lower-bound value mens.4
to reasonably approach the true values, 2. A discontinuity in the toughness-
the notch must always be sufficiently tempering curve is suggested in the
sharp, and the plastic zone size must
remain small enough, relative to speci-
2 W. A. Backofen and M. L. Ebner, "Metal-
men geometry; furthermore, at the
lurgical Aspects of Fracture at High Strength
lower toughness regions, loading axiality Levels," Watertown Arsenal, WALTR 310.24/5-
becomes quite critical. Considering all 4, May,
3
1963.
Unpublished results, Research Division,
1 Manager, Basic
Copyright by ASTMResearch and reserved);
Int'l (all rights Applied Mon
Crucible
Dec 7 Steel Company
13:15:25 of America, Pitts-
EST 2015
Physics, Research Division,
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4
Company of America, Pittsburgh, Pa. See p. 94.
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23
24 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

500-F (400 to 700 F) embrittlement behavior in both fatigue-cracked and


region. brittle-boundary specimens, broken
The authors attribute their unique either under impact or slow-bend condi-
conclusions on fracture-toughness de- tions.
pendence upon tempering and to the The l-in.-diameter round bars, which

FIG. 16—Dependence of Plane-Fracture Toughness Upon Tempering of Air-Melt 4340.

employment of fatigue cracks in their the authors have used for their fracture
tests, thereby rejecting all prior Charpy- tests, may, upon oil quenching, introduce
impact literature data as inapplicable. sufficient autotempering (due to the
However, in Fig. 17 are plotted fatigue- slack-quench effect) in the embrittling
cracked Charpy-impact data on con-
8 "Investigation of Fracture Toughness in
sumable electrode vacuum-arc-melted,
5 High-Strength Alloys," Progress Report No. 8,
4335-V from the recent literature, which WADD Contract AF33(616)-8165, ManLabs,
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againDownloaded/printed
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by
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DISCUSSION ON MlCROSTRUCTURE AND TOUGHNESS 25

FIG. 17—Dependence of Sharp-Crack Charpy Impact Upon Tempering of Vacuum Arc-Melted


4335-V.

FIG. 18—Influence of Notch Acuity on Klc Results for 300M Steel.

range of 4340 steels that recovery from tively lower toughness values observed
these structures may not be obtained y the authors (Fig. 16).
untilCopyright
relativelybyhigh tempering tempera- In view of these, I would like to sug-
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This may partlybyexplain the rela- gest that, in employing these relatively
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26 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

FIG. 19—Comparison of K\c Results From Several Sources.

new test schemes, we should cautiously QIC , used in this paper, is clearly denned
proceed to acquire a sufficiently large by the Irwin-Orowan-Griffith fracture-
body of data through different test mechanics analysis6 and requires no
approaches before attempting to broadly elaboration here. glc designates the
interpret results which violate a sub- critical strain energy release rate for the
stantial, established body of literature plane-strain opening-mode fracture. It is
gained through general experience. related to the plane-strain stress-in-
A. J. BAKER, F. J. LAUTA, AND R. P. tensity factor, KIC , by
WEI (authors)—Banerjee's comments
consist of a series of imputations con-
cerning the validity and interpretation
of the fracture toughness data presented
in our paper. The comments appear to where E = elastic modulus and v =
be based on a combination of false Poisson's ratio. The practical require-
assumptions and a general disregard for ments for valid determinations of glc
the principles of fracture toughness or Klc were rigorously observed in our
testing. To reply to them adequately, it experiments. Fatigue precracking was
is necessary to deal with them in se- 6
quence and at some length. G. R. Irwin, "Fracture Mechanics," Struc-
tural Mechanics, Pergamon
EST Press,
2015 New York,
The fracture toughness parameter, N. Y., Dec
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1960, p. 557.
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DISCUSSION ON MlCROSTRUCTURE AND TOUGHNESS 27

employed to ensure adequate notch differences in sulfur and phosphorus


acuity. contents, since they influence fracture
Specimen sizes were chosen to insure toughness. Backofen and Ebner's results9
adequate constraint; for example, 1-in.- for this steel are replotted in Fig. 19
diameter specimens were used for glc using the tensile strengths reported by
measurements on Steel A (AISI 4340 Shih et al.10 With sulfur and phosphorus
steel) tempered at 800 F when f-in.- levels intermediate between Steels A and
diameter specimens were found to be B, the steel exhibits a plane-strain frac-
inadequate for this tempering treatment. ture toughness intermediate between
Axiality of loading was good and intro- that of Steels A and B. The agreement
duced errors of less than 10 per cent in with our finding is, in fact, good.
the 9ic values. It should be noted that A direct comparison between KIC
poor alignment will accentuate any results and Charpy impact test results,
embrittling phenomenon that may be as suggested by Banerjee, should not be
present, and consequent effects, such as attempted, since the bases of the two
a purported 500-F embrittlement, are as tests are quite different. Whereas K^c
likely to be observed under these testing characterizes the plane-strain opening-
conditions as any other. Since the need mode fracture, the Charpy impact test
for fatigue precracking of specimens has measures the energy required to fracture
been recognized only recently, a disagree- a mildly-notched specimen in a mixed-
ment with previously published results mode fracture with other attendant
is expected. A typical example is pro- energy losses. Similarly, Kc or gc results
vided by Fig. 18, comparing the ap- for sheet- or plate-type specimens are
parent KIC results reported by Carmen also strongly influenced by the modes of
et al7 with the authors' KI C data for fracture, plane-stress versus plane-strain,
300M steel, which is Steel C in this and comparisons with KIC values should
paper. Such discrepancies are bound to be made with caution. The continued
persist, moreover, if K^c results are com- increase of Kc values with increasing
puted and reported in complete viola- tempering temperature, 300 F to 700 F,
tion of one or more of the fracture indicated by Banerjee had been ob-
mechanics requirements. Banerjee's data served previously by the authors.11
for AISI 4340 steel tempered at 1000 F, However, this behavior reflects prin-
shown in Fig. 16, are an obvious example cipally a change in fracture mode, as
of such violation. indicated by a change from 20 per cent
Regarding the specific comparison shear in the fracture for a 300-F temper-
between the KI C results of Backofen ing treatment to 100 per cent shear for
and Ebner8 and those reported in this
paper for AISI 4340 steels, Fig. 1, it was
9
Kic recalculated using Irwin's relationship;
suggested in our paper that comparisons Kic = 0.414 n\/D,ffwhere <rn is the nominal
notch tensile strength and D is the specimen
be made at equal tensile-strength levels, diameter. Bueckner's relationship, used by
and that proper allowances be made for Backofen and Ebner, uses a constant of ap-
proximately 0.46.
7 C. M. Carmen, D. F. Armiento, and H. 10 C. H. Shih, B. L. Averbach, and Morris
Markus, "Plane Strain Fracture Toughness Cohen, "Some Effects of Silicon on the Mechani-
Measurements of High Strength Steels," Jour- cal Properties of High Strength Steels," Trans-
nal of Basic Engineering, ASME, March, 1963, actions, American Society for Metals, Vol. 48,
p. 87. 1956, p. 86.
8 W. A. Backofen and M. L. Ebner, "Metal- 11 R. P. Wei, "Fracture Toughness Testing
lurgical Aspects of Fracture at High Strength in Alloy Development," Fracture Toughness
Copyright
Levels," by ASTM
Watertown WALTR
Int'l (all
Arsenal, 310.241
rights reserved); Testing
Mon Dec and Its Applications,
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5-4, May, 1963.
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28 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

tempering treatments above 600 F, in in Charpy impact energy are regarded


O.lOO-in.-thick specimens. as evidence of a significant change in
A 500-F embrittlement, or martensite fracture toughness.
temper embrittlement per se, was not Concerning the question of auto-
indicated by our data, and Backofen tempering in the 4340 steels (owing
and Ebner8 reached the same conclusion to the use of large section size specimens),
in their study. The embrittlement indi- we must emphasize that essentially all
cated by the discusser, Fig. 16, results the fracture tests on the 0.40 per cent

FIG. 20—Effect of Specimen Size on Fracture Toughness Test Results.

from an indiscriminate averaging of two carbon steels (A, B, and C) were car-
distinctly different sets of data, and the ried out using f-in.-diameter specimens,
use of an alternately contracted and and not l-in.-diameter specimens as the
expanded scale for the tempering tem- discusser states. Only in the case of
peratures. Furthermore, the impact Steel A, tempered at 800 F, and Steel C,
and bend test data, Fig. 17, do not tempered at 1050 F, were l-in.-diameter
provide convincing substantiation of a specimens used, since additional con-
500-F embrittlement, unless the slow- straint was required. All the steels
bend test results are ignored and the studied possess high hardenability and
minorCopyright
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DISCUSSION ON MlCROSTRUCTTJRE AND TOUGHNESS 29

Figure 20 shows KIC data derived from an embrittling effect in this type of ma-
both f-in.- and ^-in.-diameter specimens terial.
of Steel A.12 The close agreement be- The authors are gratified that some
tween the two sets of values refutes the degree of agreement exists on the metal-
suggestion that autotempering can have lographic interpretations contained in
12 F. J. Lauta, Unpublished data, U. S. Steel
their paper and look forward to the
Corp., Applied Research Laboratory, Monroe- publication of Banerjee's confirmatory
ville, Pa. studies.

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RELATIONSHIPS BETWEEN STRUCTURE AND PROPERTIES
IN THE 9NI-4CO ALLOY SYSTEM

BY J. S. PASCOVER1 AND S. J. MATAS1

SYNOPSIS
The effects of alloy content and heat treatment on the strength and tough-
ness of 9Ni-4Co alloy steels are discussed in detail. The strength was deter-
mined with standard tension specimens, while toughness was evaluated with
various accepted, sharply notched specimen types.
Of the alloying elements used, carbon acted as the strongest embrittler but
was necessary as a strengthener. Silicon and the carbide-forming elements
decreased toughness, particularly at higher carbon contents. Hence, the use of
silicon at other than residual levels was undesirable. The addition of carbide-
forming elements in appreciable amounts needed careful consideration. Nickel
was used in substantial amounts to improve toughness, while cobalt was added
to inhibit retained austenite formation consequent upon the high nickel con-
tent. Cobalt enhanced self-tempering effects, particularly for the lower carbon
varieties.
Heat treatment strongly influenced the properties as a result of the at-
tendant changes in the microstructure. Isothermal transformation to lower
bainite enhanced toughness in the 0.45%C, 9%Ni-4%Co high performance
(HP) 9-4-45 steel. The toughness was superior to that of tempered marten-
site at equivalent strengths. The properties of upper bainite were not as at-
tractive as those of lower bainite. Mixed structures composed of bainite and
martensite lowered toughness.
The two commercial grades of the 9Ni-4Co alloy system, HP 9-4-25 and
HP 9-4-45, had a better combination of strength and toughness than other
carbon-strengthened steels. The self-tempering characteristics of the HP
9-4-25 grade and its inherent toughness contributed to high joint efficiences and
formability in the as-welded condition. No post-heat treatment of the welded
joint was required.

The need for materials of high sistance to premature failure owing to


strength-to-weight ratio is unquestion- pre-existing flaws. Resistance to corro-
able. Strength per se, however, is not a sive environments and to cyclic fatigue-
sufficient criterion for the use of a ma- type loading, as well as amenability to
terial in many applications. For highly fabrication, are additional requirements,
stressed structural components, the Many approaches have been used to
material must also exhibit a high re- obtain steels with both high strength and
adequate reliability (1-5) .2 This paper,
1 Research metallurgist and supervisor of high
strength steels, respectively, Research Center, 2 The boldface numbers in parentheses refer
Republic Steel Corp., Cleveland, Ohio. to the list of references appended to this paper.
30
PASCOVER AND MATAS ON PROPERTIES or ALLOY STEELS 31

however, will be confined to a discussion The 9Ni-4Co alloy steels are amenable
of an investigation aimed toward op- to various processing techniques. It was
timizing the properties of the carbon- found that at a given strength level a
strengthened, low-alloy, high-strength significant improvement in toughness can
steels by balancing the composition. The be obtained through the use of a special
final result of this study was the devel- melting practice, referred to as vacuum
opment of 9Ni-4Co-XC steels3 which arc remelt carbon deoxidation (VAR-
contain basically about 7 to 9 per cent CDOX) practice4 (5,8,9). With this
Ni, 2 to 5 per cent Co and 0.15 to 0.50 technique the product of deoxidation is a
per cent C (4-8). gas instead of a solid reaction product,
The 9Ni-4Co alloy system exhibits a as in conventional deoxidation practice.
wide range of properties. For example, This alloy system is also responsive to
ultimate tensile strengths as high as 300 thermal-mechanical treatments (1). In
ksi and, at lower strengths, impact particular, both the strength and tough-
energies up to 80 ft-lb were obtained. ness can be increased by hot-cold work-
TABLE 1—COMPOSITIONS OF ALLOY STEELS INVESTIGATED, WEIGHT PER CENT.
Alloy Heat Size, Ib c Mn Si Ni Cr Mo V Co

HP 9-4-45° 0.45 0.25 0.10 8.00 0.30 0.30 0.10 4. 00


HP 9-4-25" 0.28 0.35 0.10 8.00 0.50 0.50 0.10 4. 00
H-ll" 0.40 0.30 0.90 5.00 1.30 0.50
AISI 4340° 0.40 0.70 0.25 1.80 0.80 0.25
AMS6434" 0.36 0.70 0.27 1.80 0.80 0.35 0.20
MOD 4330" 0.35 0.90 1.30 1.80 0.95 0.40 0.14
3950831 >8000 0.43 0.02 0.01 8.00 0.09 0.08 0.19 3^
3920588 >8000 0.41 0.21 0.03 8.00 0.34 0.28 0.12 4.000
A336 150 0.46 0.21 0.24 7.29 0.20 0.19 0.08 2.0 7
A335 150 0.45 0.21 0.44 7.38 0.24 0.21 0.08 4.0!
A356 150 0.41 0.33 0.82 7.38 0.22 0.19 0.12 3.60
0 Typical alloy composition.

The lower carbon grade, referred to ing (l). Such treatment involves the de-
commercially as HP 9-4-25, exhibits a formation of austenite prior to the
Charpy impact energy of 50 ft-lb at the transformation of austenite to martensite
200 ksi yield strength level. The higher (1,2) or bainite.
carbon grade, HP 9-4-45, on the other Although some information is available
hand, will develop 25 ft-lb of impact in the literature on the effects of alloying
energy at a yield strength of 250 ksi. elements on the strength and toughness
Furthermore, the lower carbon varieties of the 9Ni-4Co alloy system (4,8,10), no
can be welded in the quenched and comprehensive study has been published.
tempered condition (200 ksi strength Thus, this paper is concerned with the
level) without preheat or postheat. The influence of composition as it relates to
higher carbon compositions, however, the strength and toughness of the
must be welded in the annealed condition 9Ni-4Co alloys when they are heat-
and fully post-treated to achieve joint treated to a tempered martensitic struc-
efficiencies in excess of 90 per cent at an ture. In addition, the properties of the
ultimate tensile strength of 290 ksi. HP 9-4-45 alloy steel, when heat-treated
3 The 9Ni-4Co-XC steels, designated com-
to a bainitic microstructure, are com-
4
mercially as HPby 9-4-X,
Copyright ASTM are
Int'lproprietary steels
(all rights reserved); MonADecproprietary melting
7 13:15:25 practice of Republic
EST 2015
of Republic Steel Corp. Steel Corp.
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32 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

pared to those obtained by tempering The production-sized heats were


martensite. melted as 70 or 5-ton basic, electric
arc-furnace heats and poured into
MATERIALS AND PROCEDURE electrode molds without additions of
Materials: metallic deoxidizers. During vacuum
consumable electrode remelting into
The chemical compositions of the heats 24-in.-diameter crucibles, the steel was
investigated are presented in Table 1. carbon deoxidized, yielding a very clean,

Specimens were austenitized, oil-quenched, refrigerated, and tempered at the tempering tem-
peratures indicated.
FIG. 1—Influence of Carbon on Strength of HP 9-4-X Alloy Sytem.

They represent two basic types—150-lb low gas content material (5,6,9). The
air induction heats (Si-Al deoxidized) and vacuum remelted ingot was then forged
commercial production-sized heats (vac- to a 4 by 12-in. slab product and hot-
uum arc remelted carbon deoxidized). rolled (2:1 cross roll) to the appropriate
The 150-lb heats were melted as air plate or sheet section thicknesses.
induction heats. Using pure materials,
two 70-lb ingots were poured, forged to Procedure:
2 by 2-in. billets and subsequently Oversized specimen blanks were cut
straightaway hot-rolled to appropriate from hot-rolled 7product,
Copyright by ASTM Int'l (all rights reserved); Mon Dec
heat-treated,
13:15:25 EST 2015
plateDownloaded/printed
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PASCOVER AND MATAS ON PROPERTIES OF ALLOY STEELS 33

dimensions. Standard sheet tensile speci- DISCUSSION


mens were used for evaluating sheet
product. The tensile strength of plate The Effect of Chemical Composition en
material was evaluated by standard Strength and Toughness:
round tensile specimens. To evaluate The primary hardening and em-
notch toughness, several types of speci- brittling agent in the 9Ni-4Co alloy
mens were used (11). system is carbon. The alloy content has

Values are for longitudinal and transverse specimens from vacuum arc remelted carbon de-
oxidized heats.
FIG. 2—Influence of Carbon on Charpy V-Notch Impact Energy of HP 9-4-45 Plate Tempered
at the Temperature Indicated.

The fatigue precracked impact speci- a secondary influence on strength but is


men employed in this study was similar very important in controlling toughness
in nearly all respects to the ASTM (6,14). The effect of carbon and alloy
standard Charpy V-notch specimen. The content on strength, ductility, toughness,
only difference lay in the fatigue crack and tempering response of martensite
introduced at the V-notch root by a will be discussed in detail in this section.
device especially designed for the purpose
(12,13). In this case, the value reported as Effect of Carbon:
W/A represents the unit work to failure The effect of carbon on the strength
in a manner analogous, but not neces- of tempered martensite in the 9Ni-4Co
sarilyCopyright
identical,byto the
ASTMGc value
Int'l deter-
(all alloy system
rights reserved);can Mon
be seenDec
in Fig. 1.7 The13:15:25 E
mined from notched
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by specimens. strength increase with increasing
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34 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

Specimens were heat-treated to various strength levels. The notch strength was determined with
fatigue-cracked, center-notched specimens 0.080-in.-thick.
FIG. 3—Influence of Carbon Content on Relative Notch Strength of HP 9-4-X Alloy System.

FIG. 4—Effect of Silicon on Notch-Strength and Yield-Strength Ratio at Various Tempering


Temperatures of Air-Induction-Melted HP 9-4-45 Steels (Longitudinal Direction).

amounts of carbon is typical of ferrous the superimposed dispersion strengthen-


martensites (15) and can be rationalized
Copyright by ASTM Int'l (all rights reserved);ing
Monby Decthe7 13:15:25
diffusion-controlled
EST 2015 carbide
by (1) the solid solution
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the martensitic
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Washington andof(2)
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PASCOVER AND MATAS ON PROPERTIES OF ALLOY STEELS 35

of strength on carbon at higher carbon It appeared that silicon not only re-
levels can be explained by the above, duced the over-all notch toughness but
it is conceivable that some of the effect also introduced the so-called 500-F
is due to the presence of increased embrittlement into the HP 9-4-45 steel.
amounts of retained austenite. However, It should be noted that the embrittle-
x-ray measurements of retained austenite ment appeared at temperatures higher
do not support this view. than the usual 500 F embrittling range.
The effect of carbon on the toughness of This shift to higher temperatures was
the 9Ni-4Co alloy system is shown in Fig. caused by the retardation of the temper-
2. As the carbon content was increased, the ing reaction by silicon (16,17).
Charpy V-notch impact toughness values Although silicon reduced the notch
decreased. The effect of higher tempering toughness of the steel drastically, it did
temperatures was to displace the impact not affect the ductility of the steel to a
toughness level at a given carbon con- great extent. The investigation of duc-
tent to higher values. For example, an tility included silicon contents of up to
impact toughness of 30 ft-lb was ob- 1 per cent.5 Similar results were reported
tained for the 0.24 to 0.28 carbon variety, when silicon was added to AISI 4340
HP9-4-25, after tempering at 400 F, steel (18).
whereas an impact toughness of 45 ft-lb There are indications that carbide-
was obtained after tempering at 1000 F. forming elements such as chromium
A more graphical description of the and molybdenum reduce the toughness
effect of carbon on the notch toughness of the steel and are conducive to 500-F
of the steel at various strength levels can embrittlement (5). Hence, chromium and
be seen in Fig. 3. The index of toughness molybdenum were kept to a minimum
in this case is the ratio of the nominal in the HP 9-4-45 steel when highest
notch strength to the yield strength, an toughness was desired.6 Because of the
indication of the load-carrying capacity embrittling effect of silicon and the
of the material in the presence of a flaw. carbide-forming elements, other alter-
It is apparent that the ratio decreased natives were sought to impart hardena-
with an increased carbon level irrespec- bility and, when possible, strength and
tive of the strength level. Thus, the toughness. Nickel was selected because
carbon content of the steel should be as of its tendency to increase toughness and
low as possible for optimum toughness, contribute somewhat to solid solution
but high enough to provide the desired strengthening. However, with increased
strength. nickel contents, greater amounts of
austenite were retained after quenching.
Effect of Alloying: This retained austenite was not elimi-
The selection of the alloying elements nated by a combination of refrigeration
in the 9Ni-4Co alloy system was based and a tempering treatment. In an effort
primarily on these effects on notch to counteract this effect, cobalt was
toughness. For example, the amount of added. The cost of cobalt made the use
silicon in the steel was kept to a minimum of this element in excessive amounts
because it reduced toughness drastically, prohibitive. Thus, the preferred com-
as shown in Fig. 4. After tempering at position range of nickel was dictated by
700 F, the steel with a 0.25 per cent
silicon exhibited a nominal notch- 5
Unpublished data, Republic Steel Corp.
6
strength to yield-strength ratio of 0.80, Carbide-forming elements were useful addi-
Copyright by ASTM Int'l (all rights reserved);tions
MontoDec 7 13:15:25
carbonEST 2015 giving ad-
whereas with the addition of 0.90 per vantages thein lower
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strength, weldability, temper
centUniversity
silicon, the ratio dropped
of Washington to 0.50.
(University resistance,
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36 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

the fact that increasingly higher nickel treatment. This is related to the de-
contents in the steel required corre- pendency of properties on the micro-
spondingly higher amounts of cobalt in structure of the steel. Thus, in this
the steel. In the as-quenched condition, section the properties of martensite,
a 0.45C-9N1 alloy retained 22 per cent bainite, and the properties of structures
austenite, a 0.45C-9Ni-2Co alloy re- containing both tempered martensite
tained 13 per cent austenite, whereas and bainite will be described and ra-
the 0.45C-9Ni-4Co, HP 9-4-45, com- tionalized.
position retained less than 6 per cent
austenite. In this latter case, the aus- Martensitic Structure:
tenite could be completely transformed
by refrigeration. As is the case with other hardenable
An attendant effect resulting from the carbon-bearing steels, the 9Ni-4Co alloy
addition of cobalt is an increase in the system responds to the hardening treat-
austenite to the martensite transforma- ment consisting of the austenite to
martensite reaction. The response of the
TABLE 2—EFFECT OF COOLING RATE martensite to normal tempering, which
ON THE PROPERTIES OF HP 9-4-25 is typical of other carbon-bearing steels,
STx!j-ii'Ij.a
can be seen in Figs. 1, 2 and 4. As the
Yield Ultimate Charpy tempering temperature was increased,
Quenching k Tensile V-Notch
Strength,6 Strength,
Medium ksi ksi
Impact at
78 F, ft-lb
the strength decreased (Fig. 1), and the
impact toughness (Fig. 2) and notch
Water 165 300 25 strength increased (Fig. 4).
Oil 166 300 25 Unlike other carbon-containing steels,
Air 175 290 30
it is difficult or sometimes impossible to
a All specimens were obtained from J^-in.-
detect the 500-F embrittlement in the
thick plate and were heat treated individually. HP 9-4-X alloy. Specifically, the notch
* The strength properties were determined on
0.252-in.-gage diameter, round tension speci- strength yield strength ratio of HP 9-4-45
mens. steel increased continuously with in-
creasing tempering temperature, as can
tion temperature,M s. The addition of be seen in Fig. 4.
4 per cent Co to a 0.25C-9Ni steel As previously mentioned, another
raised the Mstemperature from about feature of the 9Ni-4Co alloy system is
475 to 550 F. Thus, the tendency for the high Mstemperatures of the low-
self-tempering of the martensite on carbon varieties. This promotes a certain
cooling was significantly increased. The amount of self-tempering of martensite.
importance of self-tempering in HP The amount of self-tempering increases
9-4-25 for practical application will be with an increase of the Mstemperature
discussed in later sections. and a decrease in the cooling rate. Some
effects of self-tempering on cooling can
Effect of Heat Treatment: be seen in the data for air-cooled speci-
In the previous section it was shown mens shown in Table 2. Both water-
that composition changes can produce a and oil-quenched specimens had prac-
wide range of strength and toughness tically the same toughness and yield
characteristics in the tempered marten- strength, whereas the air-cooled specimen
sitic structure of the 9Ni-4Co alloy had a higher yield strength and a higher
system. The properties can be further impact toughness. The higher yield
Copyright by ASTM Int'l (all rights reserved); Mon Dec
enhanced by judicious choice of heat strength of the7 air-cooled
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PASCOVER AND MATAS ON PROPERTIES OF ALLOY STEELS 37

interpreted as an aging effect similar to ture, 425 F, and rapidly in the transfor-
that discussed by Cohen (15). mation range from 550 to 700 F, the
opposite behavior is observed for the
Bainitic Versus Tempered Martensitic
toughness-transformation temperature
Structure:
relationship. This point will be discussed
The properties of isothermally trans- further in a later section.
formed bainite have been reported to be Comparison of Figs. 5 and 6 indicates
a strong function of the transformation that high toughness at strength levels of
temperature (19,20). This can also be engineering significance was obtained.

FIG. 5—Effect of Transformation Temperature on Strength and Impact Toughness of HP 9-4-45


Steel in a y-in.-Thick Plate (Longitudinal Direction).

seen in Fig. 5 for the HP 9-4-45 alloy Further comparison can be made from
steel. The yield-strength properties Fig. 7, where the Charpy V-notch impact
varied from 230 to 180 ksi with a change energy of several heats is plotted against
in the reaction temperature from 450 to yield strength for both tempered mar-
600 F. Similarly, the ultimate tensile tensite and freshly transformed bainite.
strengths varied from 275 to 195 ksi. Figure 8 is a similar plot in which the
The toughness properties varied in an unit fracture energy, W/A = work/area,
equally marked fashion as shown in as measured by the precracked Charpy
Figs. 5 and 6. It should be noted that, impact test, is the toughness criterion.7
although the strength changes slowly In both cases it is apparent that bainitic
withCopyright near the Mstempera- structures exhibit superior toughness at
by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
temperature
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38 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

a given strength level in the 9Ni-4Co martensite-bainite structure is formed.


alloy system. It appears, therefore, that Note that while the unnotched yield
steels with lower bainitic structures may strength is relatively constant in the
be technologically interesting materials. transformation region, 400 to 500 F, the
There are, however, several factors which notch properties show a discontinuous
must be observed in attempts to evaluate reduction in the immediate vicinity of
or use high-strength bainites. the Ms.An even more striking example
of this can be found in the data for a
Effect of Mixed Structures: ICr-lMo steel (21). Furthermore, Smith,
The increase of strength with decreas- Speich, and Cohen (22) have shown that
ing transformation temperature, ob- the bainitic transformation itself will

Specimens were austenitized and transformed to bainite at above transformation temperatures.


FIG. 6—Effect of Transformation Temperature on Unit Energy Absorption at Room Temperature
on HP 9-4-45 Steel.

served in Fig. 5, makes transformation catalyze martensite formation at tem-


near the Mstemperature attractive. Care peratures near, but above,0.1M, .8 Con-
must be taken, however, that a 100 per ceivably, such an effect explains the
cent bainitic structure is obtained. rapid toughness change between 450 and
Figure 9 illustrates the results of a heat- 500-F bainites in Fig. 6 (M, is 425 F).
treating sequence in which a duplex Accordingly, data obtained on material
7
transformed immediately aboves M must
The bainitic structures are too tough to be be carefully interpreted.
validly tested by fatigue-cracked center-notched
specimens at section thicknesses up to at least
0.250 in. Valid K\c measurements are also diffi- 8
The catalysis is presumably an example of
cult. Copyright
Presumably, these Int'l
by ASTM high(all
strain-rate (im- Mon
rights reserved); strain
Dec induced martensite
7 13:15:25 EST 2015formation. In this
pact) Downloaded/printed
tests provide, at bythis time, the best case the requisite strain is provided by the in-
approximation of the material toughness. ception of the bainitic slow growth.
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PASCOVER AND MATAS ON PROPERTIES or ALLOY STEELS 39

FIG. 7—Relation Between Strength and Impact Toughness of ^-in.-Thick Plate of HP 9-4-45
Steel Heat-Treated to Bainitic and Tempered Martensitic Structures.

Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
FIG. 8—Relation Between Strength and Unit Energy Absorption Characteristics of |-in.-Thick
Plate Downloaded/printed
of HP 9-4-45 Steel by
Heat-Treated to Bainitic and Tempered Martensitic Structures.
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40 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

The notch strength was determined with fatigue-cracked, center-notched specimens 0.180 in.-
thick.
FIG. 9—Effect of Transformation Temperature on Notch Properties of a 9Ni-4Co-38C Alloy Steel.

FIG. 10—Effect
Copyright of Testing
by ASTM Temperature
Int'l (all on Impact
rights reserved); Mon DecToughness
7 13:15:25of HP2015
EST 9-4-45 Steel Heat-Treated
to a Bainitic and Tempered
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ksi.
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PASCOVER AND MATAS ON PROPERTIES or ALLOY STEELS 41

It seems reasonable, therefore, that orientation may also cause variations in


poor toughness properties will also result strength-toughness relationships is not
from incomplete isothermal transforma- surprising. Pickering (26) has shown that
tion followed by quenching to form lower bainitic structures have lower
martensite. Such an effect has been noted transition temperatures than upper
elsewhere.9 bainitic structures of lower strength
levels.
Comparison of Upper and Lower Bainite: The question of transition temperature
Considerable study of the kinetic is somewhat obscure in the 9Ni-4Co
features of the bainite transformation alloy system because of the nature of the

FIG. 11—Variation of Plane-Strain Fracture Toughness With Yield Strength for Several High-
Strength Steels.

(23,24,25) has indicated that there is at impact energy test temperature curve,
least a distinct metallographic difference as shown in Fig. 10. However, the dis-
between upper and lower bainite. Lower tinction between upper and lower bainite
bainite is characterized by precipitation is perhaps responsible for the small (10
of carbides at about a 60 deg angle to ft-lb) change in impact energy which
the bainitic-ferrite plate, major axis, occurs between the 600 and 700-F
while upper bainite may be recognized bainites (Fig. 5), a temperature range in
by carbide precipitation parallel to the which the strength changes from 180 to
plate axis. That this difference in carbide 138 ksi. Matas and Hehemann (23) have
Copyrightcommunication,
9 Private by ASTM Int'lW.(all reserved); Mon Dec that
rights Thio-
Hughes, suggested the transition
7 13:15:25 from upper
EST 2015
kol Chemical Co., 1961. by
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42 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

ture range 650 to 700 F, regardless of ksi strength level, whereas AMS 6434
composition. and AISI 4330 (modified) had CKIvalues
Thus, these data indicate that trans- of 80 ksi \/in. These compositional
formation of the HP 9-4-45 steel to effects confirm the previous analysis (4)
lower bainite results in a material with of sheet materials under plane-stress
high toughness and strength. Care must testing conditions. A comparison with
be taken, however, to avoid mixed maraging steels and nonferrous materials
structures and upper bainite. has been published elsewhere (10).
One wonders if, perhaps, a substantial The role of alloy composition is not
portion of the controversy and reticence only reflected in the strength and tough-
over the use of bainitic structures may ness but also in other properties such as
not be due to either mixed structures or fabricability, fatigue strength, and stress
upper bainite. Specifically, many low- corrosion characteristics. As a result of
alloy, high-strength steels and nearly all the alloy balance, the lower carbon
low-carbon (<0.35 per cent C) steels varieties of the HP 9-4-X alloy system
have as M temperature of 600 F or exhibited a capability for being welded
above. Such a situation makes it im- in the heat-treated condition without
possible to achieve a fully lower bainitic preheat or postheat. Joint efficiencies in
structure. Since most of the construc- excess of 90 per cent in 1-in.-thick plates
tional alloy steels are in this group, it of HP 9-4-25 were obtained at the 200
follows that most of the data do not ksi strength level (6,7,8,10). The benefits
represent the best properties of bainite. of alloy composition were further demon-
strated by the fact that specimens of
9Ni-4Co Alloy Steels and Other Carbon- HP 9-4-25 steel, which were cut from
Bearing High Strength Steels: as-welded 1-in.-thick plates, could be
bent 180 deg around a mandrel of 2T
The preceding sections have shown the radius without cracking, suggesting the
effects of various factors on the strength presence of adequate ductility for forma-
and toughness of the 9Ni-4Co alloys. bility in the as-welded condition. The
The success of the 9Ni-4Co research self-tempering characteristics of the
program may be measured by compari- alloy presumably contributed to the
son with similar high-strength steels. toughness and formability of the as-
A critical comparison of alloy effects welded steel. At these strength levels,
may be made by evaluating fracture other steels required a postheat treat-
toughness under severe plane-strain con- ment to develop these high-weld joint
ditions. Such a comparison can be seen efficiencies and formability (3,7,8,10).
in Fig. 11, where it is apparent that the Resistance to fatigue-type cyclic load-
toughness of HP 9-4-45 is significantly ing and to stress corrosion was not
greater than that of other carbon- altered by the alloy composition and
strengthened steels. At a 220 ksi yield followed the known relationships. That
strength, for example, the Klc values is, the fatigue endurance limit was about
of AISI 4340 and H-ll were about 40 one half of the ultimate tensile strength
ksi \/in-, whereas that of HP 9-4-45 as with other carbon-bearing alloy steels
was 70 ksi -\/iri- The importance of alloy (10). The stress corrosion characteristics
balance is also apparent at a lower were commensurate with the superior
carbon content. The plane-strain frac- toughness of this alloy system (6,10).10
ture Copyright
toughness of the HP 9-4-25 steel
by ASTM Int'l (all rights reserved); 10Mon
Private
Dec communication, R. 2015
7 13:15:25 EST L. Davis,
was about 110 ksi Vm".
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PASCOVER AND MATAS ON PROPERTIES or ALLOY STEELS 43

CONCLUSIONS 0.25 per cent carbon variety. Presum-


ably, this effect was responsible for the
The strength and toughness of 9Ni-
low weld-cracking susceptibility of the
4Co alloy steels were observed to change HP 9-4-25 steel.
markedly with variations in composition 4. The toughness of isothermally
and heat treatment. As a result of these transformed, lower bainitic structures in
observations, the following conclusions the HP 9-4-45 steel was, in general,
can be stated: higher at a given strength level than
1. Carbon is the basic strengthening those exhibited by tempered martensitic
element in this alloy system. However, structures.
the embrittling effects which accompany To obtain the highest toughness, care
this strengthening require that the car- must be taken that the structure is fully
bon content be maintained at a minimum bainitic. Upper bainitic structures had a
consistent with the desired strength. lower strength-toughness combination
2. Silicon not only reduces the tough- than the lower bainitic structures.
ness of 9Ni-4Co alloy steels but also 5. The HP 9-4-X steels showed a
induces 500-F embrittlement. The silicon greater toughness than several other
content must therefore be at a minimum carbon-bearing alloy steels at a given
to obtain maximum toughness. Carbide- strength level under all testing conditions
forming elements such as chromium investigated. This was achieved as a
and molybdenum tend to lower tough- result of proper balancing of composition.
ness, particularly at high carbon con- Furthermore, the high plane-strain frac-
tents. Careful consideration should be ture toughness and weldability of HP
given to their addition to the 9Ni-4Co 9-4-25 should make it very attractive for
alloys in substantial amounts. highly stressed, heavy-section applica-
3. Nickel has long been regarded as tions.
contributing to toughness of alloy steels
and is present in substantial amounts in A cknowledgment:
the HP 9-4-X alloy system. The in- The authors wish to express their
creased amounts of retained austenite, appreciation to S. W. Poole and, in
which are commonly occasioned by the particular, to Dr. J. K. Jackson of the
presence of nickel, were avoided through Republic Steel Research Center for
addition of cobalt. The higher Ms tem- many useful suggestions and for their
perature owing to the cobalt additions assistance in the preparation of this
resulted in a self-tempering effect in the manuscript.

REFERENCES
(1) S. J. Matas, M. Hill, and H. P. Munger, Transactions, American Society for Metals'
"Ausforming and Hot-Cold Working Vol. 55, 1962, p. 58.
Methods and Properties," Mechanical (4) S. J. Matas, M. Hill, and H. P. Hunger,
Working of Steel I, Metallurgical Society "Current and Future Trends for Steels
Conferences, Gordon and Beach, New with High Strength and Toughness,"
York, N. Y., Vol. 21, 1964, p. 143. Metals Engineering Quarterly, Vol. 3, No. 3,
(2) C. F. Zackay, W. M. Justusson, and D. J. August, 1963.
Schmatz, "Deformation of Metastable (5) T. E. Perry, S. W. Poole, and S. J. Matas,
Austenite—An Interim Report on a New "Development and Melting of an Ultra-
Process," Metal Progress, Vol. 80, Septem- high Strength 9%Ni-4%Co Steel," Electric
ber, 1961, pp. 68-72. Furnace Proceedings, AIME, Vol. 20, 1962,
(3) Copyright
R. F. Decker, J. T. Eash,
by ASTM Int'l and
(all A. J. Gold-
rights p. 308.
reserved); Mon Dec 7 13:15:25 EST 2015
man, "18% Nickel
Downloaded/printed byMaraging Steel," (6) "Manufacturing Process Development for
University of Washington (University of Washington) pursuant to License Agreement. No further repr
44 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

High Strength Steels," ASD Project No. Kinetics of Tempering," Transactions,


8-157, Contract AF33(657)-1127, Interim American Society for Metals, Vol. 46,
Progress Report, Republic Steel Corp., 1959, p. 812.
September-November, 1963. (17) C. J. Altstetter, M. Cohen, and B. L. Aver-
(7) Aerospace Materials Handbook; Vol. 1, bach, "Effect of Silicon on the Tempering
Ferrous Alloys, V. Weiss and J. G. Ses«ler, of AISI 43XX Steels," Transactions,
editors, Syracuse University Press, 1963, American Society for Metals, Vol. 55, 1962,
Revised 1964. p. 287.
(8) S. J. Matas, "Influence of Impurities and (18) C. H. Shih, B. L. Averbach, and M. Cohen,
Related Effects on Strength and Toughness "Some Effects of Silicon on the Mechanical
of High Strength Steels," American Properties of High Strength Steels,"
Society for Metals, Metals Engineering Transactions, American Society for Metals,
Quarterly, Vol. 4, No. 2, May, 1964, p. 48. Vol. 48, 1956, p. 86.
(9) T. E. Perry, "High Vacuum Degassing (19) K., J. Irvine and F. B. Pickering, "Low
with Induction Stirring Makes Cleaner Carbon Bainitic Steels," Journal, The
Steels," Metal Progress, Vol. 84, August, Iron and Steel Institute, Vol. 187, De-
1962, p. 88. cember, 1957 p. 292.
(10) S. J. Matas, J. S. Pascover, and W. F. (20) F. B. Pickering, "The Mechanism of
Barclay, "Tough High-Strength Steels for Bainite Formation in Low Alloy Steels
Aerospace Applications," Sixth National Containing up to 0.4% Carbon," Proceed-
Symposium on Materials for Space Vehicle ings, Internationaler Kongress fuer Elek-
Use, Society of Aerospace Material and tronenmikroskopie 4, Berlin, 1958, pp.
Process Engineers, Vol. 2, Seattle, Wash., 628-637.
November, 1963. (21) "Properties of Ultrahigh Strength Bainitic
(ID "Fracture Testing of High-Strength Sheet Structures," Armour Research Foundation,
Materials," ASTM Bulletin No. 243 ASD-TDR-63-458, May, 1963.
January, 1960, No. 244, February, 1960; (22) M. F. Smith, G. R. Speich, and M. Cohen,
also Materials Research & Standards, Vol. 1, "Anomalous Kinetics of the Bainitic
May, 1961. Transformation Just Above the Martensite
(12) G. M. Orner and C. E. Hartbower, "Sheet Range," Transactions, AIME, Vol. 215,
Fracture Toughness Evaluated by 1959, p. 528.
Charpy Impact and Slow Bend," Welding (23) S. J. Matas and R. F. Hehemann, "The
Journal, Research Supplement, September, Structure of Bainite in Hypoeutectoid
1961. Steels," Transactions, AIME, Vol. 221,
(13) S. V. Radcliffe, M. Schatz, G. M. Orner, 1961, p. 179.
and G. Bruggeman, "The Flow Tempering (24) R. H. Goodenow, S. J. Matas, and R. F.
of High Strength Steels," Final Report, Hehemann, "Growth Kinetics and the
Contract DA-19-020-ORD 5252, WAL TR Mechanism of the Bainite Transformation,"
320 4/3-1, ManLabs Inc., 1962. Transactions, AIME, Vol. 227, 1963, p. 545.
(14) "Manufacturing Process Development for
(25) G. R. Speich and M. Cohen, "The Growth
High Strength Steels," ASD Project No.
8-157, Contract AF33(657)-1127, Interim Rate of Bainite," Transactions, AIME,
Progress Report, Republic Steel Corp., Vol. 218, 1960, p. 1050.
July-September, 1963. (26) F. B. Pickering, "Fracture Characteristics
(15) M. Cohen, "The Strengthening of Steel," of Bainitic Steels," Proceedings, European
Transactions, AIME, Vol. 224,1962, p. 638. Regional Conference on Electron Micros-
(16) W. S. Owen, "The Effect of Silicon on the copy, Delft, 1960, p. 477.

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DISCUSSION
1
P. V. RiFFiN —Results of room tile-brittle transition with testing tem-
temperature Charpy impact tests have perature (Fig. 10).
been presented. Do the authors have Table 3 shows the superiority of
data on transition temperature or other bainitic structures over tempered mar-
criteria of toughness? Most previous tensitic structures in HP 9-4-45 steel.
studies indicate martensite has higher The comparison is made on the basis of
toughness than bainite at the same the same yield strength and also on the
strength level. basis of the same ultimate tensile
B. R. BANERJEE2—For the sake of strength. In each case the bainitic struc-
uniformity in terminology, I would like tures had higher toughness values,
to suggest that the term quasi-cleavage irrespective of the testing method, than
be used to describe the semi-brittle the tempered martensitic structures. For
cleavage fractures encountered in these example, at the 260/275 ksi ultimate
materials by the authors. The ASTM tensile strength level, plane strain frac-
Subcommittee is also recommending ture toughness numbers, KI C , were of
preferred use of this term. the order of 80/110 ksi Vui- for the
In our own studies of AISI 4340 steels, bainitic structures, whereas A'jc were
we find that tempered martensites have only 50/60 in the case of tempered
better toughness and lower transition martensitic structures. Similarly, at the
temperatures than bainites at the same 210/220 yield strength level, the bainitic
yield-strength level. It is important to structures had KI C values in excess of 90
make these toughness comparisons at the ksi -\Xin-) whereas the tempered mar-
same strength level, rather than in the tensitic structures were of the order of
same temper condition. 55/65 ksi \/in.
J. S. PASCOVER AND S. J. MATAS With regard to the comments of
(authors)—The authors appreciate the Riffin and specifically to the comments of
comments by Riffin and Banerjee. The Dr. Banerjee that the bainitic structures
reply to both discussions can be found have a poorer toughness than martensitic
in the written version of our paper. structures at a given strength level, the
Restated briefly, there is no question in authors cannot offer any definite ex-
our minds that the low temperature planation. However, it is proper at this
bainitic structures give a better combina- point to bring to the attention of the
tion of strength and toughness than discussers the fact that such discrepan-
tempered martensitic structures even at cies were also observed by other investi-
various testing temperatures, as vividly gators and were attributed in part by
shown in Fig. 10. Mr. Riffin's question Hehemann, Luhan, and Troiano3 to
concerning the transition temperature is mixed structures and incomplete trans-
difficult to answer, since this alloy formation of austenite to bainite. The
system does not exhibit a definite duc- effect of mixed structures on the fracture
toughness can be clearly seen in Fig. 9 of
our paper.
1 Metallurgist, TJ. S. Army Materials Re-
search
2
Agency, Watertown Arsenal, Mass. 3 R. F. Hehemann, V. J. Luhan, and A. R.
Manager,
Copyright byApplied Physics
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Dec 7"The Influence
13:15:25 EST of Bainite on Mechani-
2015
Research, Crucible Steel Company of America, cal Properties," Transactions, American So-
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45
TABLE 3—TYPICAL TOUGHNESS AT VARIOUS TESTING TEMPERATURES OF HP 9-4-45, ^-IN.-THICK STEEL PLATE HEAT
TREATED TO A BAINITIC AND A TEMPERED MARTENSITIC STRUCTURE OF THE SAME STRENGTH LEVEL (LONGITUDINAL
DIRECTION).
Charpy V-Notch Impact0, ft-lb yyifr KIc
Structure Heat Treatment YS.ksi u±c., «.»i
RT -100 F -320 F in-lb/in.2, RT ksi
JV in.
J\.-L

Bainite 1 hr 1600 F —> AC —» ^ hr 1450 F 220/230 260/275 35/40 35/40 15/25 700/800 80/110
-> 7 hr 450 F

Tempered martensitic 1 hr 1600 F —> AC —> Yi hr 1450 F 235/245 260/275 20/25 20/25 10/15 450/550 50/60
-> oil -» 2 hr - 120 F -> 2 hr
500 F —> 2 hr - 120 F —> 2 hr
500 F

Bainite 1 hr 1600 F -> AC -* ^ hr 1450 F 210/220 240/255 35/50 35/50 15/25 1200/1500 +90
-> 7 hr 500 F

Tempered martensitic 1 hr 1600 F -» AC —> ^ hr 1450 F 210/220 235/245 22/27 20/25 10/15 600/700 55/65
-»• oil -» 2 hr - 120 F -» 2 hr
650 F -> 2 hr -120 F -» 2 hr
650 F
0
Fatigue pre-cracked Charpy V -notch impact specimens, 0.394 by 0.394 by 2.16 in.
6
Slow-bend, Single-edge notched specimens, J^ by ^ by 4^ in. and % by M by 8 in.

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HIGH-STRENGTH STAINLESS STEELS BY DEFORMATION AT
ROOM TEMPERATURE
BY S. FLOREEN1 AND C. R. MAYNE2

SYNOPSIS
Low-silicon stainless steel sheets were rolled 40 per cent at room temperature
and heat-treated 24 hr at 800 F. Yield strengths of 240 ksi were obtained in
iron-nickel-chromium alloys. Through the use of 7 to 12 per cent cobalt as a
supplemental hardener, the yield strengths were increased to 270 ksi. Notch
tensile ratios of unity were obtained using NASA-ASTM sheet specimens.

The austenitic stainless steels are well earlier work which indicated that, if the
known for their ability to be strengthened silicon was maintained under 0.15 per
by cold working. While it is recognized cent, the notched properties of subzero-
that the actual composition of an austen- rolled materials were greatly improved
itic stainless steel governs its response (I).3 Deoxidation of the present heats was
to cold working, there has been little accomplished by adding 0.1 weight per
systematic study of the factors which cent aluminum before pouring.
will yield high strengths by cold working The ingots were hot-worked to j-in.-
and also maintain good fracture tough- thick plate and then cold-worked to a
ness. The present study was designed to 0.100-in. sheet. They were annealed 1 hr
study some of these factors. at 1950 F, air cooled, cleaned, and then
rolled 40 per cent at room temperature.
MATERIALS AND PROCEDURES The reduction used was 40 per cent,
A series of 30-lb induction-melted because the data of Espey and co-work-
heats was prepared using electrolytic ers (2) indicated the anisotropy would no
metal charges. Table 1 gives the composi- be severe with this amount of reduction.
tions of the chromium-nickel heats. Rolling was generally done in three or
In order to obtain higher strengths, four passes on a laboratory mill using 8-
cobalt and/or molybdenum additions in.-diameter rolls. The alloys were cooled
were studied in a second series of alloys. to room temperature after each pass.
The compositions of these heats are given After rolling, the 0.060-in.-thick sheets
in Table 2. were heat-treated 24 hr at 800 F, and
It should be noted that the silicon then machined to NASA-ASTM smooth
content of all the heats is much lower and edge-notched tension specimens 1-
than that encountered in normal produc- in. wide. The notched specimens had a
tion. Low silicon contents were incor- minimum stress concentration factor,
porated in these materials because of Kt, of 18. The specimens were taken in
the longitudinal direction only.
1 Research associate, Research Laboratory,
Several of the alloys were given other
International
2
Nickel Co., Sterling Forest, N.Y.
3
Product development metallurgist, Inter- The boldface numbers in parentheses refer
national Nickel Co., New York, N.Y. to the list of references appended to this paper.
47
48 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

TABLE 1—CHEMICAL COMPOSITION OF Cr-Ni STAINLESS STEELS,


WEIGHT PER CENTS, BALANCE Fe.
Heat Cr Ni Mn Si C N

VACUUM INDUCTION MELTS

1 19.8 10.1 0.45 0.10 0.04 0.01


2 18.2 10.3 0.72 0.11 0.04 0.01
3 17.0 5.3 0.48 0.07 0.05 0.01
4 18.9 7.7 0.78 0.11 0.05 0.02
5 18.8 8.6 0.75 0.10 0.06 0.01
6 18.4 8.2 0.01 0.10 0.05 0.01

AIR INDUCTION MELTS

7 18.7 7.4 0.05 0.13 0.07 0.02


8 18.8 6.1 0.21 0.02 0.07 0.03
9 15.7 7.4 0.30 0.04 0.07 0.03
10 16.3 7.2 0.25 0.03 0.06 0.04
11 17.1 7.2 0.20 0.02 0.07 0.04
12 17.8 5.4 0.31 0.08 0.08 0.04
13 17.7 6.0 0.25 0.05 0.08 0.04
14 17.6 7.2 0.21 0.02 0.08 0.03
15 17.7 5.5 0.21 0.08 0.08 0.03
16 17.8 5.6 0.18 0.07 0.10 0.03
17 17.8 5.5 0.15 0.02 0.14 0.03
18 14.4 7.2 0.50 0.03 0.06 0.02
19 16.0 5.5 0.46 0.01 0.05 0.02

TABLE 2—CHEMICAL COMPOSITION OF Co-Mo CONTAINING STAINLESS


STEELS, WEIGHT PER CENTS, BALANCE Fe.
Heat Cr Ni Mn Si C N Co Mo

AIR INDUCTION MELTS

20 18.7 6.0 0.24 0.03 0.06 0.03 1.7


21 18.7 6.0 0.21 0.01 0.06 0.03 3.5
22 18.7 7.1 0.26 0.02 0.06 0.04 2.2
23 18.8 7.2 0.25 0.01 0.05 0.03 3.9
24 16.8 6.5 0.45 0.01 0.06 0.03 3.1
25 16.1 6.7 0.40 0.01 0.06 0.03 7.5
26 15.7 5.1 0.14 0.02 0.06 0.03 8.4
27 14.6 5.1 0.24 0.05 0.05 0.03 7.7 2.0
28 12.7 5.2 0.07 0.05 0.07 0.03 7.8 3.8
29 15.2 9.2 0.22 0.05 0.05 0.02 3.1
30 13.7 5.2 0.19 0.05 0.06 0.03 7.8
31 13.6 4.2 0.20 0.05 0.05 0.02 10.7
32 14.3 6.1 0.23 0.05 0.04 0.03 11.1
33 13.9 6.9 0.20 0.05 0.04 0.02 1.8

heat treatments or refrigerated and heat- Yield strengths up to 252 ksi were ob-
treated. These procedures will be de- tained in the chromium-nickel alloys.
scribed below. Yield strengths up to 270 ksi alloys were
obtained in the alloys containing cobalt,
RESULTS AND DISCUSSION or cobalt plus molybdenum. The ratio
The tensile properties of the specimens of the notch tensile strength to the
rolled 40 perby ASTM
Copyright cent and heat-treated
Int'l (all rights reserved);24 smooth
Mon Dec tensile
7 13:15:25 ESTstrength
2015 was about unity
hr atDownloaded/printed
800 F are given by in Tables 3 and 4. in all cases.
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FLOREEN AND MAYNE ON HIGH-STRENGTH STAINLESS STEELS 49

TABLE 3—ROOM TEMPERATURE TENSILE PROPERTIES OF Cr-Ni


STAINLESS STEELS.0
0.2% Offset Ultimate Elongation Net Fracture Notched NTS
Heat Yield Tensile in 2 in., % Stress, ksi6 Tensile
UTS'*
Strength, ksi Strength, ksi Strength, ksic

1 136 148 10
2 101 116 34
3 195 196 9
4 191 207 4 234 217 1.04
5 159 183 6 219 189 1.03
6 191 208 5 257 223 1.07
7 198 209 6 250 216 1.03
8 252 253 4 267 250 0.99
9 215 216 4 247 219 1.01
10 239 239 5 247 228 0.96
11 218 222 5 251 236 1.06
12 238 240 3 244 227 0.95
13 222 223 3 244 230 1.03
14 206 214 5 237 223 1.04
15 215 216 5 240 200 0.93
16 221 223 5 246 228 1 02
17 231 233 7 269 238 1.02
18 197 197 4 249 217 1.10
19 192 193 2 254 215 1.11
0 Specimens rolled 40 per cent at room temperature and heat-treated 24 hr at 800 F after rolling.
b NASA-ASTM l-in.-edge notch specimen, Kt = 18; based on post crack area.
c NASA-ASTM l-in.-edge notch specimen, Kt = 18; based on machined notch area.
d Notched tensile strength/ultimate tensile strength.
TABLE 4—ROOM TEMPERATURE TENSILE PROPERTIES OF Co-Mo
CONTAINING STEELS."
0.2% Offset Ultimate Elongation Net Fracture Notch Tensilec NTS
Heat Yield Tensile in 2 in., % Stress, ksi6 Strength, ksi
Strength, ksi Strength, ks UTS'*

20 232 233 4 259 244 1.04


21 231 236 3 260 241 1.02
22 206 224 4 245 232 1.03
23 216 228 4 255 235 1.03
24 224 225 2 277 239 1.06
25 243 244 2 279 244 1.00
26 268 269 2 293 270 1.00
27 270 270 2 276 267 0.99
28 251 251 2 285 277 1.10
29 196 221 2 253 225 1.02
30 219 219 2 268 239 1.09
31 223 223 2 259 221 0.99
32 255 255 2 282 250 0.98
33 208 209 2 264 230 1.10
" Specimens rolled 40 per cent at room temperature and heat-treated 24 hr at 800 F after rolling.
6 NASA-ASTM l-in.-edge notch specimen, Kt = 18; based on post crack area.
cNASA-ASTM l-in.-edge notch specimen; based on machined notch area.
d Notched tensile strength/ultimate tensile strength.

Equipment for accurately measuring much higher than the yield strengths,
the true stress at fracture was not readily An examination of the fractured surfaces
available. However, estimates were made of the tension specimens indicated that
of the net fracture stress by the ink- all had failed in a ductile manner; there
staining method
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7 13:15:25 EST 2015
erally, the net fracture
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50 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

Specimens rolled 40 per cent at room temperature and heat-treated 24 hr at 800 F.


FIG. 1—Yield Strength Versus Stability for Cr-Ni Stainless Steels.

Specimens
Copyrightrolled 40 perInt'l
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roomreserved);
temperature
Monand
Decheat-treated
7 13:15:2524 hr at
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2015
FIG. Downloaded/printed
2—Yield Strength byVersus Stability for Stainless Steel Containing Cobalt and Molybdenum.
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FLOREEN AND MAYNE ON HIGH-STRENGTH STAINLESS STEELS 51

have excellent resistance to brittle frac- peak yield strength of approximately 270
ture at the strength levels investigated. ksi appears at a stability number between
As was stated previously, all of the 20 and 21.
materials contained a maximum of 0.15 The results in Fig. 2 also indicate that
per cent silicon because it had been
shown by previous work (1) that, lower- TABLE 5—TENSILE PROPERTIES OF
ing the silicon content from the normal STAINLESS STEELS ROLLED 40 PER
CENT AND HEAT TREATED 24 HR AT
0.5 to 0.7 per cent, found in most austen- VARIOUS TEMPERATURES.
itic stainless steels, to 0.15 per cent Heat
maximum, permitted strengths of sub- Treating Yield Ultimate Elong. in
Heat Tempera- Strength, Strength, 2 in.,
zero-rolled stainless steel to be increased ture, F ksi ksi %
while still maintaining high notch tensile
properties. Although this previous work 196 198 4
30
1 800 219 219 2
was done with stainless steels rolled ] 900 196 196 4
at subzero temperatures, the tensile (1000 152 156 5
strengths were similar to those in the 200 202 4
present paper, and it is felt that the 31 1 800 223 223 2
lowering of the silicon content to 0.15 ) 900 200 201 4
[1000 153 160 10
per cent maximum is a major contribut-
ing factor to the excellent fracture tough- 204 209 4
ness of these sheet materials. 32
1 800 255 255 2
) 900 216 221 3
The earlier study of subzero-rolled (1000 166 176 6
alloys (l) showed that empirically the
yield strengths could be correlated with
TABLE 6—TENSILE PROPERTIES OF
composition by means of a stability STAINLESS STEELS ANNEALED, RE-
number. This number is based on the FRIGERATED 16 HR AT -106F, AND
effects of the individual alloying ele- HEAT-TREATED TEMPERATURES.
24 HR AT VARIOUS

ments on the Ms temperature, as meas-


ured by Eichelman and Hull (3). Figure 1 Heat Yield Ultimate Elong. in
Treating
Heat ' Tempera- Strength, Strength, 2 in.,
shows the results for the chromium- ture, F ksi ksi %
nickel stainless steels from Table 3
plotted in this fashion. The results are 131 184 6
1 8 158 189 8
reasonably consistent, and show a similar 30. | 900 172 181 6
curve to those found for zero-rolled stain- (1000 131 146 8
less steel (1). A peak strength of close to
128 189 6
240 ksi was achieved at a stability factor 01 1 800 162 199 7
ol
between 21 and 22. | 900 174 184 6
The results of Eichelman and Hull (1000 143 156 7
did not include an allowance for cobalt 108 187 7
and molybdenum. The stability formula 6* oo 1 800 171 203 7
was modified to include these two ele- ) 900 159 190 8
(1000 108 150 11
ments by using the results of Coutsoura-
dis (4) for the effect of cobalt and those
of Irvine and co-workers (5) for the effect from 1 to 4 per cent cobalt had no effect
of molybdenum on the Ma temperature. on the yield strength, but that cobalt
Figure 2 shows the yield strengths of the contents of 7 to 12 per cent raised the
cobalt and molybdenum-bearing alloys strength approximately 30 ksi. There
as aCopyright
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52 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

using molybdenum by itself or in con- strengthening by cold deformation. We


junction with cobalt. This last result estimate the strengthening by cold roll-
shows that there was no marked cobalt- ing to be 80 ksi.
molybdenum hardening such as found Heat treating raised the strength to
in maraging steels (6). approximately 240 to 270 ksi, depend-
Several alloys were tested as cold- ing upon the cobalt content. This latter
rolled at room temperature, and with strength increase does not depend notice-
heat treatments of 24 hr at 900 or 1000 F. ably upon whether the martensite was
Only the smooth tensile properties were formed by refrigeration or by cold work-
measured. The results are given in Table ing, and thus the hardening due to heat
5. Cold rolling alone without heat treat- treating does not appear to be associated
ment gave yield strengths of approxi- with the cold-working operation itself.
mately 200 ksi. Heat treating at 900 or The reason for the added hardening
1000 F gave lower strengths than those due to cobalt is not clear. Cobalt has
obtained by heating at 800 F. been found to produce a rather weak
Other specimens annealed 1 hr at 1950 age hardening in low-carbon iron-nickel
F were refrigerated at —106 F for 16 hr, martensites (7), and also to modify the
which resulted in partial transformation tempering characteristics of carbon
to martensite. Afterwards, they were martensites (8). The latter effect is
heat-treated. The tensile properties of perhaps the more plausible explanation
these materials are given in Table 6. for the present hardening, but further
They had yield strengths on the order of work is necessary to clarify the hardening
120 ksi after refrigeration. Heat treating mechanism.
raised the strengths by amounts that are
comparable to the strength increases CONCLUSIONS
obtained by heat treating the cold-rolled 1. Low-silicon chromium-nickel stain-
materials, which we believe indicates less steels had yield strengths on the order
about the same amount of transforma- of 240 ksi and excellent toughness after
tion in the refrigerated and cold-rolled rolling 40 per cent at room temperature
specimens. and heat treating at 800 F.
Rolling 40 per cent at room tempera- 2. Through the use of cobalt as a
ture resulted in yield strengths of about supplemental hardener, it was possible
200 ksi, some of which is due to trans- to achieve strengths of 270 ksi while
formation to martensite and some due to still maintaining excellent toughness.

REFERENCES
(1) S. Floreen and J. R. Mihalisin, "High- ing, and thus the hardening due to heat
Strength Stainless Steel by Deformation at Spontaneous Transformation of Austenite
Low Temperatures," Advances in the Tech- to Martensite in 18-8 Type Stainless Steel,"
nology of Stainless Steels, ASTM STP 369, Transactions, American Society for Metals,
Am. Soc. Testing Mats., to be published. Vol. 45, 1953, p. 77.
(2) G. B. Espey, M. H. Jones, and W. F. Brown,
Jr., "The Sharp Edge Notch Tensile (4) D. Coutsouradis, "Action du Cobalt dans
Strength of Several High-Strength Steel les Aciers a Durcissement Structural," Me-
Sheet Alloys," Proceedings, Am. Soc. Test- moirs Scientific Revue de Metallurgie, Vol. 58,
ing Mats., Vol. 59, 1959, p. 837. 1961, p. 503.
(3) H.Copyright
C. Eichelman and F. Int'l
by ASTM C. Hull, "The Ef-
(all rights (5) K.
reserved); J. Irvine,
Mon Dec 7D.13:15:25
T. Llewellyn,
EST 2015and F. B.
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FLOREEN AND MAYNE ON HIGH-STRENGTH STAINLESS STEELS 53

Pickering, "Controlled - Transformation Alloys Based on Iron—18% Nickel," Trans-


Stainless Steels," Journal of the Iron and actions, Quarterly American Society for
Steel Institute, Vol. 192, 1959, p. 218. Metals, Vol. 57, 1964, p. 38.
(6) R. F. Decker, J. T. Eash, and A. J. Goldman, (8) V. K. Chandhok, J. P. Hirth, and E. J.
"18% Ni Maraging Steel," Transactions, Dulis, "Effect of Cobalt on Tempering Tool
Quarterly American Society for Metals, Vol. and Alloy Steels," Transactions, Quarterly
55, 1962, p. 58. American Society for Metals, Vol. 56, 1963,
(7) S. Floreen, "Hardening Behavior of Ternary p. 677.

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AN EVALUATION OF THE 18NI-9CO-5MO MARAGING
STEEL SHEET
BY D. L. CORN1

SYNOPSIS
An investigation was conducted on 0.070-in.-thick 18Ni-9Co-5Mo, 300 ksi,
maraging steel sheet to determine its applicability for use in high-strength
pressure vessels. This study includes the effects of aging as-received material,
re-annealing material, the combined effects of annealing and aging, and the
influence of cold working and aging upon the properties and micro-structure of
this maraging material.
Austenite retained at room temperature was found as a result of aging at
950 F for 8 hr, or annealing in the temperature range of 1200 to 1250 F. Mate-
rial containing significant amounts of austenite at room temperature was found
to age unsatisfactorily; however, if material containing austenite is plastically
strained, the aging response markedly improves. Material containing no
austenite was also strengthened by virtue of the cold work, but a loss in
strength was obtained after stretching beyond 2 per cent tensile plastic strain.
Duplex aging cycles were investigated, and it was found that the heat treat-
ment time required to reach a specified strength can be reduced by using a
duplex aging cycle instead of a single aging cycle.
In addition, the microstructures produced by various heat treatments are
presented and interpreted in terms of the austenite-to-martensite transforma-
tion, martensite-to-austenite reversion, and precipitation reactions.

The maraging alloy steels have been detrimental and to take advantage of
undergoing rapid development, pri- those which are superior.
marily because of their very high In order to more completely under-
strength and excellent toughness. Much stand the maraging steels metallurgical
is already known about their mechanical and mechanical behavior, four areas that
properties and metallurgical charac- were felt to require understanding, even
teristics (1-4) ,2 but because of their rapid for limited use of this alloy, were denned
development, a complete metallurgical and investigated.
technology of the maraging steels does 1. The metallurgical characteristics
not yet exist. To apply this alloy prop- and mechanical properties of material
erly, all of its various properties must be containing appreciable amounts of aus-
known to allow for those which are tenite (termed reverted austenite) at
1 Research metallurgist, Research Projects room temperature, owing to annealing
Section, Douglas Aircraft Co., Inc., Santa in the temperature range 1200 to
Monica,
2
Calif. 1250 F, were studied.
The boldface numbers in parentheses refer
to the list of references appended to this paper. 2. The effects of single and double
54
CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 55

aging on microstructure and mechanical work must be considered in addition to


properties were determined. the usual effects of plastic deformation.
3. The effect of tensile plastic strain 4. The influence of annealing heat
on annealed and aged mechanical prop- treatment on mechanical properties and
erties and metallurgical characteristics microstructure was evaluated.
was investigated. The influence of plastic The results of investigations in these
strain on reverted austenite-to-mar- four areas are presented in this paper.
tensite transformation activated by cold MATERIAL INVESTIGATED
TABLE 1—CHEMICAL ANALYSES OF The material investigated was con-
THE MARAGING STEEL INVESTIGATED, sumable - electrode, vacuum - remelted
0.078-IN. SHEET." 18Ni-9Co-5Mo maraging steel in the
Precision Douglas Mill form of ten 54 by 120 by 0.078-in. sheets.
Element Limits, Analysis, Analysis, Each sheet was designated by a different
% weight % weight %
letter that was always included as one
Nickel ±0.20 18.62 18.68 of the specimen identification marks.
Cobalt ±0.20 8.87 8.97 The material was obtained from the
Molybdenum ±0.10 4.77 5.07
Titanium ±0.05 0.59 0.72 Allegheny Ludlum Steel Corp. in the
Manganese ±0.002 0.017 0.011 annealed condition, 1500 F for 1 hr, and
Carbon ±0.002 0.013 0.019
Phosphorous ±0.001 0.003 0.004
was stretcher-leveled approximately 1
Sulphur ±0.001 0.007 0.010 per cent at the producer's mill subse-
Nitrogen ±0.002 0.007 0.003 quent to the anneal.
a Supplied by Allegheny Ludlum Steel Corp.
Chemical analysis of the material is
6 Average of 13 to 19 determinations. given in Table 1.

Upper and lower configurations were used for testing annealed material and aged material, re-
spectively. Dotted circles in grip areas of lower configuration show where metallographic analysis
was performed.
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
FIG. 1—Tension
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56 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

SPECIMEN PREPARATION ensure that the amount of stress these


AND TESTING areas had been subjected to during test-
Approximately 0.004 in. was initially ing had not affected the microstructure,
ground from each side of all specimens several aging heat treatments were
prior to heat treatment. Temperatures repeated and the resultant microstruc-
during heat treatment were monitored tures were compared to those obtained
with at least five chromel-alumel thermo- using the broken tension specimens. No
couples located on the specimens. All differences were found. Metallographic
specimens were prepared for heat treat- analysis of the annealed specimens was
ment either by degreasing in hot tri- performed on separate specimens in-
chloroethylene vapor or by a triple cluded for that purpose, so that the

FIG. 2—As-Received Microstructure Showing Fine Martensite (X 500).

rinsing procedure, which consisted of effect of stress was not a problem. All
rinsing first in isopropyl alcohol, second metallographic specimens were me-
in distilled water, and finally in isopropyl chanically polished down to at least a
alcohol again. 6-n diamond wheel and electropolished
All tension specimens, represented by on a Disa-electropol, Model 53-C. The
the configurations in Fig. 1, were tested settings used are as follows:
in accordance with ASTM Method
E 8.3 After testing, the broken specimens Solution: 67 ml of perchoric acid (70 per
cent), 131 ml of distilled water,
of the aged material were used for metal- 700 ml of ethanol, and 100 ml
lographic analysis using the areas in the of butylcellosolve.
grip portion, as shown in Fig. 1. To Aperture: 6 ml in diameter,
Flow rate: 3.5 (arbitrary units),
Copyright of
3 Methods by ASTM
TensionInt'lTesting
(all rightsofreserved);
MetallicMon Current
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setting0.6 to 0.9 amp,
Materials, 1964 Book ofbyASTM Standards, Part Voltage setting:25 to 30 v, and
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pursuant to License sec. No further reproductions autho
CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 57
All specimens were etched immediately ing heat treatments can be divided into
after electropolishing in Carapella's etch, two major classes:
which is composed of the following: 5 1. those that are characterized by an
g of FeCl3, 2 ml of hydrochloric acid incomplete martensite-to-austenite
(HC1, concentrated), and 99 ml of transformation at the annealing tempera-
ethanol. ture, which causes a chemically in-
The x-ray diffraction experiments were homogeneous structure; as a result,
performed with a Norelco x-ray diffrac- significant amounts of austenite are

Direct carbon replica chrome-shadowed at 45 deg. Second phase indicated by arrow.


FIG. 3—As-Received Microstructure Showing Grains of Approximately 2-ju Diameter and Traces
of a Second Phase (X 14,500).

tion unit equipped with a diffractometer subsequently retained upon cooling to


using chromium radiation. The magnetic- room temperature.
force measurements were made with a 2. Those which are characterized by
Magne-Gage, Model 6, using magnet the transformation of all the martensite
number one. to austenite at the annealing tempera-
RESULTS AND DISCUSSION ture, and then the complete transforma-
tion of this7austenite back2015
to martensite
Properties of Annealed Material:
Copyright by ASTM Int'l (all rights reserved); Mon Dec 13:15:25 EST
upon cooling to room temperature.
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Microstructure—The types
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58 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

shown that annealing at 1500 F or above, value obtained for the average grain
and air-cooling, resulted in a structure diameter in Fig. 3 is about 2 p. Therefore,
which was essentially wholly martensitic this maraging steel appears to be very
(1,2). Since the as-received material had fine-grained.
been mill annealed at 1500 F for 1 hr, The Ms and M/ temperatures for this
it was expected that it would be wholly alloy are 300 to 310 F and 200 to 210 F,
martensitic. This was confirmed by x-ray respectively (1^4). The dependence of

Arrows point to second phase, which is probably ferrite. Direct carbon replica chrome-shadowed
at 45 deg.
FIG. 4—Microstructure of Specimen Annealed at 1500 F for 1 hr and Air Cooled (X 24,900).

diffraction, which revealed no retained the Ms temperature on grain size and


austenite. The as-received microstructure the influence of the alloying elements on
is shown in Figs. 2 and 3. Figure 2 shows the Ms temperature are presented in
the fineness of the martensite, and Fig. 3 Ref. (4).
shows what appears to be grains. Accord- Some specimens were annealed at
ing to the standard ASTM rating for 1500 F for 1 hr and air cooled at Douglas
grain size in steels, it is much finer than in addition to the mill anneal. The result-
ASTM 8, which
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grainreserved);
diam- MoningDec
microstructure is shown in Fig. 4.
7 13:15:25 EST 2015
of about 25 p, orby less, whereas the This figure shows the same grain size as
eter Downloaded/printed
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CORN ON 18Ni-9Co-5Mo MARAGING STEEI. SHEET 59

Fie, 5—Microstructure of Specimens Annealed at 1800 F for 6 to and Air Cooled.

in Fig. 3, but an extra phase is visible martensite transformation could not be


at the grain boundaries. Upon closer induced in any Fe-Ni alloy containing
examination, this phase also seems to less than 15 per cent Ni with negligible
appear in minute quantities in Fig. 3. carbon content, even with quenching
It is suggested that this second phase is rates up to 5500 C/sec. Instead, a trans-
massive ferrite similar to that observed formation occurred which resulted in
by Marshall et al (5), massive ferrite formation. The authors
The observation of primary massive also mentioned, however, that a quench-
ferrite in low-carbon, iron-nickel alloys ing rate as low as 5 C/min would produce
is not unusual and has been noted by a martensitic transformation in iron-
several other investigators. Gilbert and nickel alloys containing 19 to 31 per cent-
Owen (6) found
Copyright thatInt'lthe(allaustenite-to-
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nickelDecand7 negligible
13:15:25 ESTcarbon.
2015 Jones and
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60 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

Pumphery (7) discussed both the austeri-' nickel alloys containing 4.9 and 14.6 per
ite-to-ferrite and the austenite-to-mar- cent nickel. Both contained negligible
tensite transformations for two iron- carbon. Decker (4) discussed the influence
of heating rate on the martensite-to-
ferrite plus austenite transformation in
a maraging steel.
Annealing at higher temperatures than
1500 F produces grain coarsening as was
expected. The microstructure of a speci-
men annealed at 1800 F for 6 hr and air
cooled is shown in Fig. 5. This figure
shows the Widmanstatten morphology
and grain size which has increased to
about ASTM 4. Unlike the specimen
annealed at 1500 F, a second phase was
not observed at 1800 F. This suggests
that the ferrite might have been formed
because of incomplete homogenization
at the lower annealing temperature.
FiG. 6—Microstructure of "Specimen "An-
nealed at 1200 F for 2 hr and Air Cooled (X X-ray diffraction measurements re-
500). vealed no austenite in either the 1500

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FIG. 7—Microstructure of Specimen Annealed at 1200 F for 2 hr and Air Cooled (X 14,500).
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CORN ON 18Nt-9Co-5Mo MARAGING STEEL SHEET 61

Direct carbon replica chrome-shadowed at 45 deg.


FIG. 8—Microstructure of Specimen Annealed at 1200 F for 18 hr and Air Cooled (X 14,500).

DirectCopyright
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FIG. 9—Microstructure
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Specimen Annealed at 1200 F for 2 hr and Air Cooled (X 14,500).
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62 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

or 1800-F specimens. This does not rule iron-nickel alloy containing 9 per cent
out the possibility that the second phase nickel nominally. Therefore, the austen-
observed in the specimen annealed at ite is retained upon cooling to room
1500 F is austenite, however, because temperature because its higher nickel
small amounts of austenite (less than content has lowered its Ma temperature
3 per cent) are very difficult to detect below room temperature.
with x-ray diffraction techniques. However, this preferred dissolution of
Annealing in the 1200 to 1250-F range nickel into the austenite is not instan-
produces a markedly different micro- taneous but diffusion controlled. It is
structure from that obtained by anneal- suggested that this effect might give
ing at 1500 F or above. This is shown in rise to the formation of ferrite envelopes
Figs. 6 to 9. Figure 6 shows the fineness surrounding the austenite upon cooling
of the structure, which appears to be a to room temperature in the following
white continuous matrix with many tiny way. The martensite areas immediately
black islands dispersed in it. This is surrounding the austenite would be the
verified by the electron photomicro- first to be depleted of nickel. This would
graphs, Figs. 7 to 9, in which the islands lower the nickel content of these affected
are clearly visible. It is suggested that areas below 15 per cent. According to
these islands are austenite and the con- Gilbert and Owen, as noted above, the
tinuous matrix is martensite. By com- formation of massive ferrite cannot be
paring the micro-structures obtained suppressed in iron-nickel alloys contain-
with different times at 1200 F, Figs. 7 ing less than 15 per cent nickel, even by
and 8, it is seen that the microstructure extremely fast quenching rates. Consider-
changes little with respect to time, if at ing the tendency of carbon to segregate
all. Figure 9 shows that the same micro- in austenite also, it is conceivable that
structure is also obtained by annealing at the aforementioned areas surrounding
1250F for 2 hr. This type of reaction the austenite could contain less than
has also been observed by Allen and 15 per cent nickel and 0.01 per cent
Early in iron-nickel alloys (8). The discus- carbon. Therefore, upon cooling to room
sion that follows is the same type that temperature, the areas immediately
was used by them. surrounding the austenite could trans-
Equilibrium considerations can be form to massive ferrite.
*
used to explain the foregoing observa- Also, the alloying elements, molyb-
tions. At 1200 F, austenite and mar- denum and titanium, because of their
tensite (or ferrite) are costable. Once limited solubility in austenite, would not
this equilibrium amount of austenite is be expected to diffuse into the austenite
approached almost no more growth of but away from it. This would tend to
the austenite occurs. This is the reason enrich the martensitic matrix in molyb-
that the amount of austenite remains denum and titanium, and especially the
constant. areas immediately surrounding the aus-
The iron-nickel phase diagram (9) tenite. The potent ferritizing tendencies
shows that nickel is preferentially dis- of molybdenum and titanium would
solving in the austenite. This austenite then also make this area more likely to
"sink" effect has also been suggested by transform to ferrite. Segregation of the
Marshall et al (5) and Crussard et al (10). molybdenum into martensite or ferrite
In addition, Crussard et al found up to has also been suggested by Decker (5).
44 per cent nickel in austenite nuclei Literature on the iron-nickel-carbon
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usingDownloaded/printed
an extraction technique
by with an systems furnishes some interesting con-
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 63

FIG. 10—Annealed Strength as a Function of Time.

siderations which might be helpful in dence of ferrite formation. Only mar-


understanding maraging steels. Edmund- tensite was found when the alloy was
sonCopyright
(11) studied a 1Int'l
by ASTM per(allcent
rightscarbon-10 quenched
reserved); Mon from EST
Dec 7 13:15:25 a fully
2015 austenitic condi-
perDownloaded/printed
cent nickel steel by and found no evi- tion. Marshall et al (5) found that, with
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64 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

a 0.10 per cent carbon-8, 7 per cent nickel peratures. At 1300 and 1500 F, this is
steel proeutectoid ferrite formation could followed by a gradual return to the as-
be induced if tempered at 1100 F for 5 received ultimate strength. At 1200 and
days. However, upon quenching from a 1250 F, a decline in ultimate strength
fully austenitic state, a complete austen- occurs after the peak also, but whether
ite-to-martensite transformation was ob- it will eventually return to the as-
tained. Gilbert and Owen, however, could received strength has not been demon-
not prevent ferrite formation in iron- strated.
nickel alloys containing 15 per cent or 3. The elongation initially increases
less of nickel and negligible carbon. It rapidly at all four temperatures. It then
then appears that for iron-nickel-carbon gradually returns to the as-received
alloys containing less than 15 per cent elongation at 1250, 1300, and 1500 F.
nickel, the carbon content dictates The 1200 F curve appears to level off at
whether the austenite will transform to about 11 per cent elongation.
martensite or ferrite. All three of these properties indicate
one trend very strongly. This is that the
Mechanical Properties: properties tend to approach their original
The mechanical properties of the as- values until there is a return to the 100
received material are represented by the per cent martensitic behavior. This is
points on the ordinate axis in Fig. 10 exhibited to a lesser degree at 1200 F,
(top left}. The 0.2 per cent offset yield but at the other temperatures the trend
strength is approximately 40 ksi less is very definite.
than the ultimate strength, which is Younkin (12) has reported hardness
about 170 ksi. The elongation is usually data on annealed material similar to
8 per cent. The mechanical properties those presented above. He shows the
of material containing reverted austenite, room temperature hardness of 18Ni-
however, are considerably different. This 9Co-5Mo maraging steel dropping as the
is shown in Fig. 10, which presents annealing temperature is increased (all
strength as a function of time for four specimens were held at temperature for
different annealing temperatures. 100 hr). Room temperature hardness
Several characteristics that are com- starts at Rc 51 at 900 F and drops to
mon to these curves can be seen: R. 32 at 1300 F and Rc 31 at 1400 F.
1. Initially, at 1200 and 1250 F, an This curve, if determined at increasingly
abrupt increase in yield strength occurs. longer times, would probably develop a
This is followed by a large drop in yield discontinuity at the AS temperature.
strength, which also occurs at 1300 and These results are in reasonable agreement
1500 F. The drop at 1500 F is tfery small, with the results obtained here. An exact
but is considered significant because it comparison cannot be made because of
was observed at all the lower tempera- the inherent differences in the types of
tures. However, if this drop is to be data obtained.
considered significant, then the subse- The initial rise in strength is probably
quent increase must be considered signifi- due to the compound Ni3 (Ti, Al) being
cant also. At all the temperatures stud- precipitated in the martensitic matrix,
ied, except 1200 F, the yield strength which causes some combination of disper-
appears to eventually behave as the yield sion and precipitation hardening. The
strength of wholly martensitic material. slight rise in yield strength in Fig. 10,
2. Copyright
An abrupt increase in ultimate (bottom right) mentioned previously,
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strength
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initially occurs following the initial drop could also be
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 65

due to the precipitation of Ni3 (Ti, Al), rate of diffusion of the alloying elements
except this time in the newly formed in the matrix.
austenite which would again cause some Figures 11 and 12 show stress-strain
slight precipitation hardening. Support curves of specimens having received the
for these suggestions is found in the annealing heat treatments of 1500 F for
iron-base austenitic alloy, A-268, which 1 hr and 1250F for 2 hr, respectively.
is hardened by the precipitation of Nig Figure 11 is typical of the type of stress-
(Ti, Al) in this same temperature range strain curve that is obtained with a fully
(13). annealed steel. Figure 12, however, is not
At present, it is difficult to say what typical. Portion B of the curve appears
mechanism is causing the large drops in to be a region in which about 1 per cent
plastic strain occurs with almost no in-
crease in stress. Portion C consists of

Tested in the annealed condition.


Tested in the annealed condition. FIG. 12—Stress-Strain Curve of Specimen
FIG. 11—Stress-Strain Curve of Specimen Annealed at 1250 F for 2 hr.
Annealed at 1500 F for 1 hr.
the work-hardening phenomenon and
yield strength after the initial increase ultimate fracture.
at 1200 and 1250 F, and the somewhat A similar type curve is found in Ref.
smaller drops observed at 1300 and 14. Here the stress-strain curve of a
1500 F. It is proposed, however, that single crystal of copper containing 0.4
these drops are all caused by the same per cent arsenic is shown. It contains
mechanism and are always accompanied essentially the same features as Fig. 12.
by the retention of some austenite upon The author states that the B portion ofa
cooling to room temperature. This means the curve is associated with recrystalliza-
that some retained austenite is possible tion. He further suggests that the B
even when an annealing temperature of portion of the curve is due to a decrease
1500 F is used, if the time at temperature in dislocation density, which causes a
is short enough. The effect becomes large release "of energy. This suggests
increasingly less pronounced as the tem- that a Cottrell cloud mechanism is acting
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perature is raised because of the higher to stabilize the dislocations, and the dis-
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66 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

locations stabilized in this manner are reverted austenite transforming almost


breaking away from the solute atoms and completely to martensite. The C portion
becoming mobile at about the same would then represent behavior of essen-
energy level. Thus, an avalanche of dis- tially martensitic material. This would
locations results which produces con- mean that the C portion of the curve
siderable plastic strain. should be similar to that of the plastic
Similarly, the B portion of the marag- region of a wholly martensitic specimen
ing steel curve in Fig. 12 might represent (Fig. 11), and it is, in that both display
the work hardening phenomenon. The
rate of work hardening, however, is con-
siderably different. In addition, a massive
transformation of austenite to martensite
would remove all the austenite-mar-
tensite interfaces, which probably had
been pinning a large number of disloca-
tions. The removal of these interfaces
would then free these dislocations, and
allow them to become mobile again.
This in turn would result in large strains
and cause the behavior shown in portion
B of Fig. 12.
An important variable which was not
FIG. 13—Microstructure of Specimen Aged considered in the foregoing discussion is
at 875 F for 8 hr and Air Cooled (X 500). the isothermal transformation of the

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FIG. 14—Microstructure
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 67

Direct carbon replica chrome-shadowed at 45 Arrow points to area containing reverted aus-
deg. tenite.
FIG. 15—Microstructure of Specimen Aged at FIG. 16—Microstructure of Specimen Aged at
750 F for 312 hr (13 days) and Air Cooled (X 950 F for 8 hr and Air Cooled (X 500).
14,500).

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FIG. 17—Microstructure
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68 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

reverted "austenite to martensite after precipitates than that seen in Fig. 14.
heat treatment when the specimen is In general, the aged martensitic structure
stored at room temperature. According appears coarser than the annealed mar-
to Machlin and Cohen (15), isothermal tensitic structure.
transformation occurs in high-nickel, Figures 16 and 17 show the overaged
iron^nickel alloys with a carbon content structure. Figure 16 shows the fine
of less than 0.04 per cent. If isothermal martensite with an area that appears to
transformation at room temperature is be the initial stages of austenite rever-
occurring, then the microstructure and sion. The austenite has probably depleted
aging response should both change with nickel from the surrounding areas. This
respect to time. However, no experi- would explain why the area etches more
ments were performed to specifically darkly. Figure 17 is an electron photo-
show this change. micrograph which shows about the same

FIG. 18—Strength as a Function of Time at 950 F.

PROPERTIES or AGED MATERIAL


Microsiruciure:
Microstructures of aged material are
presented in Figs. 13 to 17. Figure 13
shows the fine martensitic structure
obtained upon aging at 875 F for 8 hr.
Because of the fineness of the structure,
some difficulties were encountered in
focusing.
Figure 14 is an electron photomicro-
graph of a specimen aged at 875 F for
8 hr and appears to show grains. Figure
15 presents the microstructure of a speci-
men aged at 750 F for 312 hr. It appears a Duplex FIG. 19—Microstructure of Specimen Given
Aging Heat Treatment of 900 F for 9
to contain
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 69

FIG. 20—Effect of Secondary Aging Heat Treatments on Tensile Yield Strength.

FIG. 21—Effect of Secondary Aging Heat Treatments on Ultimate Tensile Strength.

structure as specimens aged at a lower coarser. This could result from the
temperature. Again, the grain boundaries preferential attack of the electropolish
are visible, but the structure appears a or etchant (or both) on the precipitate
little rougher than those of the specimens particles. Barclay and Jackson (16) have
aged at lower temperatures. It appears shown an excellent electron photomicro-
that as the aging temperature is, in- graph of these precipitates using trans-
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EST 2015
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70 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

Mechanical Properties: tively. They show that a primary aging


Figure 18 shows ultimate and yield heat treatment of 900 F for 9 hr, followed
strength as a function of aging time at by air cooling, plus a secondary aging
950 F for specimens from B sheet. It heat treatment of 700 to 800 F for 8 hr
shows that overaging occurs relatively and air cooled, produced the highest
fast at 950 F. It has been suggested that strengths. It is suggested that this type
this loss in strength is not an overaging of behavior is a result of different types
phenomenon (loss of coherency of pre- of precipitates appearing at different
cipitates and subsequent growth), but temperatures.
instead is caused by reversion of the

FIG. 22—Effect of Marforming on Aged Ten-


sile Strength.
FIG. 23—Strength as a Function of Tensile
Cold Work Performed Between an Austenite-
martensitic matrix to austenite (3). This Stabilizing Anneal and an Aging Treatment.
is consistent with the observation of
reverted austenite in a specimen that Effect of Cold Working:
has been aged at 950 F for 8 hr, as shown
in Fig. 20. Figure 22 presents ultimate and yield
strengths as a function of tensile plastic
Duplex Aging Heat Treatments: strain prior to aging. The tensile plastic
Figure 19 presents the microstructure strain was performed on specimens of
of a doubly aged specimen. It shows a as-received, wholly martensitic material.
microstructure that is essentially the Then after marforming,4 they were aged
same as the microstructure of specimens at 885 F for 8 hr. The data indicate that
aged only once. strengthening results from tensile mar-
Figures 20 and 21 present the effect of forming, but that there is a critical
duplex-aging heat treatments on yield amount of tensile cold work above which
strength and ultimate strength respec- no more strengthening is obtained.
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4 Term recently given for cold working of
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annealed martensite in maraging steels.
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 71

FIG. 24—Magne-Gage Reading as a Function of Tensile Cold Work Performed After an Austenite-
Stabilizing Anneal, 1250 F for 2 hr.

nealed martensite also increases the decrease in strength after 50 per cent
strength for a given aging treatment. reduction in area has been exceeded. The
Decker et al (1) show that strength in- indication is, therefore, that after a
creases almost directly proportional to certain amount of cold work, whether
the amount of reduction in area. Siede tensile or compressive, no further
(17) and Gilewicz (18) also present data strengthening is to be expected. Rather, a
that Copyright
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72 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

FIG. 25—X Ray Intensity Ratio of y {220}/a {211} as a Function of Tensile Cold Work Per-
formed After an Austenite-Stabilizing Anneal, 1250 F for 2 hr.

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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 73

are operating here. First, strengthening 100 per cent martensitic structure is
from the cold work occurs because of also being approached. According to
the increased dislocation density. In Fig. 23 then, at least 8 per cent tensile
this steel, however, at the aging tem- stretch would be required to transform
perature employed austenite is a stable all of the stabilized austenite to mar-
phase (9). Therefore, there is always tensite.
some tendency for the martensite to Second, it was previously suggested
revert to austenite. Cold working pos- that the B portion of the stress-strain
sibly increases this tendency for the curve shown in Fig. 12 represented al-
martensite to revert to austenite. Since most complete transformation of the
it has been previously suggested that reverted austenite to martensite. The B
loss in strength is due to reversion to portion only covers about 1 per cent
austenite (3), excessive cold working plastic strain. Therefore, if almost
could cause a loss in strength because complete transformation during the B
the strengthening effect of cold work portion does occur, some other mech-
is more than offset by the reversion to anism is operating in the newly trans-
austenite. formed martensite to strengthen it. It

TABLE 2— EFFECT OF PLASTIC STRAIN ON MATERIAL CONTAINING


STABILIZED AUSTENITE.0

Specimen No. Amount of Plastic Magne-Gage Reading -y[220}/a{211), %


Strain, % 7{200}/a{200), %

AT 48 0 0 80.0 to 87.1 4.3 to 7.2


AT 76 1 65 to 73 44.2 4.0
AT 21 2 90 to 98 44.5 1.8
AT 100 4 114 to 119 36.2 2.5
AT 52 8 123 to 131 26.0 2.6
a All specimens were annealed at 1250 F for 2 hr and air cooled prior to plastic straining.

Figure 23 shows that stabilized aus- is suggested that this strengthening


tenite will transform to a product as a might be caused by chemical homogeni-
result of tensile cold working capable of zation of the alloying elements due to
being aged. This figure shows ultimate strain-activated diffusion at room tem-
and yield strength as a function of the perature. The newly formed martensite
amount of tensile stretch given to is probably very high in nickel (11)
specimens containing stabilized aus- and carbon but low in molybdenum
tenite, which were subsequently aged at and cobalt, as was previously discussed.
885 F for 8 hr. Strength is observed to It has been shown by Decker (4) that
increase as the amount of tensile stretch both molybdenum and cobalt are neces-
is increased until at 8 per cent stretch, sary for an adequate aging response.
the strength is approaching that of aged Therefore, the strengthening shown in
100 per cent martensitic material. Fig. 23 after 1 per cent stretch possibly
At least two hypotheses may be used could be due to a strain-activated chemi-
to explain this behavior. First, it can cal homogenization of the martensitic
be assumed that strength is directly matrix.
proportional to the amount of martensite To test the above hypotheses, an
available to age. This would mean that additional experiment was performed in
as full strength
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74 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

FIG. 26—Longitudinal Tensile Strength as a Function of Time at 1500 F Prior to Aging at 885 F
for 8 hr.

Magne-Gage and x-ray diffraction meas-


urements were then performed on the
specimens, and the results are presented
in Figs. 24 and 25 respectively. Figure
24 shows that the Magne-Gage reading
increases rapidly with respect to strain,
and then appears eventually to approach
the readings obtained for 100 per cent
martensite. Figure 25 shows that the
intensity ratio of the 7{220}/a{211}
and planes obtained using x-ray diffrac-
tion decreases as the amount of tensile
stretch increases.
Both fgures support the suggestion
that austenite is indeed transforming
to martensite as a result of tensile
stretch. Neither set of data, however, is
adequate quantitatively to describe the
phenomena occurring.
The x-ray diffraction data cannot be
Direct carbon replica chrome-shadowed at 45 used quantitatively because of the large
deg.
FIG. 27—Microstructure of Specimen An- amount of preferred orientation of the
nealed at 1250 F for 2 hr and Air Cooled Fol- austenite. This is demonstrated by
lowed by Aging at 875 F for 8 hr and Air Cool-
ing (X 8200).
Table 2, in which the 7 {200} /a{200}
ratio is also presented. The 7J220}/
austenite (as a result of annealing at a {211} ratio was used because it ap-
1250Copyright
F for 2 hr) were tensile-stretched
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to several amounts of
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 75

ture. More work on this preferred martensite condition is being approached


orientation is currently in progress. at 8 per cent tensile stretch. Further-
Because of the large amount of pre- more, it supports the first hypothesis,
ferred orientation encountered using the because it indicates that the amount of
x-ray diffraction technique, another austenite which is transformed to

FIG. 28—Microstructures of Specimens Given Annealing Heat Treatments and Aged for 8 hr
and Air Cooled (X 500).

method was sought with which to meas- martensite is a function of the amount
ure the amount of austenite. The Magne- of tensile stretch. It also indicates,
Gage was used because it is less sensitive however, that the major portion of this
to a preferred orientation than the x-ray transformation occurs in the initial
diffraction technique. The Magne-Gage stages of plastic strain, which supports
data appears to be more informative the second hypothesis. However, to
than the x-ray diffraction data because make the aforementioned inferences
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it does indicate that the 100 per cent
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76 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

ble assumption that the Magne-Gage tanium are necessary for an aging re-
reading is directly proportional to the sponse to occur at 850 to 900 F.
austenite content must be made. There- Figure 28 shows light photomicro-
fore, the above data are only indicative graphs of aged specimens. They are
of trends. presented to demonstrate that the prior
annealing heat-treatment temperature
Effect of Annealing on Aged Properties: can be estimated by examination of
; The effect of time at 1500 F on aged the aged microstructure. This figure
strength is shown in Fig. 26. These shows the increase in the size of the
specimens are all longitudinal and were martensitic platelets as the annealing
taken from sheet C. The strengthening temperature and time are increased. No
obtained by annealing for f hr appears significant increase in platelet size is
to be significant, and may be due to the observed after 6 hr at 1500 F (see Fig.
precipitation of Ni3(Ti, Al) as was sug- 13 for comparison). However, the anneal
gested to be the reason for the initial at 1800 F for 6 hr produced especially
strengthening seen in Fig. 10. After 1 large martensite. The Widmanstatten
hr, the material is losing strength and structure of the martensite is also easily
continues to do so with respect to time. seen in* the microstructure of the speci-
This loss in strength probably is the men annealed at 1800 F for 6 hr.
result of austenitic grain growth.
Figure 27 shows the microstructure CONCLUSIONS
obtained with a specimen which has 1. The maraging steel investigated
been annealed at 1250 F for 2 hr, air has an apparent as-received grain size
cooled to room temperature, and then that is considerably smaller than ASTM
aged at 875 F for 8 hr. This figure is No. 8.
very similar to Fig. 9. From this it is 2. Annealing in the temperature range
inferred that the microstructure is 1200 to 1250 F produces austenite which
relatively stable, and is not affected is retained upon cooling to room tem-
significantly by aging. However, the perature.
continuous phase does appear to have a 3. Reverted austenite in 18Ni-9Co-
rougher appearance in Fig. 27 than it 5Mo sheet displays a high" degree of
does in Fig. 9. This is hi agreement with preferred orientation.
the aforementioned suggestion that the 4. Annealing in the 1200 to 1250 F
continuous phase is martensite because range increases annealed ductility and
the martensite has already been shown ultimate strength, and can lower or
to become somewhat coarser in appear- raise the annealed yield strength de-
ance as it is aged. pending upon the time that the specimen
Material containing stabilized aus-
was held at temperature.
tenite does not respond to aging as well
5. No changes in microstructure were
as material that is wholly martensitic.
This is shown by the points on the observed to occur with respect to time
ordinate scale in Fig. 23. The lack of a when annealed from 2 to 18 hr at 1200 F.
proper aging response is probably due 6. Microstructure of aged martensite
to chemical segregation. The austenite, is coarser in appearance than that of
as mentioned previously, is high in annealed martensite. In addition, as the
nickel and carbon, but probably con- aging temperature and time are in-
tainsCopyright
little by
or ASTM
no molybdenum and creased, the microstructure becomes
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CORN ON 18Ni-9Co-5Mo MARAGING STEEL SHEET 77

7. Some reversion to austenite occurs Further straining beyond this amount,


after an aging heat treatment of 950 F however, results in a loss in strength.
for 8 hr. 11. Reverted austenite can be trans-
8. Duplex aging heat treatments re- formed by tensile cold working to a
quire less heat treatment time to reach product that is capable of being aged,
a specified strength level than do single and the evidence is strong that this
aging heat treatments. product is martensite.
9. No difference in microstructure 12. As the annealing temperature is
could be discerned between single- and increased above 1500 F, the resultant
double-aged specimens. martensitic structures obtained after
10. Marforming increases strength up subsequent aging contain increasingly
to 2 per cent tensile plastic strain. larger martensitic platelets.

REFERENCES
(1) R. F. Decker, J. T. Eash, and A. J. Gold- (10) C. Crussard, M. Kron, A. Constant, and
man, "18% Nickel Maraging Steel," J. Plateau, Discussion of "The Charac-
Transactions, American Society for Metals, teristics of 9% Nickel Low-Carbon Steel,"
Vol. 58, No. 1, March, 1962. Transactions, American Society for Metals,
(2) "Maraging Steels—Preliminary Data," Vol. 55, 1962, p. 1021.
Allegheny Ludlum Steel Corp., Pittsburgh, (11) B. Edmundson, "Thermal Stabilization of
Pa., 1961. Austenite in a 10% Ni, 1% C Steel," Acta
(3) S. Floreen and R. F. Decker, "Heat Treat- Metallurgica, Vol. 5, April, 1957.
ment of 18% Maraging Steel," Transac- (12) C. M. Younkin, Discussion of "Heat
tions, American Society for Metals, Vol. 55, Treatment of 18% Maraging Steel,"
No. 3, September, 1962. Transactions, American Society for Metals,
(4) R. F. Decker, "Maraging Steels; Structure- Vol. 55, No. 3, September, 1962.
Property Relationships," Technical Paper (13) M. Brown, "Metallurgical Characteristics
371, Research Laboratory; International of A-286 Alloy," Defense Metals Informa-
Nickel Co., Bayonne, N. J., April 1, 1963. tion Center, Memorandum 59, Battelle
(5) C. M. Marshall, R. F. Hehemann, and Memorial Institute, Columbus, Ohio, July
A. R. Trolano, "The Characteristics of 9% 26, 1960.
Nickel Low-Carbon Steel," Transactions, (14) Dislocations and Mechanical Properties of
American Society for Metals, Vol. 55, 1962, Crystals, John Wiley & Sons, Inc., New
p. 135. York, N. Y., 1957.
(6) A. Gilbert and W. S. Owen, "Diffusionless (15) E. S. Machlin and M. Cohen, "Isothermal
Transformations in Iron-Nickel, Iron- Mode of the Martensitic Transformation,"
Chromium, and Iron-Silicon Alloys," Ada American Institute of Mining, Metal-
Metallurgies Vol. 10, 1962, p. 45. lurgical, and Petroleum Engineers, Trans-
(7) F. W. Jones and W. T. Pumphery, "Free actions, Vol. 194, 1952, p. 489.
Energy and Metastable States in, the Iron- (16) W. F. Barclay and J. K. Jackson, Discus-
Nickel and Iron Manganese Systems," sion of "18% Nickel Maraging Steel,"
Journal of the Iron and Steel Institute, Transactions, American Society for Metals,
London, October, 1949, p. 121. Vol. 55, 1962, p. 1069.
(8) N. P. Allen and C. C. Earley, "The Trans-
formations a —> y and y —> a in Iron-Rich (17) A. Siede, "A Review of Developments on
Binary Iron-Nickel Alloys," Journal of the Maraging Steels," Curtiss-Wright Corp.,
Iron and Steel Institute, London, December, May, 1962.
1960, p. 281. (18) "Maraging Steel Project Review," Aero-
(9) M. Hansen, Constitution of Binary Alloys, nautical Systems Division, Technical
McGraw-Hill Book Company, Inc., New Documentary Report 63-262, Wright-
York, N. Y., second edition, 1958. Patterson Air Force Base, Ohio, May, 1963.

Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
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THE METALLURGY AND PROPERTIES OF COLD-ROLLED
AM-350 AND AM-355 STEELS
BY T. H. McCuNN,1 G. N. AcGEN,1 Personal Member ASTM, AND
R. A. LuLA,1 Personal Member ASTM

SYNOPSIS
AM-350 and AM-355 are controlled-transformation precipitation-hardening
steels. AM-350 is more familiarly known in sheet and AM-355 in bar form
where hardening is produced by heat treatments alone. Annealed at 1900 F, the
materials are essentially austenitic at room temperature, but the austenite is
very unstable. By cold deformation, a substantial amount of martensite is
formed. The mechanical properties of cold-rolled products can be controlled
over a wide range and vary as functions of per cent deformation, amount of
martensite produced, and tempering treatment.
The mechanical properties of these materials are extremely interesting from
an engineering point of view. Higher strength with better toughness can be at-
tained than with Type 301, which is the stainless steel generally used in the
cold-rolled condition.
This paper deals with the metallurgy and properties of cold-rolled AM-350
and AM-355. The mechanical properties are shown as functions of the amount
of deformation, deformation temperature, and prior annealing temperature.
More detailed mechanical properties of AM-350 and AM-355 CRT (20 to 30
per cent reduction) are given including toughness studies. AM-350 in particu-
lar has been evaluated for the supersonic transport and appears to meet the
stringent requirements for this application.

The cold-rolled austenitic stainless- was developed and gained considerable


steel sheet products were first used as acceptance, especially in the transpor-
structural materials shortly before the tation industry, and also in other fields
Second World War. While the composi- where high strength combined with
tion originally used was the 18 per cent corrosion resistance was needed.
chromium, 8 per cent nickel steel with a The mechanism of work hardeniif of
rather high carbon content, it was soon metastable austenitic steels was first
discovered that higher strength could be described by Aborn and Bain (I).2 Dur-
attained by cold working a leaner com- ing the period of commercial develop-
position with 17 per cent chromium and ment of these steels considerably more
7 per cent nickel. Thus, AISI Type 301 work on the mechanism of work harden-
1
Project supervisor, research associate, and 2
chief research metallurgist—stainless steels, The boldface numbers in parentheses re-
respectively, Research Center, Allegheny Lud- fer to the list of references appended to this
lum Steel Corp., Brackenridge, Pa. paper'.
78
McClJNN ET AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 79

ing was done (2,3,4). Quantitative in- other hand, promote the formation of
formation relating composition with austenite. By proper balance of these
stability of austenite during plastic elements it is possible to have a com-
deformation was eventually developed pletely austenitic structure free of delta
by Post and Eberly (5). Later Eichelman ferrite. This is, in general, desirable for
and Hull (6) determined by dilatometric ease of processing since steels containing
methods the relative effectiveness of duplex structures are difficult to hot
each element in lowering the Ms tem- roll. The freedom from delta ferrite is,
perature. Systematic studies by Cina however, unessential.
(7,8) and Angel (9) clarified the relation- The austenitic steels in the composi-
ship between stress, plastic deformation, tion range of 18 per cent chromium, 8
composition, temperature of deforma- per cent nickel can transform to marten-
tion, Ms and Md, and amount of mar- site when plastically deformed such as
tensite formed. in cold rolling. The stability of the aus-
The relationship between processing tenite which respect to transformation
and work hardening of 17/7 chromium- to martensite is also controlled by the
nickel steels was investigated by Lincoln balance of alloying elements. Almost all
and Mather (4) and Espey et al (10). the elements tend to stabilize the austen-
They showed that the rate of work ite, even those promoting delta-ferrite
hardening during rolling is constant formation at high temperatures. The
above approximately 250 F and under relative stabilizing power of each element
approximately —50 F but decreases varies considerably, and it can be meas-
considerably from —50 F to +250 F. ured as the effectiveness of each element
Attempts have been made to take ad- in lowering the Ms temperature of the
vantage of the high strength obtained alloy. The most powerful elements in
by cold rolling at subzero temperatures this respect are carbon and nitrogen.
(11,12) for developing higher strength Other common alloying elements such as
Type 301, but the process has remained nickel, chromium, manganese, and sili-
in the experimental stage because of con are much less potent.
technological difficulties. With sufficient alloying elements,
In this short review we have mentioned the Ms temperature can be depressed
only those steps that we consider to under room temperature and in this
be most important in the development way it becomes possible to retain an
of metastable austenitic steels. There are, austenitic structure after cooling from
however, a considerable number of other high temperatures. With a proper com-
papers which have contributed to the position balance, martensite can be
knowledge of the mechanism of work formed by plastically deforming the
hardening of these steels. In the follow- austenite at temperatures above the Ms.
ing an attempt will be made to summa- By increasing the temperature of plastic
rize this work to date. deformation, the amount of martensite
In iron-chromium-nickel steels the formed decreases and above a certain
structure after cooling from high tem- temperature called the Md, the trans-
perature is determined by the balance formation does not take place.
of the alloying elements. Chromium, Although much research has been
molybdenum, tungsten, silicon, titanium performed on metastable austenitic
and columbium tend to promote the steels, until recently there was only one
formation of delta ferrite. Carbon, commercial alloy based on this principle.
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
nitrogen, manganese, and nickel, on the This alloy is AISI Type 301 available
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80 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

in four cold-rolled tempers varying in is small. The strength level developed


yield strength from 75,000 to 140,000 in these steels is above' 200,000 psi, and
psi, minimum values, and in tensile their formability is superior to Type 301
strength from 125,000 to 185,000 psi, at the same strength level.
minimum values. A nonstandard, extra-
hard temper of 160,000 psi minimum Metallurgical Characteristics of AM-350
yield strength has recently found limited and A M-355:
usage in missiles. For all practical pur- AM-350 and AM-355 were specifically
poses AISI Type 301 is limited to about developed as controlled-transformation
200,000 psi strength level. Strength above stainless steels; that is, either an austen-
200,000 psi can be attained but requires itic or martensitic structure may be
excessive cold rolling, and the ductility produced in the alloys through heat
is low while the directionality of mechan- treatment alone. Control of structure,
ical properties is high. or Ms temperature, is produced through
Because of the special features of the the precipitation of M23C6 carbides.
stress-strain curve of cold-rolled Type Such precipitation alters the composi-
301 and the high directionality, particu- tion of the matrix and, thereby, changes
its austenite stability or stability against
TABLE 1—NOMINAL COMPOSITION OF transformation to martensite.
AM-350 AND AM-355.
To produce the desired control of
Element AM-350 AM-355
structure, the chemical composition of
Carbon 0.08 0.13 these alloys and other controlled-trans-
Manganese 0.80 0.95 formation steels must be controlled,
Silicon 0.25 0.25 and are controlled, to unusually narrow
Chromium 16.50 15.50
Nickel 4.25 4.25 limits. The chemical compositions of the
Molybdenum 2.75 2.75 alloys, given in Table 1, also make the
Nitrogen 0.10 0.10 alloys adaptable to hardening during
cold working through the formation of
larly the large difference between the martensite. The ensuing discussions
tensile yield and compressive yield will be largely confined to AM-355 but,
strength in the rolling direction, special in most cases, are also applicable to
design procedures have been advocated AM-350. The alloys differ in certain
by Watter and Lincoln (13). respects as controlled by their differ-
Recently Malagari and Lena (14) have ences in composition. AM-350, because
established that the degree of directional- of its higher chromium content, is
ity, as expressed above, decreases with somewhat more stable against trans-
increasing instability of the alloy. Thus, formation during plastic deformation and
alloys forming more martensite than contains approximately 10 per cent delta
Type 301 have mechanical properties ferrite. AM-355, on the other hand,
which are more attractive to the de- generally contains 0 to 5 per cent delta
signer. ferrite. AM-355, because of its lower
AM-350 and AM-355 alloys, the topic stability and slightly higher carbon
of this paper, are both metastable austen- content, has somewhat higher mechani-
itic steels with the austenite less stable cal properties than AM-350 with a given
than that of Type 301. The stress-strain amount of cold reduction.
curve of these steels has a longer straight- AM-355 in its most stable condition,
line portion, more like the low-alloy that is, upon annealing from tempera-
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
martensitic steels, and the directionality tures of about 1875 F or higher where
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McClJNN ET AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 81

all carbides are dissolved, is somewhat temperature at annealing temperatures


less stable than Type 301. The usual in excess of 1875 F is caused by increases
Ms temperature range, measured on a in the austenitic grain size. Experiments
large number of commercial heats, is on similar compositions (6) indicate that
about —50 to 70 F in this condition. an increase in one ASTM grain size
The Ms temperature of the alloy, as a number causes an 8-F elevation in
function of solution-annealing tempera- Ms temperature.

FIG. 1—Effect of Solution Anneal Temperature on Ms Range of AM-355.

ture, is illustrated in Fig. 1. At lower By adjusting the annealing tempera-


annealing temperatures the spread in ture, a wide variation in austenite sta-
Ms temperatures between various heats bility can be achieved. Figure 1, which
is relatively small. The spread is largely illustrates this, most aptly applies to
controlled by variations in nitrogen thermal heat treatments, but also ap-
content. At 1875 F and above the spread plies to martensite formed as a result
in Ms values becomes larger and is con- of deformation. This is true since there
trolled primarily by variations. in: both appears to be a definite relationship
carbon and nitrogen content, the two between Ms temperatures and Md
elements in the composition that have, temperatures, that is, the maximum
by far, the greatest effect upon the Ms temperature at which a given amount of
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temperature. The slight increase in Ms cold reduction will produce a given
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82 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

amount of martensite (5). The Md tem- cipitation treatments prior to rolling),


perature to produce a measurable by changing the rolling temperature, or
amount of martensite with 80 per cent by varying the amount of reduction.
reduction appears to be about 600 F The hardness or strength of the mar-
above the Ms temperature in similar tensite can be varied by regulating the
compositions (6). dissolved nitrogen and carbon content.

FIG. 2—Effect of Cold Reduction on Longitudinal Tensile Properties of AM-355.

When cold rolling unstable alloys of In AM-355 the carbon content, but not
this type, the strength produced in the the nitrogen, can be adjusted by heat
alloy appears to depend upon two or treatments prior to rolling as illustrated
more factors. The strength level with a in Fig. 1.
given deformation will increase with Figure 2 illustrates the effects of cold
amount of martensite, and will also reduction on the mechanical properties
increase with the hardness or strength of AM-355. Initial annealing tempera-
of the martensite thus produced (9). The tures of 1900 and 1710 F are represented
former can be varied either by changing in the figure. Upon annealing at 1710 F
the Copyright by ASTM
composition Int'l (allorrights
(by alloying reserved); Mon Dec 7 13:15:25 EST 2015
by pre- all but about 0.05 per cent carbon is
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McCUNN ET AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 83

FIG. 3—Effect of Tempering Temperature on Longitudinal Tensile Properties of AM-355 Cold


Rolled 30 per cent.

precipitated as M23C6 carbides so that


the Ms temperature is about 175 F, as
shown in Fig. 1. Prior to rolling, then,
the alloy contains a mixed structure of
martensite and highly unstable retained
austenite. The retained austenite readily
transforms to martensite during cold
rolling as evidenced by the steep increase
in yield strength at small reductions.
As little as 5 per cent cold rolling is
sufficient to reduce the retained austenite
to a value below 20 per cent. Upon near
completion of transformation of the
austenite to martensite, at about 10
per cent reduction, the work hardening
curve levels off and increases only
slightly with further reduction. The
further slight increase in strength is
attributed to work hardening of the
martensite.
Upon annealing at 1900 F all the car-
bides are dissolved, causing a reduction FIG. 4—Microstructure of AM-355 Annealed
Copyright by ASTMtoInt'l (all rights at Dec
reserved); Mon 1900 7F,13:15:25
Cold Rolled 30 per cent, and Tem-
EST 2015
in Ms temperature room temperature pered 3 hr at 850 F (X500).
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84 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

or below. The retained austenite here is At about the same strength level,
considerably more stable than that ob- annealing at 1900 F produces somewhat
tained upon annealing from 1710 F. higher ductility than annealing at 1710 F.
After 30 per cent reduction, for example, In addition the initial higher temperature
the alloy still contains 60 to 70 per cent annealing treatment produces material
retained austenite. As a result, work having better formability, corrosion

FIG. 5—Structure of AM-355 Annealed at 1900 F, Cold Rolled 30 per cent, and Tempered (X5000).

hardening proceeds more slowly but resistance, and stress-corrosion resist-


continues to increase to beyond 50 per ance. The 1900 F anneal, however, has
cent cold reduction. At about 25 to 30 the disadvantage of producing greater
per cent reduction the yield strengths directionality in properties in agreement
of sheet annealed at either temperature with the results by Malagari and Lena
are about equivalent. Beyond this value (14). In view of these characteristics the
the sheet annealed at 1900 F, by virtue alloy is almost exclusively produced
of its higher carbon content, is stronger after annealing in the range of 1875 to
evenCopyright
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retained austenite are still
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McCUNN ET AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 85

what prone to delayed cracking, partic- tensile properties of the alloy annealed
ularly in heavy gages. This can be, at 1900 F and cold rolled 30 per cent.
and is, eliminated by a short heating or Temperatures in excess of about 900 F
tempering operation in the temperature produce a precipitous decrease in both
range of about 750 to 850 F. The reac- yield strength and elongation. These
tion taking place during tempering is coincide with a sharp increase in the
extremely rapid and is, therefore, amount of martensite present in the

FIG. 6—Effect of Rolling Temperature on Longitudinal Tensile Properties of AM-355.

amenable to line heat-treating opera- alloy, as measured magnetically, upon


tions. As little as 1 min at temperature subsequent cooling to room tempera-
is sufficient to produce nearly full effects. ture.
The tempering operation produces a Figure 4 is a micrograph at X500
marked increase in yield strength, a showing the distribution of austenite
smaller decrease in tensile strength, and and martensite in cold-rolled AM-355.
generally has little effect on the elonga- This particular specimen was annealed
tion.Copyright
Figure 3byshows
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(all rights at Mon
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F, cold rolled 30
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tempering treatments on
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86 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

etching phase is tempered martensite, Figure 6 shows the effects of cold-


while the remainder of the matrix is rolling temperature upon the longitudinal
austenite. A few dark streaks are ob- mechanical properties of AM-355. The
served. These are carbides that were not strip was initially annealed at 1950 F,
dissolved during the short annealing cold rolled 30 per cent at the various
operation at 1900 F. Figure 5 is a surface temperatures and tempered 3 hr at
replica of the alloy at X5000 in the 825 F. The strip, in this case, was cooled
same condition. The spherical particles or heated to the desired temperature
are polystyrene balls used to show the before each pass. During rolling of
direction of shadowing. Electron micros- continuous coils, the material generally
copy shows that one, and possibly two, attains temperatures of about 150 F. This
fine precipitates are produced in the is the reason for the higher than normal
martensite during tempering. Based properties attained during rolling at
upon similar work on the alloy in the room temperature. Based upon Fig. 6
conventional heat-treated condition, one the Md temperature, for 30 per cent
of these appears to be an M2X type reduction, is between 200 and 300 F for
phase, tentatively identified as Cr2N. the alloy. The Md temperature will, of
Tempering at temperatures in excess of course, shift upwards if the amount of
about 900 F causes precipitation of deformation is increased.
coarser particles in the martensite be-
lieved to be M23C6 carbides. This pre- Mechanical Properties of Cold-Rolled
cipitation of carbides, as well as relief AM-355 and AM-350:
of internal stresses during tempering, As shown in the previous section, an
is believed to lead to the additional extremely wide range of strength can be
formation of martensite upon cooling obtained in AM-355 by controL of the
from high tempering temperatures, as reduction in cold rolling. Two strength
shown in Fig. 3. levels became of major interest and,
The residual austenite present after consequently, were more thoroughly ex-
annealing at 1900 F and cold rolling 30 plored with respect to elevated-tem-
per cent is on the order of 50 to 75 per perature properties, corrosion resistance,
cent. The retained austenite, based upon and formability. These two strength
mechanical property data, is stable at levels are achieved by cold rolling 20 to
temperatures of —100 F. If the alloy is 30 per cent and about 70 per cent after
not cold rolled prior to cooling to a 1900 to 1950 F anneal, both followed
—100 F, 50 to 90 per cent martensite is by tempering in the range of 750 to
formed (15). This indicates that the 850 F. The former has become known as
cold rolling has appreciably stabilized the CRT condition and the latter, the
the austenite against transformation by XH condition.
thermal treatments. This is in agreement Most of the mechanical property data
with data by Fiedler et al (16) to the shown in this section were obtained on
effect that stainless steels exhibit stim- AM-355. More complete data on fatigue
ulation of transformation by small strength and fracture toughness, how-
strains and retardation at strains ever, are available on AM-350 CRT.
greater than about 12 per cent. Partial Thus, some properties will be shown for
elimination of this mechanical stabiliza- AM-355, while other properties will be
tion effect is believed to contribute for AM-350. All indications are that the
strongly to the increase in martensite alloys can be used interchangeably.
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produced by temperingbyabove 900 F.
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McCUNN ET AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 87
TABLE 2—TYPICAL TENSILE PROPERTIES OF AM-355 CRT AND XH AT
ROOM TEMPERATURE.

Condition Test Direction 0.2% Yield Ultimate Tensile Elongation,


Strengh, psi Strength, psi %

CRT longitudinal 220 000 240 000 17.0


transverse 200 000 240 000 15.0
XH longitudinal 340 000 342 000 1.0
transverse 335 000 360 000 1.0

FIG. 7—Tensile and Compressive Properties of AM-355 CRT.

is the strength level of the material on between longitudinal and transverse


which the data were obtained. testing directions are typical of cold-
Typical tensile properties at room rolled austenitic stainless materials.
temperature for both the CRT and XH Elevated-temperature tensile and com-
conditions are given in Table 2. The pressive properties of a typical heat in
CRT condition offers a material of the CRT condition are shown in Fig. 7.
around 200,000 psi yield strength with The strength at elevated temperatures
good elongation, while the XH condition is quite good and does not decrease
offers a material with very high yield precipitously until the temperature is
strength of about 335,000 psi. The high enough to result in over tempering.
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88 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

FIG. 8—Transverse Tensile Properties of AM-355 XH.

TABLE 3—RUPTURE STRENGTH OF perature, the elongation increases some-


AM-355 CRT.
what and then decreases again. Ele-
Test Tempera- Stress for Rupture, ksi vated temperature tensile properties of a
ture, F Ihr 10 hr 100 hr 1000 hr typical heat in the XH condition are
192 191 190 182
shown in Fig. 8. The very rapid decrease
800
900 171 158 135 116 in strength starts at a somewhat lower
1000 128 110 85 65 temperature than that of the CRT condi-
tion because of the higher amount of
above room temperature is due to the cold work of the XH condition.
lack of martensite formation during Rupture strengths in the CRT condi-
testing. With further increase in tem- tion are given in Table 3. At 800 F the

TABLE 4—CREEP PROPERTIES OF AM-355 CRT."

Test Creep Strain from Loading to Indicated Times, % Minimum


Temperature, F Stress, psi Creep Rate,
Ihr 10 hr 100 hr 500 hr 1000 hr %/1000 hr

700 190 000 0.045 0.101 0.151 0.186 0.211 0.047


800 70 000 0.008 0.029 0.055 0.086 0.108 0.0013
800 100 000 0.015 0.034 0.093 0.150 0.196 0.062
800 150 000 0.051 0.115 0.175 0.273 0.361 0.149
0 Determined on material having tensile properties about 20,000 psi higher than typical proper-
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ties shown in Fig. 7.
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McCuNN ET AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 89

rupture strength up to 1000 hr life is very limited. The material has been
not much lower than the short-time fabricated into spiral-wound cases joined
tensile strength. Some creep data at 700 by spot welding or by adhesives.
and 800 F are given in Table 4. AM-355 CRT and XH are not suit-
Stress-corrosion data on a typical able where fabrication requires brazing
heat of AM-355 CRT are given in Table or fusion welding, because the effects of
5. Resistance in these accelerated labora- the cold work would be destroyed.
tory tests and other environments is However, the materials are adaptable to
good but not as good as that of Type spot-welded structures in which proper

TABLE 5—STRESS-CORROSION PROPERTIES OF AM-355 CRT."

Stress, per
cent of TTPI Q»n & Alternate Kure Beach
Ultimate HCl-Se02 immersion0 Salt Sprayd SaltSlurry^ ^Jg"
Tensile 80 ft Lot 800 ft Lot
Strength

10 G-359* G-359 G-24 hr G-750 G-750


G-359* G-359 G-24 hr G-750 G-750

35 G-359* F-133 F-24 hr G-1000 G-1000


G-359A C-209 C-3 hr G-1000 G-1000

50 C-2 hr' G-359* G-359 F-2 hr C-84 G-1000


F-2 hr» G-359A G-359 F-12 hr C^7 G-1000

70 F-3 hr G-359 * C-l F-12 hr G-800 C-84 C-167


F-l hr G-359A G-360 F-12 hr G-800 C-100 C-136

0 Testing times are in days unless otherwise stated.


6 1 per cent selenium dioxide in 50 per cent by volume hydrochloric acid solution at room tem-
perature.
c 3^i per cent NaCl solution at a cycle of 10 mm. immersion and 50 min air dry.
d 20 per cent neutral salt spray cabinet.
e Moist NaCl deposit on stressed area at about 250 F.
f Cracked.
" Complete failure.
h
No cracks.

301 cold rolled and stress relieved to configuration and design offset the low
similar strength levels. strength of the weld area.
While AM-355 CRT has high strength,
the material has relatively good forma- Fracture Toughness:
bility. In a Vee-block bend of 120 deg, AM-350 and AM-355 in the CRT
minimum bend radii are about IT (T = condition were developed specifically for
sheet thickness) for longitudinal and IT advanced airframe application as fuse-
for transverse directions. The material lage and wing skins. In this respect one
can be stretch-formed to some extent. of the important properties requiring
Both bending and stretch-forming should extensive study is fracture toughness.
be carried out at room temperature, AM-350 and AM-355 CRT have been
since the good formability is dependent included in many of the current investi-
upon additional transformation of mar- gations being conducted by United
tensite during deformation. The for- States Government agencies or private
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of AM-355XH Int'lof(all rights
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90 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

gram is that of NASA for evaluation of posed at 550 F at the same stress level.
sheet alloys for the Mach 3 supersonic The notch strength to yield strength
transport. ratio is used as a qualitative measure of
For the purpose of this paper we will fracture toughness. The data are aver-
rely solely on the data obtained by ages of longitudinal and transverse
NASA Lewis Research Center3 in a properties since the difference between
program concerned with screening ma- the two is rather small. As shown in
terials for the supersonic transport. The Table 6, the material has very good
program consisted of determination of fracture toughness at room temperature
ultimate tensile and yield strengths as before exposure. At 650 F before ex-
well as sharp notch-tensile strength posure, the material shows a slight de-
using the l-in.-wide specimen recom- crease in fracture toughness, which is a
mended by the ASTM Special Com- characteristic of all ferrous alloys inves-
mittee on Fracture Testing of High- tigated by NASA. Exposure of 1000 hr

TABLE 6—SMOOTH AND NOTCHED TENSILE PROPERTIES OF AM-350 CRT.0


Smooth Notched Ratio of
Exposure Time, f^™ ^^ Ultimate Notched
nr 0.2% Yield Ultimate Tensile UTS to
ture, F ture, F Tensile
Strength, psi Strength, Strength, psi Smooth
psi 0.2% YS

room 180 000 220 000 205 000 1.14


650 145 000 175 000 150 000 1.04

1 000 650 room 180 000 220 000 205 000 1.14
650 145 000 175 000 150 000 1.04

3 000 650 650 145 000 175 000 128 000 0.88

10 000 550 650 142 000 170 000 135 000 0.95

Cold reduced 20 per cent and tempered 3 hr at 825 F.

Strength Materials (18). While AM-350 TABLE 7—FATIGUE BEHAVIOR OF


AM-350 CRT.
and AM-355 were tested at three
strength levels, produced by cold rolling Test Mean Fatigue
Strength
20, 30, and 45 per cent and tempering, Test Specimen" Tempera- Stress, at 10' Cy-
ture, F psi cles, psi
AM-350 cold rolled 20 per cent has the
most attractive properties, and there- Smooth -nor 40 000 120 000
fore has been investigated more exten- Smooth room 20 000 90 000
Smooth room 40 000 112 000
sively, especially with respect to the Smooth 550 F 40 000 110 000
effect of exposure under stress on notch
strength. Notched6 -110 F 40 000 60 000
Notched room .20 000 40 000
The data obtained at Lewis Research Notched room 40 000 55 000
Center are shown in Table 6. The 1000 Notched 550 F 40 000 57 500
and 3000-hr specimens were exposed 0Longitudinal specimens.
at 650 F with a stress of 40,000 psi, 6Theoretical stress concentration factor of
while the 10,000-hr specimens were ex- the notch, Kt, was 4.0.

3 Most of these data were published (17) ; at 650 F has no effect on the fracture
additional unpublished NASA data were ob- toughness at room temperature or 650 F.
tainedCopyright
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McCuNN EX AL ON COLD-ROLLED AM-350 AND AM-355 STEELS 91

and 550 F, respectively, show a slight or by the amount of cold reduction. Low
decrease in fracture toughness when annealing temperatures, by virtue of the
tested at 650 F. presence of carbides, result in a very
unstable austenite and low carbon con-
Fatigue Properties: tent of the austenite. Some martensite
Another important property in con- may form upon cooling to room tem-
nection with application of these ma- perature and substantial amounts of
terials in airframes is fatigue strength. martensite are formed with low per-
Tables 7 and 8 show data obtained at centages of cold reduction. The strength
Battelle Memorial Institute for NASA of the martensite is relatively low be-
on AM-350 CRT (19) .4 At a mean stress cause of its low carbon content. High
of 40,000 psi, the fatigue strength at 107 annealing temperatures result in a more
cycles is approximately 50 per cent of stable austenite and maximum carbon
the tensile strength for smooth speci- content of the austenite. The structure
is austenitic at room temperature, and
TABLE 8—TENSILE PROPERTIES OF
AM-350 CRT USED FOR FATIGUE TESTS. all the martensite formed is produced
during cold rolling. The strength of the
Test Ultimate Elonga-
0.2% Yield
Temperature, Strength, Tensile
psi Strength, tion in martensite is relatively high because
F psi 2 in., %
of its high carbon content. This latter
-110 F 221 000 272 500 20.2 method of obtaining the desired strength
Room 221 000 233 000 21.1 level is preferred for commercial produc-
550 F 184 000 201 000 3.7 tion of these alloys.
Annealed at 1900 to 1950 F, cold
mens, while the notched fatigue strength rolled about 30 per cent, and tempered,
is approximately 50 per cent of the AM-350 and AM-355 have a yield
smooth strength. strength in the neighborhood of 200,000
psi with about 15 per cent .elongation.
SUMMARY Elevated-temperature short-time
AM-350 and AM-355 are controlled- strength, rupture strength, and creep
transformation stainless steels, in which strength are very good up to about 800 F.
high strength can be obtained upon The alloys have relatively good forma-
cold rolling as well as by heat treatment. bility and exhibit good stress-corrosion
The compositions of the alloys are resistance. This excellent combination
balanced so that substantial amounts of of properties has led to more extensive
martensite are formed during cold studies in connection with use of the
rolling. The strength is dependent alloys in advanced airframes. These
primarily on the amount of martensite investigations have shown that the
formed and the hardness or strength of alloys have good fatigue strength in the
the martensite produced. The amount of temperature range of —110 to 550 F.
martensite formed can be controlled by Fracture toughness has remained good
annealing treatments prior to cold rolling after 10,000-hr exposure under stress.

REFERENCES
(1) R. H. Aborn and E. C. Bain, "Nature of the Nickel-Chromium Rustless Steels,"
Transactions, American Society for Steel
4 We are indebted to Batelle Memorial Treating, Vol. 18, 1930, pp. 837-873.
Institute and NASA
Copyright for permission
by ASTM Int'l (all torights
publish (2) V.
reserved); N. Dec
Mon Krivobok, R. A. Lincoln,
7 13:15:25 EST 2015and R.
the data. Patterson, "Austenitic Stainless Alloys,"
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92 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

Transactions, American Society for Met- (11) V. N. Krivobok and A. M. Talbot, "Effect
als, Vol. 25, 1937, pp. 637-677. of Temperature on the Mechanical Prop-
(3) R. Franks and W. O. Binder, "Tension erties, Characteristics, and Processing of
and Compression Stress-Strain Character- Austenitic Stainless Steels," Proceedings,
istics of Cold-Rolled Austenitic Chromium- Am. Soc. Testing Mats., Vol. 50, 1950,
Nickel and Chromium-Manganese-Nickel pp. 895-928.
Stainless Steels," Journal of the Aeronauti- (12) C. R. Mayne, Low-Temperature Properties
cal Sciences, Vol. 9, September, 1942, pp. of High-Strength Aircraft and Missile
419^38. Materials, ASTM STP 287, Am. Soc.
(4) R. A. Lincoln and W. H. Mather, "Effect Testing Mats., 1961, p. 150.
of Temperature of Cold Rolling, Tempera- (13) M. Watter and R. A. Lincoln, Strength
ture of Testing and Rate of Pulling on of Stainless Steel Structural Members as
Tensile Properties of Austenitic Stainless Function of Design, First Edition, The
Steels with Low Nickel Content," Re- Republic Press, Pittsburgh, Pa. 1950.
gional Technical Meetings, American Iron (14) F. Malagari and A. J. Lena, unpublished
and Steel Institute, 1947-1948. data presented at AIME meeting, Pitts-
(5) C. B. Post and W. S. Eberly, "Stability burgh, Pa., November 2, 1962.
of Austenite in Stainless Steels," Trans- (15) G. Aggen, "Phase Transformations and
actions, American Society for Metals, Heat-Treatment Studies of a Controlled-
Vol. 39, 1947, pp. 868-888. Transformation Stainless Steel Alloy," D.
(6) G. H. Eichelman, Jr. and F. C. Hull, Eng. Sc. Thesis, Rensselaer Polytechnic
"The Effect of Composition on the Tem- Institute, August, 1963.
perature of Spontaneous Transformation (16) H. C. Fiedler, B. L. Averbach, and M.
of Austenite to Martensite in 18-8 Type Cohen, "The Effect of Deformation on
Stainless Steel," Transactions, American the Martensitic Transformation in Austeni-
Society for Metals, Vol. 45, 1953, pp. 77- tic Stainless Steels," Transactions, Ameri-
95. can Society for Metals, Vol. 47, 1955, pp.
(7) B. Cina, "Effect of Cold Work on the 267-285.
7 —» a Transformation in Some Fe-Ni-Cr (17) G. B. Espey, R. T. Bubsey, and W. F.
Alloys," Journal of the Iron and Steel Brown, Jr., "A Preliminary Report on the
Institute, Vol. 177, August, 1954, pp. 406- NASA Sheet Alloy Screening Program for
422. Mach 3 Transport Skins," Proceedings,
(8) B. Cina, "The Metastability of Austenite Am. Soc. Testing Mats., Vol. 62, 1962,
in an 18-8 Cr-Ni Alloy," Journal of the pp. 837-856.
Iron and Steel Institute, Vol. 179, March, (18) "Fracture Testing of High-Strength Sheet
1955, pp. 230-239. Materials: A Report of a Special ASTM
(9) T. Angel, "Formation of Martensite in Committee," ASTM Bulletin 243, Jan-
uary, 1960, p. 29; also ASTM Bulletin
Austenitic Stainless Steels," Journal of
244, February, 1960, p. 18.
the Iron and Steel Institute, Vol. 177, May, (19) D. N. Gideon, C. W. Marschall, F. C.
1954, pp. 165-174. Holden, and W. S. Hyler, "Final Summary
(10) G. B. Espey, M. H. Johns, and W. F. Report on Exploratory Studies of Mechan-
Brown, Jr., Evaluation of Metallic Mate- ical Cycling Fatigue Behavior of Materials
rials in Design for Low-Temperature Ser- for the Supersonic Transport to National
vice, ASTM STP 302, Am. Soc. Testing Aeronautics and Space Administration,"
Mats., June, 1961, p. 140. June 30, 1963, Battelle Memorial Institute.

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DISCUSSION

J. L. CLUPPER1—With respect to can occur under conditions involving


manufacturing procedures, did you an- long times at high temperatures. Since
neal at 1900 F? If so, what was the a decarburized surface is less stable,
effect of decarburization on properties? larger amounts of martensite will be
What was your treatment for rolling formed upon subsequent cold rolling.
prior to final reduction? With excessive decarburization the sur-
T. H. McCuNN, G. N. AGGEN, AND face can transform almost completely to
R. A. LULA (authors)—The treatment martensite. The effect on properties
prior to the final cold reduction, as well will depend on the amount of marten-
as all intermediate gage treatments, is a site, the carbon content of the marten-
continuous anneal at 1900 to 1950 F. site, and the depth of the decarburized
We have not experienced decarburization layer. We can state in general terms that
to the extent that properties were seri- decarburization is detrimental to prop-
ously effected. However, decarburization erties such as formability and fatigue
1 The Carpenter Steel Co., Reading, Pa. life at room temperature.

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93
FRACTURE MICROMECHANICS IN HIGH-STRENGTH STEELS

BY BANI R. BANERjEE1

SYNOPSIS
Because tempered martensites provide some of the most desirable combina-
tions of strength and ductility, a study was made of secondary-hardening
steels—Type H-ll (Crucible 218) and Type 422, and a martensi tic-harden-
ing low-alloy high-strength steel, Type 4340—to relate fine structural aspects
to strength and fracture properties.
The fracture process was shown to consist of many discontinuous crack
initiation, coalescence, and propagation steps merging together to produce the
macroscopic fracture front. The observed large scatter in fracture toughness
of air-melt 4340 in the 500-F embrittlement region was explained in terms
of the high sensitivity of the fracture-toughness test to structural disconti-
nuities at inclusion-matrix interfaces in a deformation limited matrix. Such
effects were absent in vacuum-melted 4340 steels.
Tempering the two secondary hardening steels at temperatures well below
the secondary hardening region produced an optimum combination of strength
and toughness. A fourfold toughness benefit in 422 and a substantial benefit in
218 were thus demonstrated without loss of yield strength.
Tempered-martensite embrittlement, 500 F, and temper brittleness, 900 to
1000 F, were explained in terms of a unified mechanistic concept involving pre-
cipitation locking of dislocation intersections and jogs, along with high dislo-
cation densities during carbide re-solution and reprecipitation steps.

In the use of high-strength steels, the the critical stress needed to change a
problem of catastrophic brittle failure slowly propagating crack to a fast prop-
continues to challenge the designer and agating one. It involves the stress re-
baffle the metallurgist. Brittleness is a quired to change a plastic-crack growth
property that almost everyone intui- into an essentially elastic propagation.
tively understands, yet it is quite dim- This concept provides the basis of the
cult to precisely define. State of stress, ASTM recommended fracture-toughness
strain rate, section thickness, and tern- criterion, Kc , defined as the critical-
perature are among the significant stress intensification ahead of a slowly
macroscopic factors that affect brittle propagating crack, at the onset of rapid
behavior in metals. Of all the macro- crack propagation. Despite the known
scopic descriptors that have been used difficulties in precisely determining this
to define toughness or brittleness of parameter at its critical value, this con-
metals, the most significant one involves cept, when properly used, provides the
designer with an effective parameter
» Supervisor, Basic Research and Applied whkh he can uge with & reasonable de-
Physics Sections, Research Division, Crucible
Steel Company of America, Pittsburgh, Pa. gree of Safety.
94
BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 95

In addition to the macroscopic con- 0.120-in. sheet, and chemical analyses,


siderations, the metallurgist must con- grain size, and inclusion ratings were
tend with the detailed structural aspects determined for each. Table 1 gives the
of fracture, because in the ultimate chemical analyses of the materials.
analysis, the structural and atomistic Sheet-tension tests were used for
steps that underlie these macroscopic both smooth and notch-tensile prop-
phenomena must be understood before erties. For smooth tension testing, speci-
the metallurgist can intelligently opti- mens of 2-in. gage length, 0.35-in.-wide,
mize strength and ductility in his mate- and 0.067-in.-thick were used to obtain
rials. ultimate tensile and 0.2 per cent yield
Therefore, this study (l)2 was under- strength. For notch properties, center-
taken to carefully reexamine the fine notched (2) fatigue-cracked specimens
structural characteristics of some well- 0.067 by 2 by 7.5 in. were used. Speci-
known high-strength materials and to men blanks were sheared from annealed
relate these characteristics to significant sheets and machined to dimensions (1).
strength and toughness parameters. At the ends of the spark-discharge
Because tempered martensites provide machined center notch, fatigue cracks
some of the most desirable combinations 0.3 to 0.4 times the specimen width,
of strength and ductility, the two major were introduced.
types of materials within this group All austenitizing treatments were in a
were included in the study: (1) the predesiccated argon atmosphere, but
martensitic-hardening low-allow Type tempering treatments were in air. Aus-
4340, and (2) the secondary-hardening tenitizing, refrigerating at — 320 F, and
type of alloy steels, namely, Type H-ll tempering were always done in rapid
(Crucible 218) and Type 422 stainless. succession, with a minimum of time
In addition, the role of impurities and between steps. The fully heat-treated
inclusions on fracture toughness and specimens were finish machined by
impact toughness was explored. equally wet grinding both sides of the
0.120-in. blanks to 0.067-in. final thick-
MATERIALS AND METHODS ness; the edges were also machined to
A vacuum-induction-remelted (VIR) precise dimensions. Thus freedom from
4340 and an air-melted 4340 electric- possible decarburized layers was en-
furnace heat of similar chemistry were sured. The finish-machined specimens
used to evaluate the role of inclusions were carefully inspected to check toler-
and impurities. Other data, confirming ances and to record dimensions.
the findings in this report, were obtained Specimens of 4340 were austenitized
for a variety of melting techniques using at 1550 F for a ^ hr, oil quenched, and
closely related 4340 chemistries, but refrigerated; they were then tempered 2
these data will be omitted for the sake hr at each tempering temperature. Cru-
of brevity. cible 218 specimens were austenitized at
Commercial-quality Crucible 218 and 1850 F for a \ hr, oil quenched, and re-
Type 422 air-melted heats were used for frigerated; they were then tempered for
comparative studies of embrittlement 2 plus 2 hr at each tempering tempera-
phenomena in these tempered marten- ture. Type 422 specimens were aus-
sitic materials. tenitized at 1900 F for 1 hr, oil quenched,
The materials were hot rolled to and refrigerated; they were tempered
2
The boldface
for 2 hr at each temperature.
Copyright by numbers in parentheses
ASTM Int'l refer
(all rights reserved); Mon Dec 7 13:15:25 EST 2015
to the list of references
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96 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

TABLE 1—CHEMICAL ANALYSIS OF MATERIALS IN WEIGHT PER CENT.

Steel C Mn P S Si Ni Cr V W Mo N O H,
ppm

Air -melted 4340. 0.40 0.72 0.02 0.015 0.24 1.80 0.82 0.29 0.008 0.0024 0.8
VIR 4340 0.37 0.54 0.003 0.011 0.28 1.90 0.85 0.27 0.0008 0.0009 0.3
Crucible 218 0.41 0.36 0.015 0.012 0.99 0.22 5.01 0.48 1.29 0.002 0.0041 0.7
Type 422 0.20 0.74 0.014 0.018 0.24 0.81 12.22 0.23 1.05 1.01 0.017 0.0072 0.4

FIG. 1—Gross Fracture Types in Notched Tension Specimens.

sheet specimens were cold rolled to about in glacial acetic acid electrolyte was
a 0.001-in. thickness, sealed under argon used; while for Crucible 218, a 7.5 per
in vycor tubes, and heat treated as cent chromic acid in glacial acetic acid
desired. A modified Heidenreich tech- electrolyte was used. For electron frac-
nique (3) was used throughout for the tography, a two-stage cellulose-acetate
final Copyright
electrolytic polishing step. For 4340 carbon replica technique, which is de-
by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
and 422 steels, a 9 per
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 97

For extraction replication of 4340, planes intersecting at the center of the


polished specimens were lightly etched sheet thickness. However, because of the
in 5 per cent Picral plus two drops HC1, transverse fatigue cracks at the speci-
rinsed, and dried. Carbon was evaporated men center, failures of the type shown
on the surface, and the surface etched in Fig. l(c) are more commonly en-
through the replica for 50 sec in the countered. The two or three steps be-
same etchant. After rinsing and drying, tween the fatigue crack and the trough-
plastic replicas were applied and me- and-ridge provide the geometrically
chanically stripped from the specimen. needed transition.
For extraction replication of Type 422, (d) Stepped Transverse Fracture and
the polished specimens were triple etched Orthogonal Shear Lips—This type of
in Vilella's reagent with rinse-dry steps failure, shown in Fig. Kd), is intermedi-
after each etching for 4 min. Plastic ate between the trough-and-ridge forma-
replicas were mechanically stripped. tion, Fig. \(c} and the true orthogonal
For extraction replication of Crucible shear lip fracture, Fig. l(e). In the
218, the polished specimens were etched stepped fracture, the transverse fracture
in Vilella's reagent, rinsed, and dried. alternates with shear steps in a series of
Carbon evaporation, a 1-min re-etch in steps, with orthogonal shear lips taper-
Vilella's reagent, rinse-dry, and plastic ing toward the sheet surfaces.
stripping completed the replication. (e) Orthogonal Shear Lips and Flat
Transverse Fracture—When the trans-
STRUCTURAL DETAILS OF FRACTURE verse crack acquires sufficient velocity
The distinction between the macro- to propagate itself in a continuous man-
scopic and the microscopic approach in ner, this type of fracture is encountered
the analysis of fracture behavior becomes as shown in Fig. \(e). The orthogonal
clear through a detailed examination of shear lips taper down (or up in the other
the observations possible at various half of the specimen) to intersect the
magnifications. For example, the gross sheet surface.
fracture appearance of notch-sheet ten- (f) Flat Transverse Fracture—The to-
sile specimens in these materials may be tally brittle fracture shows no macro-
classified as follows: scopic regions of shear failure, as can
(a) Single-Shear or Full-Shear Ductile be seen in Fig. !(/). On a fine-structure
Failure—This type of failure shows a scale, however, these flat fractures may
single shear plane across the sheet thick- be associated with numerous submicro-
ness, the shear plane usually being in- scopic shear deformation markings.
clined about 45 deg to the stress axis, as Beachem and Srawley (5,6) described
shown in Fig. l(a). fractures of types (a), (b), (c), and (e)
(b) Parallel Shear Lips and Trans- in a high-strength sheet material, AMS
verse Fracture—This type of failure is a 6434 steel; and of course flat-transverse
combination of the single shear and fractures, type (/), are commonly re-
transverse fracture shown in Fig. 1(6). ported. However, the stepped transverse
As the ductility decreases, the parallel fracture, type (d), was discovered as a
shear becomes narrower until a flat fracture form intermediate between the
transverse fracture occupies the entire idealized trough-and-ridge fracture, type
specimen width, as shown in Fig. !(/). (c), and the orthogonal shear lip fracture,
(c) Double Shear or Trough-and-Ridge type (e). In other words, if the material
Failure—Ideally, this type of failure is ductile enough to periodically arrest
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
would consist of two inclined shear propagation of the flat transverse frac-
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98 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

ture and generate multiple shear steps— shear transition temperature assume the
until a new transverse fracture is initi- appearance of either the single-shear lip
ated at the end of the shear step—then fracture, type (a), or the partially
such alternating fracture propagation stepped trough-and-ridge fracture, type
gives rise to the stepped-transverse (c). However, fractures in the transition

FIG. 2—Electron Fractographs from Slow Crack (a) and Fast Crack Propagation Regions (b).

(a) Specimen thinning before cracking.


(6) Discontinuous cracking.
Crack impeded and discontinuous-crack nucleation ahead of main crack. Tensile axis: «->.
FIG. 3—Crack Propagation During Tensile Elongation of Type 301 Stainless by Transmission
Electron Microscopy.

fracture. Almost any trough-and-ridge region usually exhibit the forms of types
type of fracture in these notched sheet (b), (d), or (<?). Below the nil-ductility
tension specimens
Copyright exhibits
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Int'l (all leastreserved);
a level, Moncompletely
Dec 7 13:15:25brittleESTfractures
2015 are
few steps, as shown in
Downloaded/printed byFig. l(c). characterized by a flat-trans verse appear-
Thus ductileoffractures
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 99

characterized above, may not be uniquely slowly propagating crack region and a
evident in a single specimen; in fact, fast-crack area. In both regions, essen-
even two sides of a single fracture speci- tially similar types of fracture processes
men may have different gross fractures. are seen to be occurring, despite the
In addition, edge effects, such as the significant difference in propagation
edge-shearing which forms an edge lip, rates.
Fig. !(</), are often seen when the frac- Also, a study of crack propagation in
ture path deviates substantially from the prethinned specimens, observed during
transverse direction. These can often straining by direct transmission in the
obscure percentage-shear measurements electron microscope, dramatically es-
for Ke3
cS determination; such effects must tablishes the discontinuous nature of
be guarded against in interpreting results crack propagation.
of notch tests. Figure 3 shows the propagation of a

FIG. 4—Slip Traces Due to Dislocation Motion Ahead of Crack Front in Type 301 Stainless.

However, when the detailed topo- crack in a foil specimen of Type 301
graphical contours of the numerous stainless which was subjected to uniaxial
fracture facets within these macroscopic tension while under observation by direct
fracture types are analyzed at high transmission electron microscopy. The
magnification through electron fractog- main crack was stopped at a grain
raphy, the progress of fracture is readily boundary, but the stress field ahead of it
seen to be a stop-and-go process instead was sufficient to discontinuously nucleate
of a continuous homogeneous propaga- a second crack in the adjacent grain.
tion. The process consists of numerous This process of new crack initiation
individual steps of crack initiation, through deformation is clearly evident
growth, and interactions which cumula- in the thinning of the specimen before
tively form the macroscopically observed actual crack formation, as shown in
crack front propagating within the Fig. 3(a). Figure 3(6) shows the crack,
material. still
Copyright by ASTM Int'l (all rights reserved); Mon Decdiscontinuous with respect to the
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Figures 2 (a) and (&)
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tailed fracture
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(University a produce
of Washington) crack
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100 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

FIG. 5—Mechanical Properties of Air Melted and VIR 4340.

Figure 4 clearly shows that there is a merger with one another to form the
plastic deformation zone ahead of a broad crack front that is macroscopically
crack, that is, crack propagation is not described by the methods of fracture
completely brittle. When both slip mechanics.
traces are compared, the fact that the
slip traces are formed in advance of the EFFECT OF INCLUSIONS AND IMPURITIES
crack, and not subsequent to it, is clearly ON TOUGHNESS
established. To evaluate the effect of inclusions and
Thus, despite the seeming macroscopic impurities on fracture properties, Type
continuity of unstable crack propagation 4340 steels of similar compositions were
in these materials, the actual process of prepared by air-melting and vacuum-
propagation involves an avalanche of induction-remelting techniques. Speci-
individual
Copyright crack
by ASTMinitiations
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EST 2015
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 101

heat treated and tested for strength and a distinct maximum in toughness at
fracture-toughness properties. around 400 F, followed by a definite
Figure 5 shows the smooth and notch- minimum near 600 F, shown in Fig. 5.
tensile properties of the air-melted and Also the large scatter in data points
VIR 4340 heats as a function of temper- characteristic of the air melt is signifi-
ing temperature. In each case, the yield cantly absent in the VIR material.
strength increases slightly upon temper- Charpy V-notch impact data from
ing 2 hr in the 300 to 400-F region. At both heats confirmed the 400-F maxi-
higher tempering temperatures, both mum followed by a 600-F minimum in

FIG. 6—Charpy Impact Properties of Air Melted and VIR 4340.

tensile and yield strength decline linearly toughness, as shown in Fig. 6. In these
as a function of tempering temperature. tests, a sufficient number of experiments
Despite this similarity in the smooth- were again included at each tempering
tensile properties of air-melted and VIR temperature to establish the true in-
4340, the fracture properties showed flection in this curve. Also the fracture
marked differences. For example, the appearance in both the air-melt and VIR
air-melted 4340 shows a gradual rise in Charpy specimens clearly reveals an
fracture toughness, with considerable embrittled coarse appearance near the
scatter in data, when tempered at tem- toughness minimum region. The sig-
peratures from 400 to 600 F, shown in nificantly higher energy level of the
Fig. 5. The curve in the air-melt data in VIR Charpy results, compared with
Fig. 5 represents least-squares averaging those from the air-melt 4340, should also
of data for each tempering temperature. be noted. A similar difference in the
On the other by
Copyright hand,
ASTMthe Int'l
VIR (all
heatrights
shows fracture
reserved); Mon toughness
Dec level between
7 13:15:25 EST 2015 the
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102 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

two heats at any tempering temperature the inflections in energy values in both
is evident from Fig. 5. steels.
These facts are observed despite a Thus the high sensitivity of the fa-
significantly smaller austenite-grain size tigue-cracked, plane-stress, notch-tension
in the air-melt 4340 (ASTM intercept test to rapid crack propagation in the
15.8) compared with that of the VIR presence of inclusions tends to mask the
4340 (7.2). toughness changes in the 400 to 600-F
Figure 7, which shows the as-polished region. Possibly this is because, at these
unetched microstructures of the two weak points of the impurity-matrix
heats, demonstrates the relatively larger interfaces, a through-thickness fatigue
inclusion content of the air-melt heat as crack tends to go into rapid propagation
compared with that of the VIR heat. at lower critical stress elevations than
The higher inclusion and impurity con- that for sound material, when local plas-

FIG. 7—Nonmetallic Inclusions in Air Melted and VIR 4340 (X100). Reduced 45 per cent for
reproduction.

tent of the air-melt 4340 contributes to tic deformation is severely limited by an


the scatter in the fracture toughness embrittling mechanism, as demonstrated
data, as determined on fatigue-cracked later in this discussion. In the Charpy
notch-tensile tests, in this embrittling impact test, the energy absorbed repre-
tempering region. Under embrittled con- sents the integrated total energy for all
ditions, crack initiation at inclusion or the crack initiation and propagation
impurity-matrix interfaces may be ex- steps. Thus, while the energy level of
pected to produce this scatter in prop- the air-melted steel is lower than that
erties. However, in the absence of these- for the VIR material, the embrittling
inclusions and consequent scatter in effects can be delineated in both cases.
fracture-toughness data, as in the VIR All of these changes in the fracture
heat, the toughness of 4340 reaches a properties occur during a continuously
maximum at 400 F and exhibits a sub- decreasing yield strength trend in the
sequent minimum near 600 F. Further- 400 to 600-F tempering region and are,
more, Charpy impact data, under the therefore, clearly unrelated to the yield
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
influence of rapid strain rates, exhibit phenomenon.
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 103

EMBRITTLING BEHAVIOR martensite embrittlement range and


UPON TEMPERING permitted use of higher tempering tem-
High-strength steels are known to peratures. In fact, the prevailing fear of
exhibit embrittled behavior after tern- tempered-martensite embrittlement has
pering at two distinct temperature levels, prevented use of the 400 to 700-F tem-

FIG. 8—Mechanical Properties of VIR 4340 and Crucible 218.

Thus tempered martensite embrittle- pering region, even for high-alloy steels
ment (7) develops at the 400 to 700-F such as Crucible 218 or 422. Further-
tempering region, while temper brittle- more, these steels are generally tem-
ness (7) develops in the 900 to 1000-F pered at much higher temperatures, in
region. Beginning with HY-Tuf (8,9), order to take advantage of the secondary-
various silicon modifications of low-alloy hardening reaction. A recent review (10)
high-strength steels have been introduced of heat treatment of high-strength steels
Copyright
because by ASTM
silicon Int'l (all
raised therights reserved); Mon
tempered evenDec 7 13:15:25 EST
recommends the 2015
1000-F secondary-
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104 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

422 are illustrated in Figs. 8 and 9 in


terms of their smooth and notch-tensile
properties. While VIR 4340 shows a
typical tempered-martensite embrittle-
jient in the 400 to 700-F region, the
higher-alloy steels actually exhibit their
maximum toughness in this very tem-
pering range. However, both Crucible
218 and 422 exhibit temper brittleness
at the 900 to 1000-F region.
Thus for many high-strength applica-
tions of Type 422 stainless and of Type
H-ll hot-work steels at temperatures
from the ambient to the tempering
temperature, these steels may be heat
treated at substantially lower tempera-
tures of 500 to 600-F for optimally com-
bining high strength and ductility. In
this manner, a fourfold increase of frac-
ture toughness in Type 422 and a sub-
stantial increase of fracture toughness
in Crucible 218 may be achieved, with-
out a corresponding decrease in yield
strength. A limitation may apply to
those applications involving heavy sec-
tions and complicated shapes, where
excessive retained austenite or residual
stress patterns may be a problem; in the
present study, the quenched specimens
contained less than 3 per cent retained
austenite.
The two regions of embrittlement in
high-strength steels resulting from tem-
pering are thus quite distinct: the low-
alloy steels, such as 4340, exhibit tem-
pered-martensite embrittlement at 400
to 700 F, while the high-alloy steels,
such as H-ll and 422, exhibit temper
FIG. 9—Mechanical Properties of Type 422. embrittlement in the 900 to 1000-F
tempering region.
hardening temper for both of these Furthermore, the toughness inflection
steels in air-frame applications. with a tempered-martensite embrittle-
A careful investigation (11,12) of sev- ment minimum in VIR 4340 is found to
eral high-strength steels revealed the occur during a continuous decline in
fallibility of these prevailing concepts. yield strength. In Crucible 218, the
The effects of tempered-martensite em- toughness maximum and temper brittle-
brittlement
CopyrightinbyVIR 4340
ASTM Int'land
(all of temper
rights ness
reserved); minimum
Mon Dec 7 are bothEST
13:15:25 found,
2015while the
embrittlement in Crucible
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 105

FIG. 10—Types and Relative Amounts of Carbides from 4340, Crucible 218, and Type 422 Steels

(a) 4340 as quenched. (e) Crucible 218 as quenched. (f) Type 422 as quenched.
(b) 4340 300 F tempered. (/) Crucible 218 300 F tempered. (j) Type 422 300 F tempered.
(c) 4340 400 F tempered. (fir) Crucible 218 400 F tempered. (k) Type 422 400 F tempered.
(d) 4340 600 F tempered. (K) Crucible 218 600 F tempered. (1) Type 422 600 F tempered.
FIG. 11—Extraction
Copyright Replica
by ASTM Int'l Micrographs
(all rights of Dec
reserved); Mon (top), Crucible
43407 13:15:25 EST 2015218 (center), and Type 422
(bottom).
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106 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

temperature. In Type 422 the toughness tempering of the three steels at a variety
maximum and minimum are signifi- of temperatures. The carbide types were
cantly out of phase with respect to identified by electron diffraction of ex-
changes in the yield strength. Thus the traction replicas and by X ray diffraction
fracture toughness seems to be more and microprobe analyses of anodically
sensitive than the yield or flow stress to extracted residues. Undissolved residual
fine-structural changes. carbides, though present in all three

(a) 4340 700 F tempered. (e) Crucible 218 700 F tempered. (i) Type 422 700 F tempered
(b) 4340 900 F tempered. (/) Crucible 218 900 F tempered. (j) Type 422 900 F tempered
(c) 4340 1000 F tempered. (g) Crucible 218 1000 F tempered. (k) Type 422 1000 F tempered
(d) 4340 1100 F tempered. (h) Crucible 218 1100 F tempered. (1) Type 422 1100 F tempered.
FIG. 12—Extraction Replica Micrographs of 4340 (fop), Crucible 218 (center), and Type 422
(bottom).

STRUCTURAL FACTORS steels, are not indicated in these dia-


In order to understand the underlying grams. Type 4340, austenitized at 1550 F
embrittling mechanisms, a careful study and quenched, and Type 422, austeni-
of the fine structures of these steels was tized at 1900 F and quenched, contained
undertaken. All heat treatments followed M23C6 carbide as residual particles, while
the schedules outlined for the mechanical Crucible 218, austenitized at 1850 F and
test specimens. quenched, contained MC and M7C3 as
residuals.
Carbide Analysis:
the types and rela- Extraction Replication:
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
Figure 10 shows by
Downloaded/printed
tiveUniversity
amountsof Washington
of carbides(University
formed ofduring
Washington)Extraction replica
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 107

established the morphology and disper- filmy carbide morphology persisted up


sion of the various carbides found at to 900 F (contrast with 4340 in Figs. 11
different tempering temperatures in all and 12).
three steels, as shown in Figs. 11 and 12. The M3C carbide in Crucible 218
The oil-quenched 4340 steel was found begins to redissolve at 900 F, Fig. 12(0,
to contain a filmy precipitate which was and is replaced by alloy-carbide precipi-
positively identified by electron diffrac- tation, MjC and M 7 C 3 , in a finely dis-
tion as epsilon carbide (13). This is the persed form. At 1000 F, the background
first definite diffraction evidence of of the extraction replica represents a
epsilon carbide formed as a result of cloudy mass of finely dispersed alloy-
autotempering during quenching of this carbide particles, while the plates of
steel. Upon tempering at up to 300 F, M3C, which are diminished in size by
epsilon-carbide precipitation progres- re-solution, may still be seen to persist
sively continued, as shown in Fig. 11(6). with ragged edges, as shown in Fig. 12(g).
But at 400 F and above, M3C precipita- Alloy-carbide precipitation and agglom-
tion occurred in increasing amounts, eration continue, adding M23C6 and
Fig. ll(c); individual M3C plates reached M6C precipitation near 1100 F.
0.15-ju length. At the same time, the In contrast to the 0.4 per cent carbon
epsilon carbide gradually disappeared; steels, Type 422 stainless does not pre-
at 600 F only a trace of epsilon carbide cipitate epsilon carbide as a prelude to
was detected as shown, in Figs. 10 and M3C precipitation, as shown in Fig. 10.
11(J). The stable carbide in this steel, The quenched specimen showed no car-
M3C, persisted at all higher tempering bide structure, and none was seen after
temperatures; gross agglomeration of the tempering up to 300 F (Figs. \\(i} and
M3C carbide was observed at 900 F and 0'))- Upon tempering at 400 F, M3C car-
above, as shown in Fig. 12(6) to (d). bide was precipitated in a filmy mor-
In Crucible 218, although some filmy phology (Fig. !!(&)); but at higher tem-
precipitate was found in the extraction pering temperatures, the usual platy
replica from the quenched specimen, no M3C morphology prevailed (Fig. 1!(/)).
epsilon carbide could be identified until At 900 F, the M3C diffraction inten-
after tempering at 400 F, when both sity, Fig. 10, begins to weaken, and a
the filmy epsilon carbide and M3C car- new finely dispersed alloy-carbide pre-
bide platelets were identified by elec- cipitate, M2 3 Ce, was first seen in the
tron diffraction. Also, the epsilon carbide extraction replica (Fig. 12(y)). At 1000 F
persisted at higher temperatures in rela- and above, the M3C was gradually re-
tively larger amounts than those ob- placed by the M23C6 carbide structure.
served in 4340, as shown in Figs. 10, 11, This detailed study of carbide pre-
and 12. In Fig. 12(e), M3C precipitate cipitation in the three steels suggests
platelets have envelopes of filmy precipi- that the re-solution of one carbide, and
tates, which may represent epsilon- its simultaneous replacement by another,
carbide films wrapped around the M3C is associated with an observed embrittle-
plates during the extraction step. Al- ment in terms of fracture properties.
though this apparent folding of filmy Thus in 4340 where the epsilon car-
precipitate is frequently observed, it is bide redissolves and is simultaneously
not possible to distinguish a true folded replaced by M3C carbide at 400 to 600 F,
morphology from a folding produced a pronounced tempered-martensite em-
during replication.
Copyright by ASTM Although
Int'l (all rights epsilon brittlement
reserved); Mon ensues.
Dec 7 13:15:25 EST 2015
carbide was identified by
Downloaded/printed by electron diffrac- In Crucible 218, the epsilon carbide is
tion University
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Washington) in totheLicense
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108 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

region—probably through the effect of usual platy manner. No embrittlement


silicon on carbon activity—and does not is encountered in the 400 to 700-F region.
redissolve until after the M3C precipita- But again, during re-solution of the
tion is nearly complete. No tempered- M3C and simultaneous precipitation of
martensite embrittlement is observed in M23C6 alloy carbide at 900 to 1000 F,
this region. However, at 800 F and above, temper brittleness is encountered.

(a) 4340 as quenched. («) Crucible 218 as quenched. (i) Type 422 as quenched.
(b) 4340 300 F tempered. (/) Crucible 218 300 F tempered. (j) Type 422 300 F tempered.
(c) 4340 400 F tempered. (g) Crucible 218 400 F tempered. (fc) Type 422 400 F tempered.
(d) 4340 600 F tempered. (h) Crucible 218 600 F tempered. (1) Type 422 600 F tempered.
FIG. 13—Transmission Micrographs of 4340 (top), Crucible 218 (center), and Type 422 (bottom).

when the M3C begins to redissolve and Transmission Electron Microscopy:


is simultaneously accompanied by pre- Thin sections of the three martensitic
cipitation of finely dispersed alloy car- steels were studied in detail by direct
bides, M2C and M 7 C 3 , temper embrittle- transmission electron microscopy to es-
ment ensues. tablish the nature of structural changes
And in Type 422, no epsilon carbide and dislocation distributions associated
precedes the M3C precipitation. At 400 F with these tempering reactions.
andCopyright
above, Mby3C carbide
ASTM Int'l forms, first,
(all rights in
reserved);
In 4340 steel, the quenched structure
Mon Dec 7 13:15:25 EST 2015
a filmy dispersion, and
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 109
tremely high dislocation densities and martensite probably adds to further
some microtwins, as shown in Fig. 13(a). limit slip paths, as shown in the Fig. 13 (c)
Upon tempering to 300 F, very little insert. This process continues, and at
dislocation rearrangement is evident, 600 F, finely dispersed precipitation on
although a tendency toward greater dislocation networks and at nodes of
microtwin decoration through precipita- intersecting dislocations becomes fre-
tion of filmy epsilon carbide along quently apparent, as shown in Fig. 13 (d)

(a) 4340 700 F tempered. (e) Crucible 218 700 F tempered. (i) Type 422 700 F tempered.
(6) 4340 900 F tempered. (/) Crucible 218 900 F tempered. (j)Type 422 900 F tempered-
(c) 4340 1000 F tempered. (g) Crucible 218 1000 F tempered. (fc) Type 422 1000 F tempered-
(d) 4340 1100 F tempered. (h) Crucible 218 1100 F tempered. (1) Type 422 1100 F tempered.
FIG. 14—Transmission Micrographs of 4340 (top), Crucible 218 (center), and Type 422 (bottom).

microtwin interfaces is suggested, as and insert. Similar effects are observed


shown in Fig. 13(6). at 700 F, as shown in Fig. 14(a). At this
At 400-F tempering, when epsilon tempering temperature, however, re-
carbide re-solution begins with attend- covery, carbide growth, and agglomera-
ant precipitation of M3C, even greater tion have reduced some of the internal
dislocation densities, Fig. 13(c), render strains, resulting in somewhat decreased
the structure within martensite laths dislocation density. The first evidence
almost unresolvable. A few of the platy of spheroidal carbide precipitate is also
M3C carbide precipitates are also seen. seen at this point.
In some regions,
Copyright a high
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no STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

the martensite lath structure, as shown tempered structure shown in the Fig.
in Fig. 14(6). But the platy M3C car- 13 (j) insert.
bides were still visible in the structure At 400 F, M3C carbide precipitation
in a Widmanstatten distribution. At becomes perceptibly superimposed on a
higher tempering temperatures, multiple somewhat recovered dislocation struc-
reactions of matrix recrystallization and ture, shown in the Fig. 13(&) insert.
precipitate agglomeration and growth, Growth of platy M3C precipitates con-
Figs. 14(c) and (d), produced a decline tinues up to 600 F, as shown in Fig. 13(/).
in strength properties with rapidly rising But beginning at 700 F, a finely dis-
ductility. persed precipitation which becomes more
In Crucible 218, the quenched struc- pronounced at 900 F can be seen at dis-
ture, Fig. 13(e), showed extremely high location intersections, shown in Fig.
dislocation density. Upon tempering to 14(t) and (j). A preponderance of such
300 F, some dislocation rearrangement— dislocations is evident in the insert of
producing networks—is seen, as in the Fig. 14(y). These precipitate-stabilized
Fig. 13 (f) insert. However, no further networks are a dominant characteristic
precipitation is observed. At 400-F tem- at 1000 F, as shown in Fig. 14(£).
pering, some further precipitation be- At HOOF, the climb-induced cell
comes apparent, Fig. 13(g), but the dis- structure formation, Fig. 14(/), tends to
location rearrangements have progressed initiate replacement of the martensitic
simultaneously to produce some definite structure.
networks. These processes continue up Thus, in each case of embrittlement,
to 600 F, as shown in Fig. 13(h). But at high dislocation densities, characterized
700 F the first precipitation on disloca- by general darkening and extinction
tion nodes is seen, as in the Fig. 14(e) effects in transmission micrographs, are
insert. observed. At high magnifications, pre-
At 900 F, these precipitate-locked dis- cipitation upon dislocation intersections
location nodes are abundant, as shown and jogs is also frequently evident. In
in the Fig. 14(/) insert. These precipi- these materials, the general dislocation
tate-stabilized networks are still evident concentration is not substantially re-
at 1000 F, Fig. 14(g) and insert, but at duced until these steels are overtem-
this temperature, initial formation of a pered, causing significant loss in tensile
cell-wall substructure becomes distinct. and yield strength.
The apparent improvement in notch-
strength may be related to the yield DISCUSSION
strength decline, which also occurs as a Some well-known high-strength mar-
consequence of the above fragmenting tensitic steels were carefully re-examined
of matrix structure. At 1100 F, substan- to relate their fine-structural character-
tial substructure growth and polygoniza- istics to significant strength and tough-
tion have essentially replaced the mar- ness parameters and to evaluate the
tensite structure, as shown in Fig. 14(/z). roles of thermal treatments, inclusions
In Type 422 stainless, where no epsilon and impurities. Because tempered mar-
carbide precipitates, even the quenched tensites provide some of the most de-
structure shows some dislocation network sirable strength-toughness combinations,
formation, despite the high average the fine-structural aspects of the two
dislocation density shown in Fig. 13(i). major types of materials in this group
Reduced dislocation density and some were included in the study: (1) the
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 111

4340, and (2) the secondary-hardening plane-stress notch-tensile test to rapid


type alloy steels, such as Type H-ll crack propagation at structural discon-
(Crucible 218) and Type 422 stainless. tinuities such as inclusion-matrix inter-
Detailed examination of fractures faces in an embrittled matrix. These
from the gross macroscopic scale to the probably mask the true toughness be-
fine electron microscopic scale showed havior in the 400 to 600-F region.
that the macroscopic features can be The two forms of embrittlement in
broadly subdivided into six major cate- high-strength martensitic steels, namely,
gories in terms of their appearance. But tempered-martensite embrittlement, 500
the detailed submicroscopic features F, of low-alloy martensitic hardening
reveal that the true fracture process is steels such as 4340; and temper brittle-
not a continuous homogeneous propaga- ness, 900 to 1000 F, of high-alloy second-
tion of a single crack front but a ary-hardening steels such as Crucible
discontinuous process consisting of nu- 218 and Type 422, were separately
merous individual steps of crack initia- characterized. It was demonstrated that
tion, growth, and interaction which the secondary hardening region is not
cumulatively produce the macroscop- always the optimum tempering region
ically observed crack front propagating for these alloy steels. Thus for many
within the material. Also the slow crack high-strength applications of Type 422
and fast crack propagations were both stainless, and of Type H-ll hot-work
found to be governed by similar indi- steels at temperatures from the ambient
vidual fracture processes, despite the to the tempering temperature, these
significant difference in propagation steels may be profitably heat treated at
rates. much lower temperatures (500 to 600 F),
Vacuum-induction-melted versus air- in order to optimally combine strength
melted 4340 heats of similar composition and toughness. Indeed a fourfold tough-
were tested to determine their relative ness benefit in 422 and a substantial
strength and toughness response to tem- toughness benefit in Crucible 218 were
pering. The air-melted 4340, which had thus shown.
a higher inclusion-impurity content, In all three steels, fine-structure
showed considerable scatter in fracture studies revealed that both tempered-
toughness when tempered in the tem- martensite embrittlement, 500 F, and
pered-martensite embrittlement region. temper brittleness, 900 to 1000 F, were
But the vacuum-melted material, which associated with a re-solution of one
had a lower inclusion content, showed a carbide precipitate and simultaneous
toughness maximum at 400 F, followed reprecipitation of another. This study
by a toughness decline owing to em- suggests a single mechanistic explana-
brittlement at 600 F. Charpy-impact tion of both tempered martensite em-
data revealed the toughness maximum brittlement, 500 F, and temper brittle-
at 400 F and subsequent tempered- ness in these and, possibly more
martensite embrittlement in both mate- generally, in other alloy systems.
rials. These significant changes occur
during a continuously decreasing yield Embrittling Mechanisms:
strength trend in the 400 to 600-F tem- Certain generalizations about the
pering region and are, therefore, un- mechanism of tempered martensite em-
related to the yield phenomena. These brittlement, 500 F, and about temper
observations are reconciled in terms of brittleness become possible when the de-
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112 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

lated to strength and fracture properties cells of martensite. Thus, when the
of three different high-strength alloy sys- epsilon carbide becomes critically un-
tems such as 4340, Crucible 218, and stable, in the 400 to 600-F tempering re-
Type 422 stainless steels. gion, and it must redissolve in the
In considering embrittlement resulting matrix, only local iron-atom movements
from tempering treatments of high- on the (101), = (101)a, planes would
strength steels, it should be remembered suffice to achieve the parent lattice
that vacancy-induced climb processes structure (19). However, this transformed
leading to rapid reduction in dislocation lattice, with its high carbon supersatura-
density are not observed, even in pure tion would represent volumes of highly
iron, until after tempering at 800 to strained matrix. Furthermore, this struc-
900 F (14), even though vacancies become ture must immediately reject its sub-
mobile in iron at much lower tempera- stantial supersaturation of carbon into
tures, such as at 436 to 572 F (15). In the surrounding matrix. This momentary
high-strength steels, even higher tem- carbon diffusion gradient—at the tem-
peratures would be required to activate pering temperature—may thus be visual-
the vacancy-induced climb process, be- ized in terms of a localized, severe, lat-
cause climb restraint is increased through tice-distortion gradient which must be
solute interaction with dislocation jogs accommodated by the surrounding ma-
(16), and through precipitate nucleation trix. Arrays or networks of dislocations
at dislocations, which ties the dislocations may provide this necessary accommoda-
to the precipitate by strain-field interac- tion. The arrays or networks of disloca-
tions and surface-tension forces (17). tion which are produced must interact
Transmission microscopy of Type 4340, with the already existing dislocation
Crucible 218, and Type 422 steels clearly tangles in the matrix structure, leaving
demonstrates this in terms of persistent irregular arrays or dislocation networks
high dislocation densities up to 900 F in along the outward carbon-diffusion path
4340 and up to above 1000 F in the other which are observed in the structures after
two higher alloy steels. Thus, both the tempering in the carbide dissolution
500-F embrittlement and temper brittle- range.
ness phenomena occur in a tempering Also, because of the carbon supersatu-
region where high dislocation densities ration, the stable M3C tends to precipi-
still persist, despite some dislocation- tate, utilizing dislocation intersections
density reduction through glide-based and jogs as preferred nucleation sites.
recovery processes (18). Cahn's analysis (20) shows that precipita-
Let us first consider the case of tem- tion on dislocations increases with super-
pered-martensite embrittlement in 4340 saturation. These precipitates, which
steel: in a 0.40 weight-per cent carbon would be more closely spaced along a
martensite one finds approximately one dislocation than those elsewhere, would
carbon atom for 30 unit cells of marten- lead to precipitate locking, and thus it
site. But the hexagonal epsilon carbide would be more difficult to initiate yield
phase contains 25 to 30 atomic per cent than to continue it. Of course, some of
carbon. If the close crystallographic the epsilon-carbide precipitate may
correspondence of the epsilon carbide to transform in situ (21) to M3C; however
the martensite lattice along the (101)e the bulk of the transformation seems to
and (lOl)^ planes is considered, this be through re-solution and reprecipita-
leads to an equivalent carbon concentra- tion. The dislocation locking through
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 113

tions and jogs seems to produce tem- point is merely conjecture, work is cur-
pered-martensite embrittlement in 4340. rently under way to check it.
In Crucible 218 the epsilon carbide is Thus we find that in each case of em-
stabilized in the 400 to 700-F region— brittlement, that is, tempered martensite
probably through the effect of silicon on embrittlement, 500 F, in 4340 or temper
carbon-activity—and does not redissolve brittleness in 218 or 422, re-solution of a
until after the M3C precipitation is sub- metastable carbide precipitate with at-
stantially complete. Consequently, no tendant reprecipitation of a more stable
pronounced dislocation locking is gen- carbide produces precipitation at disloca-
erated, and no tempered-martensite tion intersections and jogs, and increased
embrittlement, 500 F, is observed in this dislocation densities. Clearly, then, the
steel. embrittlement in all three cases is asso-
In Type 422 stainless, where no ep- ciated with these generalized reactions.
silon carbide is found, glide-based re- Historically, tempered martensite, 500-F,
covery processes produce dislocation embrittlement in medium-carbon, low-
rearrangements and some dislocation alloy steels has been variously ascribed
networks in the 400 to 600-F tempered- to the occurrence of cementite platelets
martensite embrittlement region, while (23), of thin ferrite networks (24), or of
the M3C plates reach 0.5-/J. length at continuous carbide films (25,26), but none
600 F. These glide-based recovery proc- of these mechanisms seem to explain the
esses are probably due to the tempera- structural observations in 4340. Temper
ture-dependent reduction in resistance to embrittlement in the higher-alloy steels
dislocation movement. And in this has also been associated with a wide
tempering region, fracture toughness of variety of precipitation reactions and
Type 422 indeed reaches a maximum. segregation to grain boundaries (27). But
However, in both the higher alloy none of these satisfactorily account for
steels, Crucible 218 and 422, as the M3C all experimental observations. This new
precipitate becomes unstable in the tem- study of fine structures in three high-
per-brittle range, 800 to 1000 F, it tends strength alloy steels suggests a single
to redissolve in the matrix. Again, rela- mechanistic explanation of both tem-
tively small iron-atom movements can pered martensite embrittlement, 500 F,
generate the required lattice relationships and temper brittleness in these and,
(22), but a 20:1 carbon supersaturation possibly more generally, in other alloy
must be dispersed. At these higher tem- systems.
peratures, 800 to 1000 F, dislocation net- In either case, precipitate-locked dis-
works are even more readily generated. location intersections and jogs, along
Such an effect is clearly observed in the with high dislocation densities, produce
high magnification insert of Fig. 14(j). an increase in flow stress, but an asso-
which may be contrasted with the rela- ciated lowering of notch toughness during
tively weak strain fields around similar re-solution of one precipitate with si-
precipitate particles before their instabil- multaneous reprecipitation of another.
ity and dissolution, as shown in Fig. Thus the embrittlement of these steels
14(f). Even in the case of the classic through thermal treatments, either in the
temper brittleness, developed upon cool- tempered-martensite embrittlement re-
ing from near the critical temperature, gion, 400 to 700 F, or in the temper-
finely dispersed precipitation upon al- brittle region, 900 to 1000 F, may be
readyCopyright
existing dislocation networks may mechanistically viewed, according to
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provide
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114 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

terms of a strong dislocation locking and 3. The role of inclusions and impuri-
a high dislocation density. The strong ties in producing scatter in fracture
dislocation locking effectively increases toughness data in the 500-F embrittling
the dislocation unpinning stress; the high region was demonstrated.
dislocation density permits the crack to 4. The secondary hardening region in
form without plastic work so that the the two alloy steels was shown to be a
effective surface energy is reduced. Both nonoptimal tempering region for the
of these factors favor embrittlement. combination of high strength and tough-
Finally, upon reaching tempering tem- ness. Tempering well below this region
peratures of 900 F and above in 4340, produced a fourfold toughness benefit in
and 1100 F in 218 and 422, several reac- 422 and a substantial benefit in 218,
tions in sequence drastically reduce dis- without loss in yield strength.
location densities, agglomerate carbide 5. Both the tempered-martensite em-
precipitates, and create substructures brittlement, 500 F, and temper brittle-
which eventually replace the entire mar- ness, 900 to 1000 F, were associated with
tensitic structure. Such processes as re-solution of one carbide and simultane-
vacancy-induced dislocation climb, and ous reprecipitation of another.
more rapid diffusion rates become the 6. A single mechanistic model explains
governing factors. However, from the both types of embrittlement: precipitate-
high-strength viewpoint this tempering locked dislocation intersections and jogs
region is of little interest, except to along with high dislocation densities
emphasize the fact that both the 500-F occur during the carbide re-solution and
embrittlement and temper brittleness reprecipitation steps for both types of
phenomena occur at lower temperatures embrittlement. Thus strong dislocation
—in a tempering region where high dis- locking and high dislocation densities
location densities still persist despite some characterize the embrittled structures.
relaxation through glide-based recovery
processes. A cknowledgments:
The author wishes to express grateful
SUMMARY acknowledgment and deep appreciation
to his colleague John J. Hauser, who has
Relating the detailed fine structural been involved in all aspects of an exten-
characteristics to strength and toughness sive research program of which this
properties of both martensitic hardening, paper represents a small part. J. M.
4340, and secondary hardening high- Capenos, G. S. Felbaum, F. S. Snyder,
strength steels, Crucible 218 and 422, and various other Crucible Research
permits the following conclusions and staff members have also materially con-
generalizations: tributed to these studies. Helpful dis-
1. The gross macroscopic fractures in cussions with Professor J. P. Hirth, Ohio
notched sheet tension specimens may be State University, are also acknowledged
subdivided into six major categories. The support of Materials Central, Di-
2. But the submicroscopic fracture de- rectorate of Advanced Systems Tech-
tails show that the true fracture process nology, Aeronautical Systems Division,
consists of numerous separate crack ini- Wright-Patterson Air Force Base,
tiation, coalescence, and propagation through contracts AF33(616)-8156 and
steps, merging to produce the macro- AF33(657)-10337, is also gratefully ac-
scopic fracture front. knowledged.
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BANERJEE ON FRACTURE MICROMECHANICS IN STEELS 115

REFERENCES

(1) B. R. Banerjee and J. J. Hauser, "Research Hauser, "Carbide Precipitation Sequence


and Application Engineering to Determine in AISI 4340 Steel," to be published.
the Effect of Processing Variables on (14) A. S. Keh, "Dislocation Arrangement in
Crack Propagation of High-Strength Steels Alpha Iron during Deformation and Re-
and Titanium," ASD-TDR 62-1034, Part covery," Direct Observation of Imperfec-
I, April, 1963. tions in Crystals, p. 213, Interscience Div.,
(2) "Fracture Testing of High Strength Mate- John Wiley and Sons, Inc., New York,
rials," ASTM Bulletin, Vol.
Vol. 4,
4, 1960,
1960, p.
p. 29;
29; N. Y., 1962.
Vol. 5, 1961, p. 389. (15) F. W. Kunz and A. N. Holden, "The Effect
(3) J. M. Capenos, J. J. Hauser, and B. R. of Short-Time Moderate Flux Neutron
Banerjee, Advances in Electron Metallog- Irradiations on the Mechanical Properties
raphy and Electron-Probe Microanalysis, of Some Metals," Acta Met., Vol. 2, 1954,
ASTM STP 317, Am. Soc. Testing Mats., p. 816.
1962, p. 26. (16) J. Montuelle, "Influence of Traces of
(4) B. R. Banerjee, J. J. Hauser, and J. M. Impurities on Polygonization of Alumi-
Capenos, "Etch-Shadow Extraction Rep- num," Compt. Rendue, Vol. 241, 1955,
lica in Fracture Studies," Review of Scien- p. 1304.
tific Instruments, Vol. 34, 1963, p. 477. (17) A. H. Cottrell, "Creep and Ageing Effects
(5) C. D. Beachem and J. E. Srawley, "Crack in Solid Solutions," Creep and Fracture
Propagation Tests of High Strength Sheet of Metals at High Temperature, Proceed-
Materials," Naval Research Laboratory ings, National Physical Laboratory Sym-
Report 5507, August 18, 1963. posium, Philosophical Library, New York,
(6) C. D. Beachem, "Effect of Test Tempera- 1957, p. 141.
ture upon Topography of Fracture Sur- (18) W. R. Hibbard and C. G. Dunn, "A Study
faces of AMS 6434 Sheet Specimens," of (112) Edge Dislocations in Bent Silicon-
Naval Research Laboratory Memo 1293, Iron Single Crystals," Acta Met., Vol. 4,
March, 1960. 1956, p. 306.
(7) B. R. Queneau, Embrittlement of Metals, (19) K. H. Jack, "Structural Transformation
American Society for Metals, Cleveland, in the Tempering of High-Carbon Mar-
Ohio, 1955. tensitic Steels," Journal Iron and Steel
(8) P. Payson and A. E. Nehrenberg, "New Institute, Vol. 169, 1951, p. 26.
Steel Features High Strength and High (20) J. W. Cahn, "Nucleation on Dislocations,"
Toughness," Iron Age, Vol. 162, Oct. 21, Acta Met., Vol. 5, 1957, p. 169.
1948, p. 64; Vol. 162, Oct. 28, 1948, p. (21) J. J. Hauser, J. M: Capenos, and B. R.
74. Banerjee, "Subihicroscopic Structures in
(9) A. G. Allten and P. Payson, "The Effect Tempering 410 Stainless Steel," Trans-
of Silicon on the Tempering of Marten- actions, American Society for Metals,
site," Transactions, American Society for Vol. 54, 1961, p^514.
Metals, Vol. 45, 1953, p. 498. (22) B. R. Banerjee, R. C. Westgren, J. M.
(10) R. J. Fiorentino, D. B. Roach, and A. M. Capenos, and E. J. Dulis, "Ausworking
Hall, "Heat Treatment of High Strength Type 422 Stainless Steel," Transactions,
Steels for Airframe Applications," DMIC American Society for Metals, Vol. 56,
Report No. 119, Battelle Memorial Insti- 1963, p. 629.
tute, Columbus, Ohio, Nov. 27, 1959. (23) C. S. Roberts, B. L. Averbach and M.
(11) B. R. Banerjee and J. J. Hauser, "A New Cohen, "The Mechanism and Kinetics of
Heat Treatment for High-Alloy High- the First Stage of Tempering," Transac-
Strength Martensitic Steels," First Quar- tions, American Society for Metals, Vol.
terly Report, ASD Contract No. AF33(657)- 45, 1953, p. 576.
10337, April 30, 1963. (24) L. J. Klinger, W. J. Barnett, R. P. From-
(12) B. R. Banerjee, J. J. Hauser, and J. M. berg and A. R. Troiano, "The Embrittle-
Capenos, "Fine Structure and Properties ment of Alloy Steel at High Strength
of a 12-Cr MoWV Martensitic Stainless Levels," Transactions, American Society
Steel," to be published. for Metals, Vol. 46, 1954, p. 1557.
(13) B. R. Banerjee, J. M. Capenos, and J. J. (25) B. S. Lement, Discussion to "The Effect
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
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116 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

of Silicon on the Tempering of Marten- (27) M. Szczepanski, The Brittleness of Steel,


site," Transactions, American Society for John Wiley and Sons, Inc., New York,
Metals, Vol. 45, 1953, p. 526. N. Y., 1963.
(26) B. S. Lement, B. L. Averbach and M. (28) A. H. Cottrell, "Theory of Brittle Fracture
Cohen, "Microstructural Changes on in Steel and Similar Metals," Transactions,
Tempering Iron-Carbon Alloys," Trans- American Institute of Mining, Metallur-
actions, American Society for Metals, Vol. gical, and Petroleum Engineers., Vol. 212,
46, 1954, p. 851. 1958, p. 192.

DISCUSSION
1
J. H. BucHER —With respect to the The work of J. M. Capus2 on the im-
attributing of tempered martensite em- pact testing of ultrahigh-purity and se-
brittlement—sometimes referred to as lectively contaminated steels has shown
500-F embrittlement and 350-C embrit- the significant, if not all-important, role

Quasi-cleavage and large dimpled rupture can be seen.


FIG. 15—AISI 4340, Austenized 1 hr at 1550 F, Quenched in Oil, and Tempered 2 hr at 400 F,
Broken at Room Temperature (X6500).

tlement—to some microstructural char- of certain elements, such as phosphorus,


acteristic, that is, precipitate-dislocation arsenic, stibium, and stannum in very
interaction, certain observations would 2
J. M. Capus, "The Influence of Trace
seem in order. Elements on the Impact Resistance of Quenched
and Tempered Low
1 Copyright by ASTM Int'l (all rights reserved); Mon Dec
Alloy EST
7 13:15:25 2015Revue de
Steels,"
Graduate student, Ohio
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DISCUSSION ON FRACTURE MICROMECHANICS IN STEELS 117

small amounts, and also other alloying known effect on the course of tempering.
elements, such as manganese, in larger Also, by micro-fractographic analysis it
amounts. Capus observed that tempered was observed that fracture along prior
martensite embrittlement did not occur austenitic grain boundaries may occur in
in these ultrahigh-purity steels, but could the embrittlement range when the indi-
be induced by selective doping of the cated impurities are present, but not if
steels with the indicated impurities. they are absent.

Intergranular fracture can be seen.


FIG. 16—AISI 4340, Austenized 1 hr at 1550 F, Quenched in Oil, and Tempered 2 hr at 450 F,
Broken at Room Temperature (X6500).

Furthermore, as yet unpublished work Currently, research is being conducted


by Capus3 and his former associates at at Ohio State University under USAF
the Birmingham Laboratory of the In- Contract No. AF 33(616)-7780 on the
ternational Nickel Co., Ltd., shows no relationship of microstructure to crack
significant difference in the structures of propagation in ultrahigh-strength steel.
the tempered high-purity and intention- As part of this investigation, the
ally doped steels, except in the case of change in fracture propagation charac-
silicon, where the element had a well- teristics of A1S1 4340 with tempering
Copyright by ASTM Int'l (all rights reserved);temperature
Mon Dec 7 in the impact
13:15:25 test at room
EST 2015
3
J.Downloaded/printed
M. Capus, private communication.
by temperature and liquid N2 temperature
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118 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

was studied by electron fractography. 2 hr essentially no intergranular fracture


Charpy V notch bars were prepared from was observed, and Fig. 15 typifies the
aircraft quality steel bars furnished by fractures at room temperature. For speci-
Republic Steel Corp.; the specimens were mens tempered at 450 F for 2 hr a de-
heat treated and broken. The fracture crease in toughness was observed and
surfaces were then replicated by a direct intergranular fracture was in evidence,
carbon replication technique and studied as shown in Fig. 16. Figure 17 deals with
both in the electron microscope and by a specimen tempered 2 hr at 550 F and
stereographic analysis of pairs of electron broken at liquid N2 temperature, and

Intergranular fracture can be seen.


FIG. 17—AISI 4340, Austenized 1 hr at 1550 F, Quenched in Oil, and Tempered 2 hr at 550 F,
Broken at 78 K (X6500).

micrographs. The tempered martensite intergranular fracture is seen again.


embrittlement was manifest both in the Figure 18 shows the finely dimpled frac-
specimens broken at room temperature ture surface characteristic of the speci-
and liquid N2 temperature. The fracture mens tempered 2 hr at 800 F, that is,
surfaces in the middle of the embrittle- just above the embrittlement range.
ment range were found to contain ap- Some small amount of intergranular
proximately 50 per cent intergranular fracture, about 10 to 15 per cent, was
fracture in prior austenitic grain bound- still observed after this treatment and
aries with lesser amounts at the ex- perhaps indicates that the intergranular
tremes. weakness
Copyright by ASTM Int'l (all rights reserved); Mon still persists
Dec 7 13:15:25 EST 2015to a much lesser
For specimens tempered
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DISCUSSION ON FRACTURE MICROMECHANICS IN STEELS 119
In summary, any explanation of tem- role of trace impurities on tempered-
pered martensite embrittlement would martensite embrittlement must still be
seem to have to include a consideration considered an open question, when one
of these two observations. First, the em- compares conflicting recent data extant
brittlement can be eliminated in ultra- in the literature.
high-purity steels and induced by trace Capus,2 for example, found that by
amounts of certain impurities. Second, reducing4 sulfur to 0.003 per cent, and
the fracture is observed to be intergranu- phosphorus to 0.001 per cent,5 in an

Small dimpled fracture and larger inclusion nucleated dimples are seen.
FIG. 18—AISI 4340, Austenized 1 hr at 1550 F, Quenched in Oil, and Tempered 2 hr at 800 F,
Broken at Room Temperature (X6500).

lar in the embrittlement range both in otherwise 4340-type steel composition,


the doped high-purity steels and in com- he was able to remove the dip in the
mercial AISI 4340. Charpy impact curve as a function of
B. R. BANERJEE (author's closure)—I tempering temperature, while this dip
would like to thank Mr. Bucher for his was clearly evident in his No. 6 steel of
thoughtful comments and discussion.
4
While impurities could well add to the Other trace impurities and gas analysis
dislocation locking process, which we were not specified.
5
A second reference to the same No. 2 steel
have discussed, and therefore constitute gives phosphorus content as 0.006 per cent.
an additional parameter that may deter- See J. M. Capus and G. Mayer, "Impact Prop-
mineCopyright
the occurrence
by ASTM Int'land
(all rights of erties
extentreserved); of High-purity Nickel-Chromium-Molyb-
Mon Dec
denum JournalEST
7 13:15:25
Steels," of the
2015Iron and Steel
tempered martensite by
Downloaded/printed embrittlement, the nstitute, Vol. 189, 1958, p. 255.
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120 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

commercial quality, containing 0.022 martensite embrittlement region are very


per cent sulfur and 0.026 per cent phos- interesting. However, despite a con-
phorus. However, Cottrell6 and his co- sciencious effort, involving visual exam-
workers have recently found that a high- ination of electron fractographs and
purity 1 Cr-Mo steel, with 0.44 per cent electron surface replicas of nickel-plated
carbon—containing as little as 0.001 per fracture edge contours, we were unable
cent sulfur, 0.002 per cent phosphorus, to establish a statistically significant cor-
0.0002 per cent oxygen, 0.00004 per cent relation of intergranular failure with
hydrogen, and 0.0017 per cent nitrogen— tempering in the tempered-martensite
still revealed the tempered-martensite embrittlement region. Our observations
embrittling effect near 500 F. would qualitatively suggest that some
Mr. Bucher's observations and elec- intergranular failure is found from the
tron fractographs suggesting preferential as-quenched to tempering anywhere up
intergranular failure in the tempered to 800 to 850 F; and a further complicat-
6
C. L. M. Cottrell, P. F. Langstone, and ing factor lies in the diversity of sub-
J. H. Kendall, "Improved Properties of Extra microscopic fracture paths invariably
High-Purity Steel in Tensile Strengths up to found within different regions of any
150 tons/in.2," Journal of the Iron and Steel
Institute, Vol. 201, 1963, pp. 1032-1037. single broken specimen.

Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
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THE EFFECT OF SOLIDIFICATION PRACTICE ON THE
PROPERTIES OF HIGH-STRENGTH STEELS
BY C. M. CARMAN,1 R. W. STRACHAN,2 D. F. ARMIENTO,1 AND H. MARKUS3

SYNOPSIS
The effect of unidirectional solidification on the mechanical properties of
high-strength steels was investigated by means of split heats of AISI 4340 and
25 per cent nickel maraging steel. One half of these heats were unidirectionally
solidified and the other half of these melts were allowed to solidify to produce an
equiaxed structure. These ingots were forged and rolled to a light gage sheet
0.040 to 0.060 in. thick.
The materials were evaluated by means of standard tension tests and frac-
ture toughness studies. By means of compliance measurements, it is possible to
determine the crack resistance as a function of absolute crack extension. This
investigative technique was used to study the AISI 4340 steel. Unidirectional
solidification did not alter the crack resistance properties of this steel. However,
a 10 per cent improvement in plane-strain fracture toughness as determined by
the pop-in technique was observed for the unidirectionally solidified material.
In order to obtain very high strength levels, the total content of hardener ele-
ments was increased in the 25 per cent nickel maraging steels. Consequently
these materials were quite brittle and the results not definitive. However, it was
demonstrated that a homogeneous structure is necessary for high values of
fracture toughness in this material.
The data were interpreted in terms of critical crack size for instability at
yield stress. Both through-cracks and part-through-cracks were considered in
this analysis.

The requirements and development investigation of these failures showed


of high-performance solid-propellant that the stress and defect size can be re-
rocket motors and other high strength to lated to the fracture toughness of the
density aerospace applications have materials through the disciplines of
directed attention toward the utilization fracture mechanics as developed by
of ultrahigh-strength steels. Early at- Irwin (I).4
tempts to fabricate large booster cases The first solutions to this problem con-
from these steels resulted in many low sisted of improving the non-destructive
stress failures upon hydrotest. Intensive inspection procedures and studying
1
methods of upgrading the fracture tough-
Metallurgist, Pitman-Dunn Institute for ness of the materials. The result of these
Research, Frankford Arsenal, Philadelphia, Pa.
2
Research staff, Massachusetts Institute of latter studies has been the adoption of
Technology,
3
Cambridge, Mass. consumable electrode vacuum-melted
Director, Metallurgy Research Laboratory, 4
Pitman-Dunn Institute for Research, Frank- The boldface numbers in parentheses refer
ford Arsenal, Philadelphia, Pa. to the list of references appended to this paper.
121
122 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

steels for the majority of the solid-pro- The effects of vacuum melting of
pellant rocket motor cases produced quality steels are generally well known.
today. Vacuum induction melting is expected
The specific effects of ingot solidifica- to promote a cleaner and perhaps more
tion variables are not well known. Re- ductile material owing to the following:
search conducted at Massachusetts (1) use of slags is eliminated; (2) deoxida-
Institute of Technology has shown that tion and degassing is caused by vac-
solidification structure has a significant uum—the use of oxide - forming melt
effect upon the properties of castings additions is not necessary for this pur-
(2-5), and it is expected that this struc- pose; (3) as a result of (1) and (2),
tural effect will also influence the proper-
ties of wrought materials.

FIG. 1—Mold for Unidirectionally Solidified FIG. 2—Macrostructure of Unidirectional 9-


9-in.-High Cylinder. in. Ingot.

The purpose of this work is to examine inclusions should be fewer and smaller;
the effects of several melting and casting and (4) total gas content is lowered.
variables upon the wrought properties of Solidification structure, that is, grain
two selected high-strength steels, AISI structure and orientation, have been the
4340 and a 25 per cent nickel maraging object of studies conducted at Massa-
steel composition. These variables in- chusetts Institute of Technology in
clude (1) air versus vacuum melting, (2) recent years. Oriented or columnar grain
columnar-grained ingot structure versus structures produced by unidirectional
equiaxed ingot structure, and (3) longi- solidification have produced improved
tudinal versus transverse rolling of the mechanical properties in castings. Duc-
ingots. Of ultimate concern are the tility especially is increased from 50 to
effects of segregation, microporosity, and 200 perMon
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inclusions upon properties
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strength wrought
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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 123

properties of columnar-structured mate- It can be seen that under these condi-


rial is not caused by the structure per se. tions solidification will occur from the
Rather, the factors which tend to pro- bottom to the top of the ingot. A typical
duce columnar growth, that is, steep macrostructure of an ingot which was
thermal gradients principally, also act unidirectionally solidified is shown in
to do the following in solidifying ingots: Fig. 2. It will be seen that the unidirec-
(1) improve feeding by reducing mushy tional growth of long columnar grains was

TABLE 1—CHEMICAL COMPOSITION OF 4340 STEEL, PER CENT."


Melting Practice Heat No. c Mn Cr Ni Mo Si

0.42 0.66 0.87 1.85 0.24 0.26


Air induction
|i
13
0.39
0.39
0.67
0.73
0.89
0.86
1.89
1.89
0.26
0.27
0.23
0.27
0.40 0.80 0.93 1.95 0.34 0.31
Vacuum induction (1 0.43 0.75 0.88 1.83 0.31 0.29
0.40 0.72 0.91 2.01 0.34 0.37
1? 0.41 0.70 0.67 1.62 0.31 0.31
a
The sulfur and phosphorus contents were less than 0.010 per cent.

TABLE 2—PROCESSING SUMMARY OF 4340 STEEL INGOTS.


Step Operation Details

1 forge fform slab approximately 2 in. thick by 6 in. wide


\ forge at 2200 F, finishing temperature 1800 F
[slow cool, vermiculite
2 machine slab faces plane /^g i n - each face
3 hot roll heat to temperature using low-carbon steel cover plate
carburizing atmosphere in furnace
roll from 0.160 to 0.170 in.
slow cool, vermiculite
sand blast
4 surface grind /check for decarburization
\grind approximately 0.015 in. per side
5 anneal spheroidize anneal
6 cold roll (cold roll from 0.040 to 0.045-in. thickness
\final width to be 6 usable in.

zone thickness; (2) create a finer cast achieved to within a short distance from
structure; (3) reduce microporosity as a the upper surface of the hot top.
result of better feeding; (4) disperse in-
clusions; and (5) decrease gross segre- MATERIALS
gation. Two steels were selected for this in-
The technique for producing unidirec- vestigation. They were 4340 steel and
tional solidification consists of casting the 25 per cent nickel maraging steel. The
molten metal against a water-cooled 4340 steel was selected because it was
copper chill. The sidewalls of the mold typical of the low-alloy tempered mar-
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are Downloaded/printed
made from a by moldable exothermic tensitic steels.
material. The
University mold is illustrated
of Washington (University ofinWashington) Three
Fig. 1. pursuant heats of 4340 steel were air-
to License Agreement. No further reproductions authorized.
124 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

induction melted, and four additional rolling. This work was performed by the
heats of 4340 steel were vacuum-induc- Applied Research Laboratory of United
tion melted. Each of the air melted heats States Steel Corp. The processing sched-
were cast into two ingots, one unidirec- ule for the 4340 steel is given in Table 2.
tionally solidified and the other allowed At the time this investigation was
to solidify in the conventional manner. initiated, the 20 and 25 per cent nickel
The vacuum melted heats were solidified maraging steels were being developed.
either unidirectionally or convention- Since the 25 per cent nickel maraging

TABLE 3—CHEMICAL COMPOSITION OF 25 PER CENT NICKEL


VACUUM-MELTED MARAGING STEEL, PER CENT."
Specifica- ic Ni Ti Al Cb B Zr Mn Si
tion . . 0.0 1/0.03 25.0/26.0 1.70/1.90 0.30/0.50 0.40/0.60 0.002/0.003 0.01/0.05 0.0/0.05 0.0/0.05
Ingot No.

8-1 0 01 + est 25.3 1.85 0.54 0.48 0.0012 0.014 0.02 0.02
8-2 .0.01 est 25.5 1.80 0.45 0.44 0.001 0.016 0.02 0.02
9-1 0.01 est 25.1 1.88 0.48 0.50 0.005 0.017 0.022 0.02
10-1 0.01 est 25.5 1.80 0.35 0.46 0.001 0.010 0.02 0.05
10-2 0.01 est 25.2 1.80 0.48 0.46 0.001 0.014 0.02 0.02
11-1 0.01 est 24.9 1.78 0.42 0.51 0.006 0.021 0.022 0.04
a
Carbon analysis based on previously analyzed heats.

TABLE 4—PROCESSING SUMMARY OF 25 PER CENT NICKEL STEEL INGOTS.


Step Operation Details

1 forge fform slab approximately 2 in. thick by 6 in. wide


start forge <2200F
|finishforge < 1700 F
(air cool
2 machine slab faces plane /^ 6 in each face
3 hot roll fheat to <2200 F using 25 per cent Ni-Fe cover plates
no furnace atmosphere
roll from 0.090 to 0.110 in. thick
air cool
sand blast
4 cold roll f cold reduction to be 50 to 65 per cent
final thickness 0.040 to 0.060 in.
final width to be 6 usable in.

ally. The chemical composition of these steel showed promise of developing


heats are given in Table 1. higher strength levels, it was selected
The as-cast ingots were cylindrical in for this study.
shape, 4 in. in diameter by approximately Six heats of this alloy were vacuum-
4 in. high and weighed 14 to 16 Ib each. induction melted at the Massachusetts
These were converted into sheets 0.040 Institute of Technology. The melting
to 0.060 in. thick, by 6-in. (usable) stock used for these heats consisted of a
width, by various lengths determined high-purity iron-nickel alloy, and the
from the final processed weight of the alloy additions used were electrolytic
ingotCopyright
stock. by
The conversion was accom- material in order to avoid contamination.
ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
plished
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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 125

FIG. 3—Forging, Rolling, and Sheet Identification for Longitudinal Sheets.

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FIG. 4—Forging, Rolling, and Sheet Identification for Transverse Sheets.
126 STRUCTURE AND PROPERTIES OP ULTRAHIGH-STRENGTH STEELS

It will be noted that these heats are


higher than the normal composition in
the contents of the primary hardening
elements, titanium and aluminum. These
additions were made in an effort to obtain
yield strengths on the order of 270,000
psi. The processing schedule for this
material is shown in Table 4.
All ingots were forged and rolled
either parallel or transverse to the longi-
tudinal direction of the ingot. The
methods of forging, rolling, and identify-
ing the various sheets are shown in Figs.
3 and 4.
EXPERIMENTAL PROCEDURES
AND RESULTS
FIG. 5—Displacement Gage for 4 in. Wide
Specimens. The primary prerequisites for these

FIG. 6—Calibration Curves for Displacement Gage.

tionally solidified and two were allowed applications are high strength and
Copyrightinbythe
to solidify ASTM Int'l (all rights manner.
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ability 13:15:25
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crack
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The compositions of these heats are sequently, the materials were studied
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given in Table 3. using standard tension tests and fracture
CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 127

toughness measurements. Standard strip tangency of the driving force curve with
tension specimens according to Specifica- the crack resistance curve, as shown in
tion QQ-M-151a were machined in both Fig. 7. Examination of this figure indi-
the longitudinal and transverse directions cates that the development of crack
of the sheet. The fracture toughness toughness with crack extension, as well
measurements were made using 4- by as the critical value of fracture toughness,
12-in. center-notched specimens. may be employed to investigate material
The fracture toughness specimens behavior.
were machined to size and heat treated When displacement measurements are
to the desired strength. The slot of used to determine fracture toughness, it
length equal to W/4: was cut into the is possible to measure the plane-strain
specimens by an electro-discharge ma- fracture toughness by the pop-in method
chining process. They were then pre-
cracked in fatigue using a reversed bend-
ing plate fatigue machine.
The fracture toughness measurements
were made using the crack opening dis-
placement technique. The displacement
gage was similar to that described by
Boyle (6) and consisted of two L-shaped
arms which are pivoted on the line of
crack extension. An extensometer is
attached to the end of the arms to meas-
sure the deflection. This equipment is
shown in Fig. 5.
The dotted curve of Fig. 6 shows the
theoretical solution for stress and dis-
placement as a function of crack length
as developed by Irwin. The solid curve
in this figure is drawn from experimental
data obtained using 4-in.-wide aluminum
specimens containing slots which had FIG. 7—Schematic Representation Showing
Tangency of Driving Force and Crack Resist-
been carefully machined to specified ance Curves at Onset of Instability. After Krafft
lengths. These curves have essentially (8).
the same shape, but the difference is
considered significant. All of the experi- as described by Boyle, Sullivan, and
mental determinations of fracture tough- Krafft (9). These investigators have
ness were made using the experimental shown that the initiation of the natural
curve. The value of wa/W was deter- tensile crack from the sharp notch or
mined from this curve using displacement fatigue crack occurs under plane-strain
measurements, and the fracture tough- conditions. This effect appears on the
ness was calculated from Irwin's tangent load-displacement record as a discon-
formula: tinuous displacement at a constant load.
This effect has been shown to occur
when the plate thickness is equal to, or
greater than, four times the plastic zone
Irwin (7) and
Copyright KrafftInt'l(8)(allhave
by ASTM reserved);size.
rightsshown MonWhen
Dec the plate thickness
7 13:15:25 EST 2015 is less than
the critical valuebyof fracture tough- the limiting value, the load-displacement
that Downloaded/printed
ness University
is that value defined by
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further reproducti
128 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

linearity. The pop-in point may be 4340 were somewhat lower than the
approximated by the intersection of a elongation values of the air-melted heats.
line drawn tangent to the linear portion In Fig. 8 are shown the crack resistance
and a line drawn tangent to the sloping curves for the air-melted 4340 steel. In
portion of the load-displacement curve. this illustration, the work function,
dW/dA, which is related to K, is plotted
4340 Steel: against the absolute crack extension,
The tensile values obtained for the a — a0.

TABLE 5—TENSILE PROPERTIES OF 4340 STEEL.


Yield Tensile Elonga-
Melting Solidification and Rolling Specimen Strength, Strength, tion,
Heat No. Practice Practice Direction 0.20%
Offset, psi psi %

1 air conventional 1a 227 900 270 300 4.1


longitudinal forge and roll
air unidirectional 1 226 400 269 100 4.5
2
transverse forge and roll
air conventional 1 226 300 272 300 5.2
transverse forge and roll
air unidirectional 1 225 700 277 000 3.6
3
longitudinal forge and roll
air unidirectional 1 221 300 276 300 4.3
transverse forge and roll
4 vacuum unidirectional 1 222 000 266 400 1.7
longitudinal forge and roll t* 221 500 269 000 1.6
5 vacuum conventional 1 221 400 266 700 2.2
longitudinal forge and roll t 219 500 270 600 1.7
6 vacuum unidirectional 1 225 300 264 500 1.6
transverse forge and roll t 220 000 262 700 1.4
7 vacuum conventional 1
transverse forge and roll t 216 300 267 500 1.7
0
b
Longitudinal.
Transverse.

various heats of 4340 steel tempered at It will be observed that the crack re-
400 F are given in Table 5. sistance increases rather rapidly with
Examination of these data shows that crack extension. These curves will ap-
the desired yield strength of 220,000 psi proach a maximum value of fracture
was achieved in all but two examples toughness provided a sufficiently wide
tested. The strength properties and specimen is tested. Only small differences
elongation values of the vacuum-melted can be observed in the slopes of these
4340 steel were essentially the same in curves, indicating that the unidirectional
both the longitudinal and transverse solidification had only a relatively small
directions.
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elongation values of the
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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 129

(a) Unidirectional solidification-transverse, forge and roll.


(6) Unidirectional solidification-longitudinal, forge and roll.
(c) Unidirectional solidification-transverse, forge and roll.
(d) Conventional solidification-transverse, forge and roll.
(e) Conventional solidification-longitudinal, forge and roll.
FIG. 8—Crack Growth Resistance Curves for Air-Melt 4340 Steel (longitudinal specimens).

Similar data for the vacuum-melted The crack resistance curves developed
4340 steel are presented in Fig. 9. from specimens transverse to the rolling
Essentially the same observations can be direction are shown in Fig. 10. It will be
madeCopyright
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resistance curve
air-melted 4340
University of steel. rises less pursuant
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130 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

extension than the curves developed from show that the maximum allowable value
the longitudinal specimens. The single of 0.80 has been exceeded in most cases.
data curve for the equiaxed solidified Therefore, the values of Kc summarized
material appears to be higher than the here are somewhat lower than the true
curves developed for the unidirectionally fracture toughness of the material at

(a) Unidirectional solidification-longitudinal, forge and roll.


(b) Conventional solidification-longitudinal, forge and roll.
(c) Unidirectional solidification-transverse, forge and roll.
(d) Conventional solidification-transverse, forge and roll.
FIG. 9—Crack Growth Resistance Curves for Vacuum-Melt 4340 Steel (longitudinal specimens).

solidified material. However, until more crack instability. However, for compara-
experimental data have been developed tive purposes the values are sufficiently
to substantiate this point, the exact accurate.
degree of significance to be ascribed to These data and the crack resistance
this behavior cannot be assessed. curves of Figs. 8, 9, and 10 indicate that
The values of fracture toughness at the unidirectional solidification had
instability are summarized in Table 6. essentially no effect on the crack tough-
Copyright
The ratios by net
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toughness the uni-
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yield stress summarized in this table directional solidified material was re-
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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 131

markably uniform and independent of in plane-strain fracture toughness has


the orientation of the direction of solidi- been reported by Ebner5 for unidirec-
fication to the rolling direction. tional solidified cast 4340 steel using
The values of plane-strain fracture notched round bars. The behavior of
toughness were determined by the pop-in these materials is consistent with the
method and are summarized in Table 7. findings of improved ductility in uni-
Rather high values were obtained in directionally solidified material. In the
these tests, since both the relatively large example of thin sheets having high values

(a) Unidirectional solidification-longitudinal, forge and roll.


(b) Unidirectional solidification-transverse, forge and roll.
(c) Conventional solidification-transverse, forge and roll.
FIG. 10—Crack Growth Resistance Curves for Vacuum-Melt 4340 Steel (transverse specimens).

plastic zone formed and the crack of fracture toughness, such as the 4340
opening could not be distinguished by steels, plastic deformation accompanying
the displacement gage. However, since all crack propagation is quite extensive.
tests were made using the same technique Calculation of the radius of the plastic
and the data exhibited good consistency, zone size, rys, for the plane stress condi-
the comparisons are considered valid. tion according to Eq 2
Examination of these data show that
the unidirectionally solidified material
exhibited approximately
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5
ture University
toughness. A similar(University
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TABLE 6— FRACTURE TOUGHNESS OF 4340 STEEL.

Heat No. Melting Practice Solidification and Rolling Practice Specimen


Direction
Breaking
Load, Ib a, psi a, in. Kc.VS i vnr "net, psi
fl'net
ffys

a
1 air conventional l 18 400 108 300 0 846 191 000 185 600 0.82
longitudinal forge and roll
air unidirectional 1 20 900 127 300 0 897 234 800 209 400 0.93
transverse forge and roll
2
air conventional 1 21 500 126 500 0 817 219 300 211 900 0.93
transverse forge and roll
air unidirectional 1 18 500 112 400 0 890 206 500 192 000 0.85
3
longitudinal forge and roll
air unidirectional 1 19 500 114 500 0 904 212 800 193 800 0.88
transverse forge and roll
4 vacuum unidirectional 1 17 000 111 900 0 803 196 100 184 900 0.83
longitudinal forge and roll t6 7 100 42 300 1 271 88 600 105 700 0.48

5 vacuum conventional 1 10 900 85 100 0 895 168 200 112 200 0.51
longitudinal forge and roll
6 vacuum unidirectional 1 19 500 122 000 o 834 216 600 198 600 0.90
transverse forge and roll t 10 300 61 300 1 047 126 500 130 400 0.60
7 vacuum conventional 1 18 700 120 900 0 889 223 200 192 500 0.89
' transverse forge and roll t 16 500 99 400 1 043 208 000 202 800 0.94
0
b
Longitudinal.
Transverse.

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CARMAN EX AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 133

using a Kc value of 200,000 psi \7rrZ and of fracture toughness under plane-strain
a yield strength of 220,000 psi gave a conditions.
value of 0.133 in., which is greater than
three plate thicknesses. 25 Per Cent NlcM Ma™g™S Steel:
However, under plane-strain condi- This material is austenitic as annealed,
tions, the plastic flow is restricted to a and hardening may be accomplished by
region at the tip of the advancing crack two methods. The first method consists

TABLE 7—PLANE-STRAIN FRACTURE TOUGHNESS OF 4340 STEEL.


Speci-
Heat Melting Solidification and Rolling men Load at a, psi aa , in. KI c ,
No. Practice Practice Direc- Pop-In, Ib psi vin.
tion

1a i r conventional 1- 13 800 81 600 0.559 115 700


longitudinal forge and roll
air unidirectional 1 15 800 96 100 0.522 133 700
transverse forge and roll
2
air conventional 1 17 810 104 700 0.512 135 000
transverse forge and roll
air unidirectional 1 15 300 93 000 0.540 131 200
longitudinal forge and roll
3
air unidirectional 1 15 100 91 900 0.525 122 800
transverse forge and roll
4. . . vacuum unidirectional 1 16 600 87 600 0.527 120 900
longitudinal forge and roll t" 5 700 33 900 0.691 53 000
5. . . vacuum conventional 1 8 200 64 300 0.513 86 300
longitudinal forge and roll
6. . . vacuum unidirectional 1 16 400 101 900 0.523 143 500
transverse forge and roll t 9 500 56 600 0.717 96 100
7 . . . vacuum conventional 1 14 600 94 300 0.517 123 100
transverse forge and roll t 12 900 77 900 0.578 113 500
0
Longitudinal.
6
Transverse.

front. The radius of the plastic zone size of cold rolling approximately 65 per cent
under these conditions is defined by Eq 3 followed by a sub-zero treatment to
transform the austenite to martensite
and maraging at 850 F. The second
method involves an ausage at 1300 F for
This calculation, using a Klc value of 4 hr followed by a sub-zero treatment to
110,000 psi \/irI and a yield strength of transform the austenite to martensite
220,000 psi, gave a value of 0.013 in. for and maraging at 850 F.
the plastic zone radius. It will be noted The strength developed by this
that this is approximately one third of material is directly related to the content
the plate thickness. It would be antici- of the hardening elements, titanium and
pated that higher percentages of micro- aluminum. The general commercial
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134 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

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FIG. 11—Structures Observed in Cold-Rolled, Sub-Zero Treated and Aged 25 per cent Nickel
Maraging Steel.

titanium and 0.15 to 0.35 per cent alu- 16 hr and maraged at 850 F for 3 hr.
minum or a total of 1.95 per cent hard- This treatment gave a yield strength of
ener. The total hardener content of these 223,500 psi, a tensile strength of 285,600
special melts was from 2.00 to 2.40 per psi, and an elongation of 2.5 per cent.
cent. These values of strength are somewhat
Since this material was received in the lower than would be anticipated from the
cold-rolled condition,
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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 135

from the grip ends of these tension heats developed quite high tensile
specimens. The structure observed, values. In general, it can be seen that
Fig. 11, clearly shows the directional the unidirectionally solidified material
effects of the cold working. Although not shdwei higher tensile properties than the
clearly denned, there are some indica- comparable conventionally solidified
tions of retained austenite. '',',-.. material*Specimens oriented transverse
Therefore, a second ^set of tension to tHe rolling direction showed higher
specimens were hardened by the ausaging mechanical^ strengths than the corre-
method. These specimens* were solution- sponding longitudinal specimens but
annealed at 1500 F for 1 hr, ausaged at with some loss in elongation.
TABLE 8—TENSILE PROPERTIES OF 25 PER CENT NICKEL
VACUUM-MELTED MARAGING STEEL.-
Rolling Specimen Yield Strength Tensile Elongation
Sheet No. Type Solidification Direc- Direc- 0.20% Offset, Strength, psi in 2 In.,
tion tion psi %

8-1 A unidirectional lb 1 280 000 301 500 2.1


8-1 A unidirectional 1 t 288 900 314 500 2.7
8-2A unidirectional 1 1 277 700 299 000 3.0
8-2A unidirectional 1 t 296 600 315 800 2.3
8-2B unidirectional 1 1 274 500 299 800 3.7
8 2B unidirectional 1 t 279 900 304 300 3.1
9-1A conventional 1 1 253 900 279 600 2.0
9-1A conventional 1 t 249 200 252 000 0.8
9-1C conventional 1 1 271 500 298 500 2.0
9-1C conventional 1 t d 243 300 0.3
10-1 unidirectional tc 1 260 500 284 400 3.2
10-1 unidirectional t t 282 700 305 100 2.5
10-2 unidirectional t 1 272 100 297 800 3.8
10-2 unidirectional t t 278 200 305 200 3.3
11-1 conventional t 1 260 200 286 300 2.5
11-1 conventional t t d 258 200 «

0 Average four to six tests.


6 Longitudinal.
e Transverse.
d Broke without yielding.
e Broke outside gage length.

1300 F for 4 hr, sub-zero treated at The fracture toughness values ob-
-100 F for 16 hr, and maraged at 850 F tained from these specimens were very
for 3 hr. This treatment gave the follow- disappointing. The values were only 20
ing mechanical properties: 279,000 psi per cent of those reported by the Inter-
yield strength, 293,100 psi tensile national Nickel Co. (11) for comparable
strength, and 3.5 per cent elongation. material.
These strength values are consistent Metallographic examination of these
with those anticipated from the total specimens showed an extremely hetero-
hardener content of the alloy. A series of geneous structure, as shown in Fig. 12.
tension and fracture toughness specimens The background in this figure appears to
were heat treated using this procedure. be aged martensite with heavy stringers
The tensile values obtained are sum- of a light etching phase. To identify this
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marized in Table 8. All of the various
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136 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

Etched in HNO3 , HC1, and CuCl2 solution.


FIG. 12—Structures Observed in 25 per cent Nickel Maraging Steel Having Standard Ausaging
Treatment.

TABLE 9—MICROPROBE ANALYSIS OF 25 PER CENT


NICKEL MARAGING STEEL, %.
Ti Ni Fe

Matrix 1.5 to 1.8 25.0 to 25.2 71.8 to 72


White Phase. 2.0 to 2.1 27.0 to 27.5 69.5 to 70

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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 137

ducted on the polished and etched speci- A series of fracture toughness speci-
men. The results of this analysis are mens were sub-zero treated with liquid
presented in Table 9. nitrogen in an attempt to minimize the
Based on this analysis and the etching retained austenite. The treatment was as
characteristics, it was concluded that the follows: solution anneal for 1 hr at

Etched in HNO3 , HC1, and CuCl2 solution.


FIG. 13—Structures Observed in 25 per cent Nickel Maraging Steel Having an Ausaging Treat-
ment Using Liquid Nitrogen for the Sub-Zero Phase.

light etching phase is austenite. This 1500 F, sub-zero treatment with liquid
examination indicated that, if the nitrogen, ausage for 4 hr at 1300 F, sub-
amount of retained
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couldreserved);
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treatment with liquid nitrogen, and
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reduced, the fracture
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be improved. toughness
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Etched in HNO3 , HC1, and CuCl2 solution.
FIG. 14—Structures Observed in Cold-Rolled, Sub-Zero Treated with Liquid Nitrogen and Aged
25 per cent Nickel Maraging Steel.
TABLE 10—TENSILE PROPERTIES OF 25 PER CENT NICKEL MARAGING
COLD-ROLLED STEEL, SUB-ZERO TREATED WITH LIQUID NITROGEN
AND AGED AT 850 F.

Specimen Yield Tensile


Sheet No. Type Strength Elongation
Solidification Rolling direction Direc- 0.20% Strength,
tion psi in 2 In., %
Offset, psi

10-1 -B unidirectional t 1 260 200 306 000 1.5


forge and roll t 295 900 326 700 1.0
9-1 -B conventional I6 1 269 200 311 700 1.8
forge and roll t c

Transverse.
6
Longitudinal.
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* Failed withoutbyyielding.
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TABLE 11— FRACTURE TOUGHNESS VALUES OF 25 PER CENT NICKEL MARAGING STEEL,
LONGITUDINAL SPECIMENS.
Treatment Sheet No. Solidification Practice Rolling Practice Kc , psi -\/in.
8-1 -A unidirectional longitudinal, forge and rol 23 000
8-1 -B unidirectional longitudinal, forge and rol 20 200
8-2-A unidirectional longitudinal, forge and roll 22 500
Solution anneal ausage and sub-zero treated 8-2-B unidirectional longitudinal, forge and roll 18 600
at - 100 F and marage 850 F 9-1 conventional longitudinal, forge and roll very brittle
10-1-B unidirectional transverse, forge and roll 30 400
10-2-B unidirectional transverse, forge and roll 21 400
11-1-B conventional transverse, forge and roll 30 100
Solution anneal sub-zero treated at — 320 F ( 8-1 -A unidirectional longitudinal, forge and roll 39 500
ausage and sub-zero treated at — 320 Fl 8-2-A unidirectional longitudinal, forge and roll 39 000
and marage at 850 F 10-1 -B unidirectional transverse, forge and roll 49 000
11-1-B conventiona transverse, forge and roll 45 200
Cold roll 60 per cent, sub-zero treatedf 9-1 conventional longitudinal, forge and roll 85 100
- 320 F and marage 10-1-B unidirectional transverse, forge and roll 66 900

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140 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

showed a 50 per cent improvement. PRACTICAL IMPLICATIONS


Metallographic examination of these
specimens, Fig. 13, showed that the After having investigated the proper-
retained austenite level had been ties of these materials, it is important to
reduced. be able to estimate how these materials
To carry this investigation a step will behave in service. The following cal-
further, tension and fracture toughness culations are presented to give the
specimens of heats 9 and 10 were ma- reader an insight into how these materials
chined from the cold-rolled stock and will behave under two service conditions:
sub-zero treated with liquid nitrogen. (1) thin-walled pressure vessels, and (2)
The specimens were then maraged at heavy sections.
850 F for 3 hr. The structure observed in The crack length at instability may be
these specimens, Fig. 14, was similar to calculated from Eq 4:
that observed in the material sub-zero
treated at —100 F (compare Figs. 11
and 14).
The tensile values obtained for these
specimens are summarized in Table 10.
The strengths developed by this method Using a Kc of 200,000 psi \/in. and a
are quite comparable to those developed stress equal to the yield strength of
by the ausaging treatment (compare 220,000 psi for the 4340 steel, this calcu-
Tables 8 and 9). lation gave a critical crack length of
The fracture toughness values for this 0.264 in. These data indicate that the
material are summarized in Table 11. 4340 steel has a high reserve of fracture
These data show that, as the quantity of toughness. The crack length at instability
retained austenite is reduced, the frac- for this material is approximately six
ture toughness is upgraded (compare times the plate thickness. Mathemati-
data for standard and liquid-nitrogen cally, the arrest of such a long crack is
ausaging treatments). The ausaging treat- possible under flat sheet conditions.
ment has been reported to embrittle However, as pointed out by Irwin (l)
this material. This effect was also ob- and demonstrated by Carman, Armiento,
served here (compare data for ausaged and Markus (12) local bulging at the
and cold-rolled, liquid-nitrogen-treated crack tip in a pressure vessel elevates the
specimens). The International Nickel local stress field so that crack arrest is
not possible.
Co. has ascribed this embrittlement to
However, of greater practical impor-
the precipitation of titanium compounds
tance is the behavior of a part-through-
in the grain boundaries. crack which is characteristic of defects
In regard to the effect of solidification most frequently found in structures. This
practices, the fracture toughness data type of defect is potentially more danger-
show that all of the heats are quite ous since its propagation is under plane-
brittle. Although the objective of high strain conditions where energy absorp-
tensile properties has been achieved, the tion is at a minimum. Irwin (13) has
reduction in fracture toughness was derived an expression relating the frac-
great enough that this material could ture toughness, crack geometry, and
hardly be considered useful for structural stress for a semi-elliptical crack. This
purposes. expression is given in Eq 5
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CARMAN ET AL ON THE EFFECT OF SOLIDIFICATION PRACTICE 141

solidified material. These calculations


show an advantage for the unidirectional
solidified material.
It should also be noted that, even with
materials having a margin of fracture
toughness, care must be taken in fabrica-
tion and inspection to eliminate defects.
However, the dimensions of the defects
For semi-circular cracks and for those described fall well within the current
which are shorter and deeper, calculation capabilities of fabrication and non-
of crack depth from Eq 5, using a KJc of destructive testing.
115,000 psi \/in. and a stress equal to
the yield strength of the material, gave a CONCLUSIONS
depth of 0.160 in. This value is considera- The results of this preliminary investi-
bly greater than the plate thickness so gation demonstrate the following points:
that the failure of the 0.040-in. plate 1. No improvements due to unidirec-
would be controlled by the Kc value. tional solidification are shown in the
Under these conditions slow crack growth plane-stress crack toughness, Kc, of
and local bulging will occur prior to the 0.040-in. 4340 sheet.
fracture. The leak-before-burst criterion 2. The unidirectional solidified 4340
will be satisfied and high burst stresses steel shows approximately a 10 per cent
are possible. improvement in the plane-strain fracture
The advantages of the unidirectional toughness, Klc. In this mode of fracture,
solidified material as determined in this plastic deformation is restricted and
investigation can best be realized in microporosity would be expected to
heavy sections where fracture is governed exert an influence on the fracture proper-
by the plane-strain fracture toughness. ties.
Calculation of the depth of crack at 3. Tensile data of the unidirectionally
instability, assuming a semi-circular solidified 25 per cent nickel maraging
crack geometry using a KIC value of steel show a superiority over conven-
110,000 psi \/in. for the conventional tionally solidified material. However,
solidified material, gave an a (crack the fracture data show the dangers
depth) value of 0.146 in. The same calcu- inherent in attempting to upgrade the
lation using a Kjc value of 120,000 psi strength of a material beyond its devel-
\/in. for the unidirectional solidified oped limits.
material gave an a value of 0.174 in. Although the data described in this
In the example in which the crack is paper are not considered fully conclusive,
long compared to its depth, Eq 5 reduces they point out a solidification technique
to which should result in higher fracture-
toughness values in structural materials.
A cknowledgment:
Calculation of the crack depth at insta- The authors wish to thank the Applied
bility using the same numerical values as Research Laboratory of United States
before gave an a value of 0.066 in. for the Steel Corp. for processing the various
conventional solidified material, and an ingots, Prof. M. C. Flemings of the
a value of 0.079 in. for the unidirectional Metallurgy Department of Massachu-
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142 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

setts Institute of Technology, who super- Krafft of the U. S. Naval Research


vised the work at M.I.T., and J. M. Laboratory for reviewing the paper.
APPENDIX I

K = parameter describing the local eleva- W = specimen width, in.,


tion of the elastic stress field at tip of <JVs = yield strength, psi,
advancing crack, psi Vin^, o"net = net section stress, psi,
/ = first or opening mode of fracture, B = specimen thickness, in.,
a = gross section stress, psi, ft = relative plastic zone size,
a = % crack length or % the minor axis of
an elleptical crack, in., v = displacement in y direction,
c = subscript denoting critical value of 9 = strain energy release rate, and
any parameter, R = crack resistance of the material.

REFERENCES
(1) G. R. Irwin, "Relation of Crack Toughness Materials Research & Standards, Am. Soc
Measurements to Practical Applications," Testing Mats., August, 1962.
Welding Journal Research Supplement, (7) G. R. Irwin, "Fracture Testing of High
November, 1962. Strength Sheet Materials under Conditions
(2) "Investigation of Solidification of High Appropriate for Stress Analysis," Naval
Strength Steel Castings under Simulated Research Laboratory, Report No. 5486,
Production Conditions," Foundry Section, July, 1960.
Metals Processing Division, Department (8) J. M. Krafft, A. M. Sullivan, and R. W.
of Metallurgy, Massachusetts Institute of Boyle, "Effect of Dimensions on Fast
Technology, Final Report, July, 1960, Fracture Instability of Notched Sheets,"
Department of the Army, Contract No. Symposium on Crack Propagation, The
Da 19-020-505-ORD-4511. College of Aeronautics, Cranfield, England,
(3) M. C. Flemings, R. V. Barone, H. F. September, 1961.
Taylor, and S. Z. Uram, "Solidification (9) R. W. Boyle, A. M. Sullivan, and J. M.
Studies on High Steel Castings and Ingots," Krafft, "Determination of Plane Strain
Transactions American Foundrymen's Soci- Fracture Toughness with Sharply Notched
ety, Vol. 69, 1961, pp. 422^35. Sheets," Welding Journal, Research Supple-
(4) S. F. Wallace, J. H. Savage, and H. F. ment 428-S to 432-S, 1962.
Taylor, "Mechanical Properties of Cast (10) R. W. Decker, R. B. G. Yeo, and C. G.
Steel as Influenced by Mass and Segrega- Bieber, "The Maraging Steels," Materials
in Design Engineering, May, 1962.
tion," Transactions American Foundry- (11) C. M. Carman, D. F. Armiento, and H.
men's Society, Vol. 59, 1951. Markus, "Fracture Toughness and Pres-
(5) S. Z. Uram, M. C. Flemings, and H. F. sure Vessel Performance," Journal of
Taylor, "High Strength Cast Steel Struc- Power Engineering, Transactions, ASME,
ture and Microporosity Effect on Mechani- Series A, Vol. 86, 1964, p. 465.
cal Properties," Modern Castings, Vol. 38, (12) G. R. Irwin, "Crack Extension Force for a
No. 1, 1960. Part-Through-Crack in a Plate," Journal
(6) R. W. Boyle, "A Method for Determining of Applied Mechanics, Vol. 29, Transactions,
Crack Growth in Notch Specimens," ASME, Vol. 84, Series E, 1962, p. 651.

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DISCUSSION

J. M. KRAFFT1—It is interesting to note notched tension specimens, as shown in


the apparent contradictory result of Table 12.
vacuum melting the 4340 steel. Here the This difference indicates that it is
plane-strain fracture toughness, K I c , is much more difficult for cracks to pop-in
improved while the elongation of the un- in sheet fracture toughness specimens
notched specimen decreases. The dis- than for a crack to extend under more
cusser has recently attempted to charac- constrained conditions. Certainly it sug-
terize metals in terms of a fixed process gests that the KIC values obtained in the
zone size: two ways should be distinguished. Also,
the KIC values obtained from circum-
ferentially notched tension specimens
may be more appropriate to the case of a
where E is Young's Modulus and n is the crack embedded in a heavy section. If so,
strain hardening exponent. If the elonga- flaws or cracks ^ of the size calculated by
tion is reduced this would suggest a the authors (or 0.0073 to 0.0088 rather
reduction in n and thus an increase in the than 0.066 to 0.079) could propagate
process zone size dT . It is not unreasona- under stresses equal to the yield strength.
ble to expect such increase as nonmetallic Detecting O.OlO-in.-deep flaws by non-
inclusions; the sites for plastic enclave destructive testing is considerably more
tensile ligament formation would be difficult than detecting those ten times
fewer, permitting their growth to a larger. Would the authors care to com-
larger size as they are fed into the crack. ment on this difference?
However, before embarking on such R. S. CREMisio3—These authors are
speculation it would be most helpful to to be congratulated for providing such
know whether the reported dimunition interesting data on a subject of timely
in elongation was indeed associated with interest.
a corresponding decrease in the strain In our solidification work at Mellon
hardening exponent. Institute, sponsored by the Universal-
MERRILL L. EBNER2—In this carefully Cyclops Steel Corp., we have been par-
executed study I was particularly ticularly interested in unidirectional
puzzled by the KIC values obtained from solidification, specifically in reference to
0.040-in. sheet specimens using the pop- high-alloy steels and high-temperature
in method. The authors' values, Table 7, alloys. Our observations generally paral-
are about three times greater than those lel those made in this paper. For example,
I obtained on similar steels at equivalent we have a fair amount of evidence that
hardness
Copyrightlevels using
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Int'l (all rights reserved); Monhigh
Dec 7temperature properties of nickel-
13:15:25 EST 2015
1
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of Washington Laboratory,of Washington)
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ington,
2
D. C. Advisory, Mellon Institute, Pittsburgh, Pa.,
Department of Metallurgy, Massachusetts and associate manager, R & D Process, Universal
Institute of Technology, Cambridge, Mass. Cyclops Steel Corp., Bridgeville, Pa.
143
144 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

nar crystallization, in respect to (1) hot The more one studies metals, the more
workability, (2) toughness, and (3) rup- one doubts that any single alloy strength-
ture and creep strength. ens by any single mechanism. However,
Though not yet completely con- we have observed that unidirectional
firmed in our experimentation, it appears solidification'tends to be more effective
in alloys whose properties are derived by
TABLE 12—Kic VALUES FOR AISI a precipitation or dispersion mechanism
4340 STEEL OBTAINED USING CIRCUM- rather than in alloys which strengthen
FERENTIALLY NOTCHED SPECIMENS."
by a transformation process. The present
Wt. %, Cfc Type of Ingot Mold Kjc, psi-v/hT results seem to bear out this contention
cd
in that the maraging steels, which are
0.36 sand ' 39 000
0.36 sandc -d 40 800 strengthened by both a transformation
0.36 sandc-d 41 300 and precipitation process, depending on
0.36 sandc 'd 36 800 condition, seem to have derived more
c d
0.36 uds - 46 700
0.36 udsc'd 42 800 benefit from unidirectional solidification
0.36 udsc'd 42 800 than the 4340 steel. One further comment
0.48 sand 29 800
along these lines is that these general
0.48 sand 29 800 results are consistent with our observa-
0.48 sand 32 600 tion that unidirectional solidification
0.48 sand 30 500
0.48 uds 29 500 seldom results in poorer properties than
0.48 uds 30 200 those related to conventional casting.
0.48 uds 32 000 In studying casting structures over a
0.48 uds 29 000
0.48 uds 33 300 wide range of unidirectionally solidified
0.48 uds 30 300 ingot sizes, we have observed two pre-
0.39 commercial* 32 400
dominant effects:
0.39 commercial* 28 000 1. Unidirectionally solidified ingots
0.39 commercial8 32 200 are structurally (as well as chemically)
0.39 commercial* 31 800
0.39 commercial* 26 100 more homogeneous than conventional
0.39 commercial" 30 700 ingots.
0.39 commercial* 30 900 2. The properties of small ingots of
0
Specimens with a major diameter of 0.75- unidirectionally cast material are more
in., fatigue-cracked after heat treatment to directly proportional to those in large
give a half-area notch. Heat treatment: Aus-
tenitized at 1550 C, oil quenched, refrigerated
ingots, whereas in conventionally cast
in liquid nitrogen, tempered 1 hr at 400 F. material this is clearly not the case.
6
All other alloy elements within specifica- My point is, if the authors were to
tion for commercial quality AISI 4340 steel.
c
These two types of ingot mold are the same produce material by unidirectional solidi-
as those used by the authors (UDS = mold fication on a commercial scale, comparing
producing unidirectional solidification). unidirectional to conventional should
d
Ingots were homogenized, 2200 F, 3 hr,
and normalized from 1750 F before being cut up. yield greater differences, with the uni-
* Reduced to 1-in.-diameter rod. directionally solidified material being
superior. In addition, the technological
that unidirectional solidification benefits application of unidirectional solidifica-
are a direct function of the strengthening tion to commercial practice would result
mechanism of a given alloy. That is, in a much more highly controlled casting
whether it be (1) solid solution strength- procedure, which in turn would be
ening, (2) precipitation or dispersion amenable to secondary techniques, such
strengthening, or (3) transformation as seeding, in a much more effective way
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strengthening.
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DISCUSSION ON THE EFFECT OF SOLIDIFICATION PRACTICE 145

ics of such a process seem to be entirely melted and the vacuum-melted 4340
reasonable and application to continuous steel is essentially the same.
processing is feasible. Carrying this analysis one step further,
Finally, our observations as to possible it appears that the n value has not been
solidification mechanisms have been that altered by the change in solidification
unidirectional solidification may lead to practices. Since dT is proportional to K^c,
orientation effects on a micro scale, the process zone size for the unidirection-
which in turn can effect the type, size, ally solidified 4340 steel is 10 per cent
and distribution of second phases in a larger than for the equiaxed solidified
beneficial way. material. Since these plastic enclave
We hope these affirmative comments tensile ligaments are nucleated by micro-
will encourage the authors to further void coalescence, a reduction in micro-
pursuits in the field of controlled solidifi- porosity should result in a larger process
cation for improvement of metal and zone size.
alloy properties. In regard to Ebner's comments, the
S. V. ARNOLD*—In view of heat authors have pointed out the problems
transfer problems, what is the feasibility which may be encountered in measuring
of scaling up unidirectional solidification plane strain when no distinct pop-in is
practice to produce steel ingots of com- observed. Consequently, the values of
mercial dimensions? K ic presented in the paper are indicative
C. M. CARMAN, R. W. STRACHAN, of trends which may be anticipated
D. F. ARMIENTO, AND H. MARKUS rather than absolute values of plane-
(authors)—We wish to thank the dis- strain fracture toughness.
cussers for their comments. Krafft has Mr. Ebner's data for these materials
equated the elongation of the smooth using circumferentially notched round
tension specimens to n, the strain hard- specimens are a valuable addition to this
ening exponent. paper. His data confirm the behavior
To verify this point, the strain harden- trends established using the sheet mate-
ing exponents of the vacuum- and air- rial and supply values of plane-strain
melted 4340 steels were determined fracture toughness which are considered
using a stepped tension specimen, as more representative of this steel.
discussed by Heyer. The n values so The pop-in of a small crack in a thin
determined are equal to 0.049 for both plate is a very complicated process. As
steels. Examination of Table 5 of the the stress field intensity parameter is
paper shows that, for most practical pur- increased, the plastic zone at the tip of
poses, n may be taken equal to the per the crack grows and may possibly extend
cent elongation for the air-melted 4340 almost through the plate. At the point
steel. However, this does not apparently when K is equal to K l c , slow crack
hold true for the vacuum-melted 4340 growth occurs and the situation rapidly
steel. The elongation of the vacuum- changes from plane strain to plane stress
melted 4340 is considerably less than its with no distinct pop-in. In very heavy
strain-hardening exponent. This may be sections when K is equal to KIC , plane-
ascribed to highly localized plastic de- strain instability occurs without slow
formation during necking of the speci- crack growth. However, it is not felt that
men. Using Dr. Krafft's analysis the a special nomenclature to describe this
process zone size, dT, for both the air- behavior is needed.
4
U. S. Army
Copyright Materials
by ASTM Research
Int'l (all In7 13:15:25
Agency,Mon Dec
rights reserved); regard EST
to 2015
Cremisio's comments.
Watertown, Mass.
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146 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

tional solidification is the improved to large size ingots. However, for such
distribution of microsegregates.5-6 Be- ingots, the face, or faces, through which
cause the precipitation hardenable steels heat is extracted must be large compared
generally are much richer in solute than with the adjoining faces, if solidification
low alloy steels, microsegregation in is to be achieved in a reasonable time.
these steels is usually more severe. This For example, a 4,000 pound ingot can be
seems to us a likely reason for Mr. made in a mold 8" x 3' x 4'. If heat is
Cremisio's observation that unidirec- extracted through the 4' x 3' face, com-
tional solidification results in greater plete unidirectional solidification can be
improvement in properties in a maraging achieved in approximately one hour.
steel than; in. 4340. However, if heat is extracted through
In answer to Mr. Arnold's question, it the 8" x 3' face, approximately 40 hours
is entirely feasible to scale this process up would be required.7
5 7
M. C. Flemings, "Microsegregation in R. F. Polich, G. E. Nereo, and M. C.
Castings and Ingots," Modern Castings, Vol. Flemings, "Directional Solidification Studies,"
46, 61964, pp. 353-362. Final Report, Department of the Army, Novem-
P. J. Ahearn and F. C. Quigley, "Mass ber, 1963; Contract No. DA 19-020-AMC-
Effect and Microsegregation in a High Strength 5753(Z), Foundry Section, Metals Processing
Steel Casting," Modern Castings, August, 1964, Division, Department of Metallurgy, Massa-
pp. 435-440. chusetts Institute of Technology.

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HIGH-STRENGTH STEEL FORCINGS
BY H. J. HENNING1

SYNOPSIS
This paper describes the existing state-of-the-art for production forgings
manufactured from steels treatable to strengths in excess of 200,000 psi.
The need for increasing cleanliness with an increasing strength requirement
is emphasized, particularly for those applications where design criteria require
high transverse ductility. Economical vacuum arc melting has been largely
responsible for bringing reliable, reproducible high-strength steel forgings to a
production level of activity.
Experience in forging a variety of alloys has highlighted relative levels of
uniformity and reliability. Some of the more often selected high-strength steels
are discussed from the standpoint of ease of forging, uniformity of strength
response, and general quality. Data are given on cleanliness, transverse
ductility, and other important properties for such alloys as Ladish D-6ac,
AMS 6427, and AISI 4340.
Methods for achieving high strengths vary from the standard quench and
draw to the more complex thermal-mechanical treatments. The latter treat-
ments, while readily applied to flat products, are difficult to impart to most
forgings because complex shapes do not lend themselves to uniform levels of
reduction.
Mechanical property values obtainable in forgings produced from maraging
steel are discussed. These steels represent a potential for the highest strengths
obtainable in the steel family. The highest ductilities, however, are obtained
by forging sequences that require added manufacturing steps. Since this repre-
sents added cost, data useful for specifying practical levels of properties are
presented.

As pointed out in a recently published Formerly, steels like AISI 4340 and
article, advancements of late have 4330 were rarely used at strengths higher
effected a significant increase in the than 180,000 psi, because they were not
design allowable strength for alloys in clean enough to exhibit the necessary
the steel family. Clearly, one of the most property uniformity. Now these alloys
important reasons for the increased are so clean that we have become
strength capability of steel has been the accustomed to ductilities at the 260,000
development of economical vacuum psi strength level that once were normal
melting, which in turn is capable of to the 150,000 psi level. Even more
producing steel about 500 times cleaner important, transverse ductilities are
that the standard aircraft quality steels nearly as high as those in the longi-
melted a few years ago. tudinal direction.
1
Metallurgist, The Ladish Co., Cudahy, Wis' Since the advantages of vacuum-
147
TABLE 1—NOMINAL COMPOSITIONS OF SEVERAL TYPICAL HIGH-STRENGTH STEELS.
Chemical Composition, per cent
Alloy Designation
C Mn Si Cr Ni Mo V Co Ti Al Other

MARTENSITIC HARDENABLE

AISI 4340 0.40 0.70 0.25 0.80 1.70 0 . 25


AISI 4330 Mod. 0 . 30 0.70 0.50 1.20 2.00 0.45 0.07
Ladish D-6ac 0.46 0.70 0.30 1.00 0.60 1.00 0.10
H-ll 0.35 0.30 1.00 5.00 1.50 0.40

SEMI-AUSTENITIC PRECIPITATION HARDENABLE

17-7 PH 0.09 0.70 0.50 17.00 7.00 1 . 20


AM 355 0.14 1.00 0.40 15.50 4.30 2.70 N O . 10
PH 15-7 Mo 0.06 0.60 0.40 14.50 7.30 2.30 1.20

MABAGING

17-4 PH 0.07 0.70 0.50 16.50 4.00 Cu4.00


18NiCoMo(300) 0.01 0.10 0.10 18.00 5.00 9.00 0.70 0.15
18NiCoMo(250) 0.01 0.10 0.10 18.00 5.00 8.00 0.40 0.15
20 Ni 0.01 0.10 0.10 19.00 1.50 0.30
25 Ni 0.01 0.10 0.10 25.00 1.50 0.30

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HENNING ON HIGH-STRENGTH STEEL FORCINGS 149

melted steel are well covered in a host of condition provided incentive for pro-
publications, this paper will de-empha- ducing forgings to closer dimensional
size that subject and consider, instead, tolerances. However, programs aimed
the following: toward achieving closer tolerances have
1. forging alloys that have achieved not been very fruitful because of the
the higher levels of uniformity, high manufacturing and tooling costs.
2. quality and acceptance criteria for Thus, production forging designs for
the high-strength steels developed since these steels have not changed much in
the coming of vacuum melting, and the past few years.
3. the application of measures to The semi-austenitic precipitation hard-
insure reliability and uniformity, par- enable stainless steels present more
ticularly in the maraging steels. imposing problems in forging. Because
some develop delta ferrite on heating,
TYPES OF HIGH-STRENGTH STEELS forging temperatures are usually lower
than for the low-alloy martensitic types.
The high-strength steels of greatest The higher alloy contents lead to greater
interest today are those which can be forging forces. Thus a larger number of
treated to strengths exceeding 200,000 forging steps are usually needed. Another
psi, such as the following: characteristic is that lower finishing
1. martensitic hardenable steels heat temperatures are necessary to insure
treated by conventional quenching and satisfactory response to subsequent heat
tempering to strengths between 200,000 treatment. On the plus side, they are not
and 280,000 psi, sensitive to decarburization and scale
2. semi-austenitic precipitation hard- far less than the martensitic types when
enable stainless (PH grades) capable of heated for forging. For these reasons,
achieving strengths ranging from 170,000 small parts may be forged with closer
to 220,000 psi, and finish allowances and sometimes with
3. maraging steels. These alloys are as-forged surfaces. These steels are not
similar in many respects to the PH widely used in the form of forgings,
steels, but heat treatable to strengths mainly because they do not offer any
in the range of 200,000 to over 300,000 strength advantages over the marten-
psi. sitic grades. Widest use is in sheet appli-
Nominal compositions of alloys typical cations because of their superior re-
for each of these groups are given in sistance to oxidation.
Table 1. Obviously, these do not com- Maraging steels are comparatively
prise a comprehensive listing, but rather new to the forging industry, and forging
are some of the more widely used forging processes are under constant study. They
alloys. are as forgeable as the martensitic
FORGING OF HIGH-STRENGTH grades, but to insure optimum mechan-
ical properties, they must be forged
STEELS
with substantial reduction in the last
The martensitic hardenable grades of operation at temperatures below 1800
steel are forged with the customary F, thereby requiring forging forces in
techniques and methods used widely for the vicinity of those required for forging
years. The newer high-strength applica- the nickel-base superalloys. What this
tions, however, have introduced special means to designers is that forgings must
problems. The difficulty and expense of
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generous con-
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150 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

equipment becomes necessary to provide Magnaflux Cleanliness—A total of


adequate forging forces. 268 test bars, representing over 70
heats of vacuum arc remelted (L) D-6ac
QUALITY OF HIGH-STRENGTH steel, were evaluated according to
STEELS frequency and severity of magnetic
We have purchased, tested, forged, indications. It is significant that over
and tested further, millions of pounds of 97 per cent of the test bars passed the
the high-strength steels produced by all 0.5/1.0 frequency-over-severity require-
of the following melting practices: (1) ment of AMS-2300A. Generally speak-
electric furnace air melting, (2) electric ing, this is several hundred times cleaner
furnace air melting followed by vacuum than the typical electric furnace grades.
degassing, and (3) vacuum consumable It is quite reassuring to know that this
electrode arc remelting. degree of cleanliness is characteristic of
In the normal course of quality con- steels utilized for missile production.
trol, numerous tests are performed More recent specifications for this
to ascertain the quality of both billets material reflect even tighter magnetic
and forgings. Advances in cleanliness cleanliness requirements. For example,
through vacuum arc remelting are one of the leading aircraft companies
illustrated vividly by data supplied by is specifying, hi essence, a maximum
the following types of tests: permissible frequency/severity rating
1. Magnaflux Cleanliness—as rated of 0.1/0.2. Analysis of the same magna-
by the Standard Aeronautical Materials flux data has shown that 93 per cent of
Specifications 2301 and 2300, the heats meet this even stricter require-
2. Microcleanliness—as rated by the ment; and this is without the mills
Jernkontoret micro inclusion comparison having prior knowledge of the tighter
outlined in ASTM E 45, requirement. This means that 93 per
3. Ultrasonic Quality—as determined cent of the heats tested have fewer than
by our own specifications similar to the four magnetic indications of a ^4 to
familiar MIL-STD-271, using standard y^-in. size on a cylindrical surface repre-
blocks containing simulated flaws in the senting 40 in.2 One must resort to a
form of flat-bottom holes as small as magnifying glass even to observe these
0.047 in. in diameter, and tiny magnetic indications before they
4. Transverse Ductility—as deter- can be rated.
mined from tensile bars removed from Microcleanliness—Microcleanliness ra-
both billet and forging. tings were compared on a statistical
Surveys were recently conducted of basis for the same heats studied for
data on each of these measures of magnaflux quality. All but one test
quality for several alloys in the high- specimen, representing only one end of
strength category. Data are presented one heat, failed to pass the stringent
in each of the succeeding sections for a worst field requirement of the following,
typical vacuum arc remelted alloy, which are based on ASTM E 45, Method
widely used in the missile field in the A.
form of rolled rings, rings for subsequent
A B C, D
flo-turning, hemispheres, and other
solid-fuel motor case components.2 Thin... 1.5 1.5 1.5 2.0
2 Heavy. 1.0 1.0 1.0 1.5
Over 50,000,000 Ib of this alloy, melted by
the vacuum-arc remelting practice,
ASTM have Int'lbeen
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rights Cleanliness—Ultrasonic
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HENNING ON HIGH-STRENGTH STEEL FORCINGS 151

testing is a standard production method disk-like and increasingly orientated


for nondestructively determining the parallel to the forging surface. Thus, the
cleanliness of steel used at the Ladish cleanliness of a steel as measured by
Co. Billet and forging cleanliness is ultrasonic inspection may appear to
compared with appropriate standard decrease with increasing reduction,
test blocks containing artificial dis- because the inclusions and other hetero-
continuities in the form of flat-bottom- geneities become increasingly favorable
drilled holes. Standards are ordinarily for detection. Essentially, the inclusions
based on the hole diameter. For example, do not increase in volume, but they do
the following standards are used fre- offer a more favorable surface for re-
quently: flecting ultrasonic waves. Indeed, if this
phenomena did not occur, the classical
Diameter of development of flow-line patterns paral-
Number Flat-Bottom
Hole, in. lel to the direction of maximum stress
8.
and directional control of maximum
%4
5. %4 forging strength and toughness would
3. %4 not be possible.
To further illustrate the improvements
Although the mathematical propor- in material quality, we have forged nearly
tions between these hole sizes appears to 3000 parts for the Minuteman missile
be small, a material being tested against program in the past several months.
a No. 3 standard is locating discontinui- Our internal rejection rate on these
ties about T the size detected at the forgings for defects traceable to raw
ultrasonic tuning level established with material was almost 4 per cent early in
a No. 8 block. Over three million pounds 1963. We have been able to reduce this
of the Ladish D-6ac alloy have been to the extent that only 2 forgings out
ultrasonically tested at a tuning level of the last 500, or 0.4 per cent, were
sufficient to detect a ^-in. flat-bottom- rejectable.
hole at both the billet and forging
stages. It is significant that over 99 VACUUM DEGASSING
per cent of this billet material passes Within the past year, we have checked
the industry-wide ultrasonic standard of the quality of both incoming billets and
a ^Vin. diameter FBH, and nearly 97 forgings made from vacuum-degassed
per cent passes the stringent ^-in. AISI4340, amounting to over 500,000 Ib.
diameter FBH standard. Tests include the standard magnaflux
However, these statistics do not imply cleanliness rating, ultrasonic testing, and
that 97 per cent of all die forgings will determination of transverse ductility.
pass the ^-in. standard. Review of die A summary of such tests follows:
forgings produced from large billets Magnaflux Cleanliness (as rated by
shows many of these involve very AMS-2301)—A total of 56 test bars
substantial reductions; for example, were rated. Frequency-Severity ratings
18-in.2 billet material is forged into large fell between 0.1/0.1 and 0.2/0.2 = 7,
hemispheres with a wall thickness of 0.05/0.05 and 0.1/0.1 = 8, and 0/0 and
less than 1-in. Whereas small inclusions 0.05/0.05 = 41. This distribution
in billet are often pencil-like and fre- represents metal that is substantially
quently tend to follow the billet axis, cleaner than the maximum F/S of ^
severe forging reductions reposition allowed by the AMS specification and is,
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by both to some extent, reflecting values at the
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152 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

lower end of the range for steels melted all vacuum-degassed material will show
by conventional electric furnace practice. this increased cleanliness. It has been
Ultrasonic Quality (As tested against our experience that the steels manu-
a ^j-in.-diameter, flat-bottom-hole factured using the vacuum carbon
Standard)—Ninety-seven per cent of deoxidizing technique yield the greatest
billet weight tested passes these strin- advantage over conventional air-melted
gent ultrasonic testing standards. When steel. Other vacuum-degassing tech-
all material is used to make 1500-lb niques reduce the tendency for the
closed die forgings, including that con- steel to flake but do not seem to neces-
taining ultrasonic indications of this sarily reduce the number of inclusions
size, 3 of approximately 100 forgings present.
failed to meet the standards. However,
once a correlation between billet and MARAGING STEELS
forging performance was established, The maraging steels have generated a
over 99 per cent passed the ultrasonic great deal of interest throughout the
requirements. industry because they offer a strength

TABLE 2—MECHANICAL PROPERTIES DETERMINED FROM HEMISPHERICAL


FORGING WEIGHING OVER 1000 LB.
Ultimate Yield Elongation, Reduction of Room Temperature
Strength, ksi Strength, ksi % Area, % Charpy Impact, ft-lb

AGED AFTER FORGING AT 900 F FOR 3 HR


297 to 303 289 to 294 6 to 8 29 to 42 10 to 14
SOLUTION TREATED 1 HR AT 1500 F, AGED 3 HR AT 900 F

297 to 300 287 to 292 7 to 8 34 to 40 10 to 13.5

Transverse Ductility—After testing capability approximately 12 per cent


over 200 forgings, each weighing in higher than the low-alloy martensitic
excess of 1500 Ib, the following distribu- steels. Will these steels be used ex-
tion of transverse ductilities was ob- tensively in die forgings? Possibly.
served : Let's look first at some of the advantages
and disadvantages.
Reduction of Area, % Per Cent of Values We read much about the high-strength
above 15 99.6
capability, for example, of the 18 per
above 20 97.0 cent nickel composition, for which the
above 25 83.0 published strength is proclaimed to be
in the vicinity of 300,000 psi. We also
This performance reflects considerably have been exposed to the .comment that
higher quality than that obtained from the alloy needs only a simple low-
conventional electric furnace air-cast temperature aging treatment after forg-
steels, where closer to 50 per cent of the ing or forming to develop this strength.
values are below 25 per cent. These statements are quite true for
Thus it can be seen that there are sheet, rod, and other rolled products that
significant advantages in specifying or receive uniform reduction during final
usingCopyright
vacuum-degassed
by ASTM Int'lmaterial.
(all rights An fabrication,
reserved); Mon Dec but what about
7 13:15:25 forgings?
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important point, however,
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HENNING ON HIGH-STRENGTH STEEL FORCINGS 153

shown that complex forging shapes do treatments, particularly on the proper-


not always lend themselves to the ties of the 18 per cent nickel grades.
uniform reduction necessary to achieve Some of our work with vacuum arc
uniform properties. We have observed remelted material has demonstrated that
mechanical properties on the 18 per cent the alloy can be worked at forging
nickel-cobalt (300) grade ranging as temperatures in the vicinity of 2150 F
follows: and subsequently heat treated to obtain,
Ultimate Yield Reduction
instead of low ductility, ductilities
Elonga-
Strength,
ksi
Strength,
ksi tion, % of Area, matching those obtained by the warm-
%
working cycles so often recommended.
270 to 300 260 to 290 2 to 8 5 to 42 The developed heat treatment cycle is
associated with approximately a 3 per
These values depend on the shape and cent drop in strength. As these treat-
size of forging and, more important, on ments develop, we find that the problems
the degree of deformation obtained in imposed by widely varying deformations
the lower forging temperature range of become less significant.
1500 to 1700 F. This does not mean that In conclusion, it is evident that the
uniform properties are not obtainable. future holds many challenges to the
In testing a large aft closure forging, forging industry in the area of high-
which received uniform deformation strength steels. The forging alloys chosen
during the final forging sequence, the for reliable production hardware will be
properties determined are given in those having the following qualifications:
Table 2, which shows the range of values (1) readily available from several sources,
to be quite narrow. This response reflects (2) characterized by processing require-
the uniform deformation imposed during ments that are relatively insensitive to
die forging in this case. the day-to-day variations encountered
The future for maraging steel forgings in normal processing operations, and
depends, in no small measure, upon the (3) capable of a high degree of uni-
levels of effective strength that de- formity from one mill source to the next
signers can reliably expect to obtain. and from one heat to the next.
The most useful and therefore practicable Although the subject of this paper
forging techniques are those which lend deals primarily with the state-of-the-art
themselves to a high degree of repro- of forging quality, it is important to
ducibility. In most forging shops this recognize that the majority of metal
means (1) forging at higher rather than failures can be attributed to factors other
impractically low temperatures, and (2) than defective steel. This report further
restricting designs to those characterized illustrates that the present day quality
by fairly uniform geometry. We have level is almost eliminating failure trace-
been exploring the effects of varying heat able to material quality.

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AUSFORM FABRICATION AND PROPERTIES OF
HIGH-STRENGTH ALLOY STEEL

BY W. W. GERBERICH,1 A. J. WILLIAMS,1 C. F. MARTIN,1 AND R. E. HEISE1

SYNOPSIS
The Ausform process has been developed for production applications to the
point that the strength, ductility, and toughness of commercially available
materials are improved by simply altering the order of conventional metal
processing.
Shear spinning is being used for Ausform fabrication of tubular components
such as missile cases with electron-beam welding being utilized to girth weld
head closures on finished cases. Electron-beam welding of steels in the Ausform-
strengthened condition proved successful with joint efficiencies of 90 per cent
obtained.
In addition to the investigation of fabrication techniques, a detailed study of
the crack propagation characteristics of ausformed steel is presented. A con-
siderable amount of fracture toughness data obtained from longitudinally rolled
specimens indicate that, for a commensurate yield strength, the toughness of
the ausformed steel is much greater than the corresponding conventionally-
treated material. For example, fracture toughness values well over 200 ksi \/in.
were attained for 250 ksi yield strength materials obtained by ausforming both
D6AC and a low-carbon modified H-l 1. Charpy V-notch impact data give simi-
lar results for both closed die and high-energy-rate forgings made of low-alloy
steels. With proper processing and alloying, toughness to strength 'ratios
greater than that obtainable with maraging steels is possible.

Materials with greater strength and strength increases. One answer to this
reliability are in demand for construction problem is the application of the Aus-
of missile and aircraft structural compo- form2 process, which increases the
nents. The strength levels obtained by strength and fracture resistance of cer-
conventional heat treatment of alloy tain alloy steels by simply altering the
steels are limited because ductility and order of conventional metal processing.
reliability generally decrease as the Until recently, strengthening of steel
1
has been accomplished by modifications
Senior research and development scientist, of alloy chemistry and heat treatment.
Applied Research Laboratory, supervisor of
Welding Section, Manufacturing Technology However, in 1954 Lips and Van Zuilen
Dept., supervisor of Process Metallurgy Section, (l)3 reported strengthening of steel by
Applied Research Laboratory, and product 2
engineer, Propulsion Product Dept., respec- U. S. Patent Number 2,934,463, April 26,
tively, Aeronutronic Division, Philco, a Sub- 1960.
3
sidiary of Ford Motor Co., Newport Beach, The boldface numbers in parentheses refer
Calif. to the list of references appended to this paper.
154
GERBERICH EX AL ON AUSFORM FABRICATION or ALLOY STEEL 155

deformation of austenite, which is main- austenite. As is seen in Fig. 1, a signifi-


tained in a metastable condition below cant processing variable is the amount of
its recrystallization temperature. Subse- plastic deformation, since yield strength
quent work by Gullotti, Eichen, and increases of 50 to 80 ksi may be achieved
Spretnak (2), Kula and Dhosi (3), Marsh- over a range of deformations from 35 to
call, Form, and Hehemann (4), Schmatz 65 per cent. It has been shown (9) that
and Zackay (5), and Grange and Mitchell strength is independent of the tempera-
(6), has shown that the strength of steel ture of deformation if the formation of
is increased by deformation of metastable nonmartensitic decomposition products
austenite. The most extensive work in can be avoided. The primary criterion for
this area has been done by Zackay (5,7), selection of an alloy steel for Ausform
Sernka (8), and Martin (9) and coworkers. processing is that the alloy be properly

FIG. 1—Mechanical Properties Versus Ausform Deformation.

This paper discusses fabrication tech- constituted to provide adequate process-


niques used in ausforming high-strength ing time without decomposition. This is
steel by sheet rolling, shear spinning, and realized by working in the bay that exists
forging. Electron beam welding methods between the transformation bands of
of joining ausformed steel are described. pearlite and bainite. The strong carbide-
To demonstrate the feasibility and forming elements, chromium, molyb-
reliability of ausformed and electron denum, and vanadium, as well as nickel,
beam-welded structures, the results of contribute largely to the stability of the
tension, impact, fracture toughness, and austenite in this region.
burst tests are presented. Alloy hardenability must also be con-
sidered in the selection of materials for
MATERIAL SELECTION Ausform strengthening. Critical cooling
The Ausform process is dependent on rates may be calculated using the method
the Copyright
plastic deformation
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156 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEEL

should be given for pearlite hardenability usual method of maintaining tempera-


of preforms and bainite hardenability of ture is to use an internally heated man-
finish formed sections. drel employing a resistance heater
arrangement. Radiation pyrometry is
FABRICATION used to monitor mandrel and work piece
Fabrication of ausformed parts may be temperatures.
accomplished by sheet rolling, rod roll-
ing, closed and open-die forging, high
energy rate forging, shear spinning,
extrusion, shock loading, or any other
deformation mode that can be applied
while steel is in the metastable austenitic
condition. Considerable work on aus-
formed steel deformed by rod rolling,
sheet rolling, and extrusion has been ac-
complished at the Ford Scientific Labora-
tory. At Aeronutronic, ausformed-
strengthened parts deformed by sheet
rolling, forging, and shear spinning have
been fabricated.
Sheet Rolling:
In order to ausform successfully by
sheet rolling, the preform must be cooled
rapidly enough from the austenitizing
temperature to miss the pearlite nose,
rolled quickly enough so that tempera-
tures do not drop into the bainitic region,
and quenched rapidly enough to form a
fully martensitic product. For small
laboratory mills of low capacity, auxilary
heating units must be provided to heat
the surface of the rolls to about 700 F, so
that nonmartensitic decomposition prod-
ucts are avoided. However, where
heavier reductions are possible, adiabatic
heating may be considerable, and tem-
perature stabilization between passes
may require time to let the material cool. FIG. 2—Ausform Shear Spin Cylinder and
Original Preform.
Shear Spinning:
Ausform processing may also be per- After the desired deformation is ac-
formed utilizing shear spinning as the complished, the part is quenched on the
deformation mode. As previously de- mandrel. This practice serves as a re-
scribed, the work piece must be main- straint to distortion. After the Ms is
tained at a temperature within the reached, a transformation expansion
metastable austenitic region of the overrides thermal7 contraction
Copyright by ASTM Int'l (all rights reserved); Mon Dec
and frees
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isothermal transformation
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GERBERICH ET AL ON AUSFORM FABRICATION OF ALLOY STEEL 157

stripping. An example of a preform and within required manufacturing tolerances


the resulting 8-ft-long ausformed cylin- since straightening of fully strengthened
der is shown in Fig. 2. parts is not practicable.
Electron beam welding has many ad-
Forging: vantages and is supplanting tungsten arc
The feasibility of conventional ham- inert gas welding and other joining proc-
mer forging techniques, using both open esses for fabricating many high-strength
and closed-die techniques, has been steel components. One major advantage
demonstrated. Standard forging prac- of electron beam welding is the high
tices were varied only by deforming at X ray quality of the welds made at a low
approximately 1000 F. Ausformed com- total heat input. The welds deposited in a
ponents have been made from various vacuum have a much lower level of ab-
alloy steels (4340, D6-AC, etc.) with the
influence of amount of Ausform deforma-
tion and anistropy evaluated. Preforms
after austenitizing were stabilized at
1000 F in a molten salt bath, then forged,
quenched, and tempered.
Also of interest is the feasibility of
using high-strain rate processes for defor-
mation of metastable austenite. The
recently developed high-energy rate
forge methods are of particular interest.
The high-energy rate forge process has
been applied to ausforming to demon-
strate the feasibility of this approach.
Ausform reductions of 50 per cent in a
single blow and 75 per cent in two blows
were realized on 3-in.-diameter, 2-in.-
thick blanks. A U.S. Industries Hermes
FIG. 3—Light Macrograph and Micrographs
Model 2600B forge press was used for the of Electron Beam Weld in D6-AC Alloy Aus-
experimental forging work. formed 75 Per Cent.

JOINING sorbed gases which may be detrimental to


Ausform fabrication requires that physical properties. The extremely nar-
welding be done on fully hardened mate- row weld deposited at a high welding
rial. This presents a challenge since any speed permits joining of heat-treated,
excessive welding heat would soften the finish-machined parts with minimum de-
base metal adjacent to the weld. There- terioration of base metal properties.
fore, the welding procedures must be Heavy fixturing is not needed in electron
designed to reduce heat-affected zones to beam welding since weld shrinkage
a minimum. Butt welds must be depos- stresses and distortion are minor.
ited with as narrow a weld bead as In contrast to tungsten arc welding of
practicable. Welding of attachments to high-strength steels where an over-
ausformed motor cases, for example, heated coarse grain structure will result,
must be done with a minimum of pene- an electron beam weld has a narrow zone
tration into the
Copyright shell material.
by ASTM Distortion
Int'l (all rights with
reserved); Mon Deca 7desirable fine2015
13:15:25 EST grain structure, as
due Downloaded/printed
to welding must by be maintained illustrated in Fig. 3. The weld was made
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158 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEEL

(a) TUNGSTEN ARC INERT GAS (TIG) WELD

(b) ELECTRON BEAM WELD


FIG. 4—Knoop Hardness Traverse of Welds in ^-In.-Thick D6-AC Alloy Steel Ausformed 75 Per
Cent and Double Tempered at 900 F.

in 0.5-in.-thick Ladish D6-AC steel aus- formed D6-AC forgings are illustrated in
formed by forging before welding and Fig. 4. The superiority of the electron
retempered at 900 F after welding. The beam process is evidenced by the ex-
fine grain structure is attributed to the tremely narrow weld and heat-affected
rapid heating and cooling rate achieved zone.
in the electron beam process. MATERIAL PROPERTIES
Microhardness traverses of tungsten
arc and electron beam welds were made Tensile Data:
to establish the extent of the heat- In evaluating the ausformed material
affected areas. The results of traverses on fabricated by sheet-rolling, standard
Copyright
the welds in by
theASTM
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thickness of reserved); Mon Dec tension
aus- 8-in.-long 7 13:15:25 EST 2015
specimens with 0.5-in.-
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GERBERICH ET AL ON AUSFORM FABRICATION or ALLOY STEEL 159

wide by 2-in.-long gage sections were Mechanical properties of D6-AC aus-


utilized. For the forged material, 0.125 formed by sheet-rolling were determined
in. and 0.250-in.-diameter rounds with as a function of tempering temperature
1-in. gage lengths were used. Both flats and compared to the conventional heat
and rounds were pulled at a constant treatment. The composition of this
cross head rate of 0.010 in./min. Load- D6-AC heat appears in Table 1. Conven-
TABLE 1—COMPOSITION OF MATERIALS, PER CENT.
Material C Mn P S Si Ni Cr Mo V

Ladish D6-AC sheet rolled 0.42 0.72 0.006 0.009 0.22 0.63 1.05 0.94 0.08
Ladish D6 AC forged 0 45 0 70 0.008 0.007 0 22 0 59 1 08 1 00 0 06
4340 air melt 0.39 0.76 0.009 0.018 0.31 1.80 0.79 0 27
H-ll vacuum melt 0.41 0.24 0.012 0.006 1.00 5 12 1 39 0 49
X-2 vacuum melt 0.23 0.24 0.016 0.004 0.96 4 86 1 20 0 51

FIG. 5—Strength of Conventional and Ausformed Ladish D6-AC as a Function of Tempering


Temperature.

deformation curves recorded from 1 and ventionally treated and ausformed mate-
2-in. gage length extensometers were rials were austenitized at 1650 F, the
used to determine the 0.2 per cent offset latter being deformed 50 per cent prior
yield strengths at room temperature. At to oil quenching. All specimens were
low test temperatures, accurate recording double tempered 2-hr per temper. As is
of the crosshead travel utilizing a differ- seen in Fig. 5, the yield or ultimate
ential transformer was sufficient to deter- strength of the ausformed Ladish D6-AC
mine the 0.2 per cent offset yield is consistently 50 ksi higher than the
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
strengths. conventional material. For the 1000-F
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160 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEEL

FIG. 6—Strength of 100 of Tempered Conventional and Ausformed Ladish D6-AC as a Function
of Test Temperature.

FIG. 7—Yield Strength as a Function of Tempering Temperature for Vacuum-Melt H-ll and
X-2 inCopyright
the Conventional
by ASTM andInt'l
Ausformed Conditions.
(all rights reserved); Mon Dec 7 13:15:25 EST 2015
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GERBERICH ET AL ON AUSFORM FABRICATION OF ALLOY STEEL 161

tempered conditions, tension tests at both conventional and ausformed mate-


temperatures to —200 F were conducted. rials are shown for various tempering
In Fig. 6, it is seen that the slopes of the temperatures between 600 and 1150 F.
yield and ultimate strength versus tem- Double 2-hr tempers were utilized except
perature curves are linear and very for the conventionally heat treated H-ll
similar. (11) where triple 3-hr tempers were used.
Ausform sheet-rolling was also per- For the H-ll material, the ausformed
formed at H-ll, and a low carbon specimens have yield strengths about 70

FIG. 8—Ductility of Conventional and Ausformed Low-Alloy Steels as a Function of Yield


Strength.

modification of it, X-2, the compositions ksi higher than the conventionally proc-
of which are given in Table 1. These con- essed ones at all tempering temperatures.
sumable electrode-melt materials were For the X-2 alloy, at the 600 F temper
austenitized at 1900 F, the conventional there was a spread of about 110 ksi in the
ones being air quenched and the aus- yield strengths of the conventional and
formed ones being oil quenched after 65 ausformed materials, while at the 1100-F
per cent deformation in the bay. The temper, this spread decreased to about
ausformed sheets were rolled by a steel 45 ksi. An interesting observation is that,
producer using conventional mill equip- for the higher tempering temperatures,
ment.Copyright
In Fig.by7,ASTM
the yield strengths
Int'l (all of the Mon
rights reserved); yieldDecstrengths
7 13:15:25 ESTconventional
of the 2015
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162 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEEL

and ausformed X-2 approached those counterpart had a reduction of area of


for the corresponding treatments of 0.40 53 per cent. Meanwhile this increase in
carbon H-ll. ductility was accompanied by an increase
In addition to the effect of strengthen- in the yield strength of about 45 ksi.
ing of sheet-rolled materials, the in- Data from round bar tension speci-
fluence of ausforming upon the ductility mens were obtained on samples taken
of the resulting structure is extremely from both closed-die forgings of 4340 and

TABLE 2—TENSILE PROPERTIES OF FORGED 4340 AND LADISH D6-AC.


0.2% Ultimate Reduc- Elonga-
Material Process Condition0 Yield Stress, tion of tion in 1
Stress, ksi Area, %
ksi In., %

[conventional 400 F 215 275 18.4 8.0


4340 •j closed -die temper 214 285 18.4 9.0
(forging longitudinal 213 283 17.2 8.0

4340 fausformed 55% 400 F temper 278 315 45.5 5.0


\closed-die forging longitudinal 271 291 52.0 6.0
fausformed 55% 400 F 241 319 8.1 5.0
4340 i closed -die temper 241 315 8.1 5.0
[forging transverse 250 315 9.8 5.0
(conventional 850 F 182 198 30.8 11.0
4340 closed-die temper 181 198 30.0 10.0
forging longitudinal 183 195 28.2 10.0
fausformed 55% 850 F 225 231 41.5 7.0
4340 •j closed-die temper 229 233 43.9 5.0
(forging longitudinal 228 233 44.7 7.0
fauformed 55% 850 F 212 217 24.4 6.0
4340 j closed-die temper 212 218 24.4 6.0
(forging transverse 211 226 24.4 7.0
fausformed 50% 1000 F 247 257 22.6 9.0
Ladish D6-AC •s high energy rate temper 253 262 29.4 9.0
(forging random 248 259 22.6 10.0
fausformed 75% 1000 F 273 281 28.2 9.0
Ladish D6-AC •j high energy rate temper 268 277 22.6 8.0
[forging random 268 276 32.1 10.0
0
All tempering temperatures 2 + 2 hr.

important. Reduction of area versus high energy-rate forgings of Ladish


yield strength is shown in Fig. 8 for the D6-AC, the compositions of which are
X-2 and Ladish D6-AC alloys. It is seen shown in Table 1. A comparison of con-
that the effect of ausforming is to main- ventionally forged 4340 and 4340 aus-
tain ductility while increasing the formed 55 per cent by forging is made in
strength of the material. Actually, for Table 2 for material tempered at 400 F
the X-2 material, there was a slight in- and 850 F. For a particular tempered
crease in ductility with ausforming. For condition, the increase of the yield
example, the conventional material strength or tensile strength by ausform-
tempered at 1100 F had a reduction of ing was about 30 to 50 ksi. Although
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
area Downloaded/printed
of 40 per cent, while
by
its ausformed there was only a slight, directionality
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GERBERICH ET AL ON AUSFORM FABRICATION or ALLOY STEEL 163

effect on the strength properties, there the joining of fabricated parts. As dis-
was a considerable effect on the ductility cussed above, the electron beam welding
as indicated by reduction of area. In con- process offers the most advantages for
trast to this, ausforming of Ladish the joining of ausformed materials. To
D6-AC by high-energy rate forging tech- determine joint efficiencies, samples were
niques minimized directionality effects. taken from pancake forgings of Ladish
Even though the disk forgings were D6-AC 0.5-in.-thick and electron beam
formed by radial flow, severe direction- butt-welded together. The only post

TABLE 3—TENSILE PROPERTIES OF ELECTRON BEAM WELDED D6-AC


PANCAKE FORGINGS TEMPERED AT 900 F
1D.2% Yield Ultimate Reduc- Elonga- Location Joint"
Condition Stress, Stress, tion of tion in 1 of Efficiency,
ksi ksi Area, % In., % Fracture %

(222 244 32 11
Conventional base metal \221 243 35 11
(220 243 35 11

(217 237 17 5 weld 97


Conventional transverse e.b. weld 1215 237 18 6 weld 97
(216 238 15 5 weld 98
(220 238 21 7 weld 98
(261 278 17 6
Ausformed 50%) base metal J264 281 19 6
(261 277 20 6
(237 249 15 4 weld 89
Ausformed 50% transverse e.b. weld
J236 245 12 3 weld 88
1235 247 18 5 weld 88
[236 248 12 3 weld 89
(281 293 26 8
Ausformed 75% base metal \282 296 22 8
[277 293 14 7

(241 252 12 3 weld 86


Ausformed 75% transverse e.b. weld
J243 249 15 3 weld 84
1241 253 15 3 weld 86
[241 242 15 3 weld 82
0
Per cent joint efficiency = transverse weld ultimate strength/average base metal ultimate
strength X 100.

ality in the radial direction was not noted welding heat treatment was a 2-hr 900 F
except at the periphery of the forging. temper which was the same as the
Tension specimens taken at random indi- original tempering temperature. As is
cate uniform strength and ductility seen in Table 3, joint efficiencies of about
characteristics as seen in Table 2. For the 97 per cent were obtained in the conven-
material ausformed 75 per cent, a yield tional structures while they were about
strength of about 270 ksi was obtained, 85 to 88 per cent in the ausformed struc-
which is quite high for Ladish D6-AC tures. This retention of strength must be
tempered at 1000 F. attributed to the rapid heating and
Since the tensile properties of the aus- cooling conditions which do not allow
formed steels are desirable for certain sufficient time for gross diffusion to occur.
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
applications, consideration was given to Even though the joint efficiencies of the
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164 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEEL

ausformed steels were lower, higher development work on ausformed steel


residual strengths were observed. As has been concerned with obtaining high
might be expected, joint efficiencies for strengths without due attention to the
ausformed 0.060-in.-thick D6-AC taken resistance to crack propagation. Thus, it
from shear spun material were higher was deemed necessary to consider the

FIG. 9—Impact Data on Forged 4340 and Ladish D6-AC.

than those for the 0.5-in.-thick material impact and fracture characteristics of
and will be discussed later. ausformed materials in the optimization
Assuming that the feasibility of of properties.
strengthening and joining has been
adequately demonstrated, it is pertinent Impact Data:
to question
Copyright the
by reliability
ASTM Int'lof any
(all aus-
rights To determine
reserved); Mon Dec impact properties,
7 13:15:25 EST 2015
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formed structure. Muchbyof the previous standard Charpy V-notch specimens
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GERBERICH ET AL ON AUSFORM FABRICATION OF ALLOY STEEL 165

were ground from heat-treated, closed- ausformed condition. For any test tem-
die and high-energy rate forgings. Speci- perature, the impact energy of the aus-
men preparation and test procedures formed material was about 6 ft.-lb higher
conformed with the specifications of than the conventionally treated material.
Watertown Arsenal (12). As seen in Fig. 9, Tempering the ausformed 4340 at 850 F

FIG. 10—Fracture Toughness and Per Cent Shear-Lip as a Function of Test Temperature for
Ladish D6-AC.

impact energies are reported for 4340 and produced a somewhat tougher material,
D6-AC as a function of test temperatures as indicated in Fig. 9. For the yield
ranging from —320 to 200 F. Data strength range of 230 to 270 ksi, the low
points represent averages of two, in most temperature toughness of the ausformed
cases three, and in some instances six 4340 was high with impact energy levels
impact tests. It is seen that the properties of 12 to 15 ft-lb persisting to about
of the closed-die
Copyright forged
by ASTM 4340
Int'l (all reserved); Mon-200F.
rightstempered Dec 7 13:15:25 EST 2015
at 400 F are considerably
Downloaded/printed by better in the Impact properties on D6-AC obtained
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166 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEEL

from high-energy rate forgings were estimate was made at a distance of two
similar to the 4340 data at — 40 F but thicknesses in from the plate edges from
increased to about 27 ft-lb at room which a KcS estimate of fracture tough-
temperature. Even though the reduction ness was made.
of area values for the high-energy rate Fracture toughness of 0.060-in.-thick
forged D6-AC are consistently lower than D6-AC tempered at 1000 F is shown for
the longitudinal specimens of closed-die various test temperatures in Fig. 10.
forged 4340 at the same yield strength In this condition the ausformed material
level, the impact energies are consider- has a 250 ksi yield strength while the
ably higher at room temperature. An- conventionally treated alloy has a 200
other consideration is that all of the ksi yield strength. Fracture toughness
closed-die forging impact specimens of the ausformed material at room
were taken in the longitudinal direction, temperature was about 220 ksi \/in!
while those from the high-energy rate which was slightly higher than that
forgings were taken at random. Also, it obtained from conventional Ladish
should be pointed out that scatter in the D6-AC. Even though the transition
impact data was excessive in a few in- temperature for the ausformed material
stances for the closed-die forgings and was about 40 F higher than the con-
less than 20 per cent in all cases for ventional condition, at temperatures
the high-energy rate forgings. A more below — 100 F the toughness of the
quantitative criterion for reliability, ausformed steel was much greater, being
especially for thin sections, is the fracture well over 100 ksi Vim to -250 F. Also,
toughness evaluation as proposed by Fig. 10 shows that the per cent shear-lip
Irwin et al (13). in fracture was consistently higher for the
Fracture Toughness Data: ausformed material than for the con-
ventionally heat-treated material at all
Standard ASTM recommended (13) test temperatures. Using Irwin's (13)
specimens 3 in. wide by 12 in. long with plasticity correction and considering the
1-in. center slots were used for all fracture gross stress, <TQ , to be equal to the yield
toughness, Kc, evaluations. Most slots strength it can be shown that in order to
were machined by the electrical discharge avoid premature failure of a pressure
process to produce notch root radii vessel,
^0.001 in. Several specimens were
subsequently subjected to a tension-
tension fatigue cycle until the crack front where a is the half-crack length of any
had propagated several hundredths of an flaw at failure. Furthermore, assuming
inch at both ends of the center slot. that any flaw would grow under plane-
Specimens were loaded at a load rate of strain conditions to about two times the
approximately 5000 Ib/min. In most thickness of the material, the failure
instances, stiffener plates were used in condition becomes
the grip area to prevent lateral buckling.
However, in several cases when the
gross stresses' were excessively large, where B is the thickness of the material.
doublers were welded on both sides of For a 0.060-in.-thick pressure vessel of
the loading pin holes. To measure the D6-AC, the ratio of fracture toughness to
slow crack propagation, the ink method yield strength should be about 0.62 to
was used at room
Copyright temperature.
by ASTM reserved);satisfy
At lower
Int'l (all rights Mon DecEq 7 2. This EST
13:15:25 condition
2015 is easily
temperatures, a perby cent shear-lip fulfilled by the 250,000 psi yield strength
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GERBERICH ET AL ON AUSFORM FABRICATION or ALLOY STEEL 167

ausformed material at room temperature ratio would have to be about 0.8. Thus,
but becomes marginal below —40 F. For the ausformed H-ll material could not
the conventionally treated material, at a be reliably used over the 225 ksi yield
yield strength of 200,000 psi, this condi- strength level for pressure vessel applica-
tion is fulfilled for temperatures some- tions.
what below — 80 F. For the ausformed X-2 alloy, it is
An investigation was also made into seen in Fig. 11 that the fracture re-
the fracture properties of O.lO-in.-thick sistance, Kc/<TyS, is well over 0.8 for all
H-ll and X-2 alloys. A fracture re- yield strength levels from 235 to 270 ksi.

FIG. 11—Fracture Toughness Comparison for Vacuum-Melt H-ll and X-2 as a Function of
Yield Strength.

sistance parameter, Kc/<rys, is shown as a Gross section stresses over 150 ksi and
function of yield strength in Fig. 11 for net section stresses on the order of 300
conventional H-ll, ausformed H-ll and ksi were realized for the ausformed X-2
ausformed X-2. Even though the con- tempered at 1000 to 1100 F.
ventional H-ll data are taken from For the 100Q-F tempered condition,
Rawe (13), identical specimens and test with a yield strength of 250 ksi and a
procedures were used to determine tensile strength of 300 ksi, several
fracture toughness. It is seen that for a specimens were fatigue cracked and
particular fracture resistance level, the subsequently tested for fracture tough-
yield strength of H-ll may be increased ness. As is seen in Fig. 11, both eloxed
about 20 to 50 ksi by ausforming. Con- and fatigue-cracked specimens indicated
sidering the by
Copyright fracture criterion
ASTM Int'l (all rightsin,reserved);
Eq 2 Mon similar
Dec 7 values
13:15:25of Kc2015
EST /<rvs for this condi-
for Downloaded/printed
O.lO-in.-thick material
by the K c /<r ys tion and represents a fracture toughness
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168 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEEL

level of about 400 ksi \/\n. These ex- were obtained with the ausformed X-2, it
ceptionally high values of fracture is appropriate to compare this to the
toughness were calculated from Irwin's 18Ni (250 and 300 ksi grades) maraging
fracture toughness equation steels (15). A toughness comparison is
made utilizing the net section stress at
failure in a fracture toughness test. As
shown in Fig. 12, the value neof t/a-y<T
S is
higher for the ausformed X-2 at any
where the term in the brackets is denned particular yield strength. One further
(13) as q and is determined from a graphi- set of fatigue-cracked specimens of the
cal representation of (tro/W)2 versus 1000-F tempered condition were run at

FIG. 12—Fracture Toughness Comparison of Ausformed X-2 and Maraging Steels.

ira/W for constant values of q. One of several low temperatures to —100 F.


the authors (14) has extended the numeri- Preliminary data indicated that the
cal solution of Eq 3 to larger values of fracture toughness of ausformed X-2 was
q so that any combination of ira/W and about 210 ksi \/'m. and the fracture
(0"oAj/*)2 may be used to solve for Kc as appearance was 70 per cent shear at
long as the upper limit of the analysis is -40F.
not violated. For the ausformed X-2 Thus far, the strength, joining, and
material tempered at 1050 and 1100 F, reliability characteristics of several
the upper limit of the fracture toughness ausformed steels have been considered
equations is exceeded, as noted by the separately. It is pertinent to question
arrows in Fig. 11. what effect a weld might have on the
Copyright
Since by ASTMhigh
exceptionally Int'l combinations
(all rights reserved);reliability
Mon Dec of7 13:15:25 EST 2015
a fabricated structure. In
Downloaded/printed
of fracture by yield strength
toughness and order to illuminate this, .several tests were
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GERBERICH EX AL ON AUSFORM FABRICATION OF ALLOY STEEL 169

run on electron beam-welded ausformed about 180 ksi \/'m. is obtained in the
Ladish D6-AC. In Table 4, it is seen that welds for both tempered conditions.
joint efficiencies of 94 per cent were Since specimens were taken from large
obtained in material tempered at 1000 diameter shear-spun material, fracture
and 1075 F. Eloxed cracks were ma- toughness of both base metal and welds

TABLE 4—TENSILE AND FRACTURE TOUGHNESS PROPERTIES OF


ELECTRON-BEAM WELDED AND BASE METAL LADISH D6-AC.
0.2% Fracture Net
Yield Ultimate Gross" Crack Tough- Section Shear-
Condition and Temper Stress, Stress, Stress Length ness Kg , Stress
ksi6 a a , ksi 2a, in. lip, %
ksi ksi\/inT »net , ksi

97.0 1.57 191 203 100


Ausformed 1000 F 260.6 262.7 106.5 1.55 214 224 100
92.5 1.27 155 173 100
Ausformed e.b. welded 1000 F . . 242.8 248.9 104.0 1.46 194 196 100
107.5 1.32 187 191 100
121C 1.54 250 239 100
Ausformed 1075 F 247.0 248.6 >102
98.0 1.32 177 200 100
Ausformed e.b. welded 1075 F. . 227.1 234.7 91.5 1.48 188 209 100
101.0 1.37 179 181 100
0
Gross stress of center-cracked to £- to 3-in.-wide specimens.
6
Joint efficiencies are approximately 94 per cent.
e
Fractured in loading pin holes.

FIG. 13—Burst-Tested Cylinders of Ausformed D6-AC Steel.

chined so that the crack tips were as should be representative of a fabricated


nearly in the center of the weld as cylinder. These toughness levels would
possible. In all cases the crack propaga- be more than sufficient to avoid pre-
tion was entirely in the weld material mature failure in a pressure vessel with
and 100 per cent shear failures were girth welds.
observed. Also shown in Table 4 are the
fracture toughness values for both base Burst Tests:
metal and by
Copyright as-welded
ASTM Int'lconditions. Two7 13:15:25
It is Mon Dec
(all rights reserved); methodsESThave
2015 been used to
seenDownloaded/printed
that a fracturebytoughness level of evaluate the Ausform properties in shear
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170 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEEL

spun cylinders; these are ring tests and 2. Yield and ultimate strengths of
closed-end pressure vessels. Rings cut low-alloy steels may be increased by 40
from cylinders are tested with unre- to 100 ksi with ausform deformations
strained ends using o-ring seals to main- ranging from 50 to 65 per cent.
tain internal pressurization. The results 3. Impact properties of 12 to 15 ft-lb
of these tests duplicate previously deter- for 4340 steel ausformed by closed die
mined uniaxial tensile data with slightly forging are retained to —200 F for yield
lower total strain indicated. strengths of 225 to 275 ksi.
The closed-end pressure vessel is 4. High-energy rate ausformed forg-
subjected to a biaxial stress condition in ings of D6-AC with yield strengths of
an approximate 2:1 ratio even though 270 ksi developed impact energies of
flat plates were used to hold pressure. 27 ft-lb at room temperature.
The test results for the specimens shown 5. Two ausformed alloy steels, D6-AC
in Fig. 13 were 292 ksi yield strength and and X-2, had fracture toughness values
311 ksi burst strength; uniaxial yield ranging from 220 ksi to 400 ksi \/m.
strength of the D6-AC material with for yield strengths of 235 to 270 ksi and
the same Ausform reduction is 262 ksi. tensile strengths of 260 to 300 ksi.
In summary, it has been indicated that 6. Net section failure stresses of the
ausformed materials have high strength, ausformed X-2 alloy were higher than
may be adequately joined by electron the 18Ni maraging steels for equivalent
beam welding, and have sufficient tough- yield strengths.
ness to make a reliable fabricated struc- 7. Joining of ausformed material by
ture. This technology is currently being the electron beam welding process
extended to the fabrication of high- results in joint efficiencies of 85 to 95
strength rocket motor case hardware. per cent depending upon material thick-
Further work on alloy processing and ness.
composition and their effect on properties 8. Fracture toughness values of aus-
of ausformed steels, as affected by low formed D6-AC with a yield strength of
temperature, directionality, and welding
250 ksi butt-welded by the electron beam
parameters, are being conducted to
extend the range of useful application. process were about 180 ksi \/in. with
100 per cent shear fracture.
CONCLUSIONS 9. Burst tests of D6-AC cylinders
1. Ausforming has been accomplished ausformed by shear spinning have re-
by sheet rolling, forging, and shear sulted in biaxial yield strengths of over
spinning. 290 ksi and 100 per cent shear fracture.

REFERENCES
(1) E. M. H. Lips and H. Van Zuilen, "Im- the Mechanical Properties of 4340 Steel,"
proved Hardening Technique," Metal Transactions, American Society for Metals,
Progress, August, 1954, pp. 103-104. 1960, p. 52.
(2) D. Gullotti, E. Eichen, and N. J. Spretnak, (4) C. W. Marschall, G. W. Form, and R. F.
"Development of New Mechanisms and Hehemann, "An Investigation of Special
Techniques for Obtaining Steels in the Treatment for Developing High Toughness
Ultra-High Strength Range," Wright Air in Ultra-High Strength Steels," Watertown
Development Command-TR-56-555, May, Arsenal Laboratory Report .310/214, AD
1957. 211011, November, 1958.
Copyright
(3) E. B. Kulaby andASTM
J. M.Int'l (all "Effect
Dhosi, rights reserved);
of (5) Mon
D. J.Dec 7 13:15:25
Schmatz and V.EST 2015
F. Zackay, "Me-
Downloaded/printed
Deformation Prior to by
Transformation on chanical Properties of Deformed Metast-
University of Washington (University of Washington) pursuant to License Agreement. No further r
GERBERICH ET AL ON AUSFORM FABRICATION OF ALLOY STEEL 171
able Austenitic Ultra-High Strength Steel," Constant Temperature," Transactions,
Transactions, American Society for Metals, American Society for Metals, 1941, p. 29.
1959, p. 51. (11) R. Rawe, "Recalculation of Fracture
(6) R. A. Grange and J. B. Mitchell, "Some Toughness Data," Report No. M-2003,
Effects of Deforming Austenite Below its Aerojet-General Corp., February, 1960,
Recrystallization Temperature," United (12) D. E. Driscoll, "Calibration of the Charpy
States Steel Corp., Report No. 833, July, Impact Machine and Procedure for Inspec-
1959. tion and Testing of Charpy V-Notch Im-
(7) J. C. Shyne, V. F. Zackay, and D. J. pact Specimens," Watertown Arsenal,
Schmatz, "The Strength of Martensite November, 1958.
Formed from Cold-Worked Austenite," (13) "Fracture Testing of High-Strength Sheet
American Society for Metals, Preprint 163, Materials," A Report of a Special ASTM
Vol. 53, 1960. Committee, ASTM Bulletin 243, January,
(8) R. P. Sernka, R. E. Heise, and S. T. Ross, 1960, p. 29; ASTM Bulletin 244, February,
"Ausform Processing of Steel by Forging," 1960, p. 18.
Aeronautical Systems Division Technical (14) W. W. Gerberich, "Theoretical and Prac-
Documentary Report No. ASD-TR-61-428, tical Aspects of Correlating Percent Shear-
March, 1962. Lip to Relative Plastic Zone Size in Brittle
(9) C. F. Martin, W. W. Gerberich, J. M. Fracture," Jet Propulsion Laboratory,
McCamont, and E. L. Harmon, "Research California Institute of Technology, T.R.
in the Mechanism of Strengthening in 32-112, September, 1962.
Ausformed Steel," ASD Technical Docu- (15) R. W. Krohn and O. A. Siede, "Research
mentary Report No. ASD-TDR-62-692, on the Binary Iron-Nickel Alloys with
February, 1962. 20-25% Nickel," Progress Reports on
(10) R. A. Grange and J. M. Kiefer, "Transfor- Contract AF 33(616)-8018, Curtis-Wright
mation of Austenite on Continuous Cooling Corporation, Wood-Ridge, New Jersey,
and its Relationship to Transformation at 1961-1962.

Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
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THERMOMECHANICAL TREATMENTS APPLIED TO
ULTRAHIGH-STRENGTH BAINITES
BY D. KALiSH,1 S. A. KuLiN,2 AND M. COHEN1

SYNOPSIS
The mechanical properties of Hll and AISI 4350 steels were determined for
a series of bainites formed from both deformed and undeformed austenites.
These bainites were also subjected to subsequent straining and tempering treat-
ments. Similar thermomechanical treatments involving martensite as the essen-
tial transformation product were included for comparison purposes.
Fifty per cent austenite deformation in Hll results in considerable strength-
ening of the subsequently formed bainite. Hll in the bainitic condition, formed
from either deformed or undeformed austenite, is strongly affected by refrigera-
tion in liquid nitrogen, owing to conversion of retained austenite when temper-
ing temperatures below 1000 F are employed. In both cases, a large secondary
strengthening is observed on tempering between 1000 and 1100 F. This results
in higher strengths and equivalent ductilities as compared to the correspond-
ingly treated martensites. Austenite deformation in 4350 has little effect on the
strength of the subsequently formed bainite, although such deformation does
enhance the strength of martensite.
HI 1 and 4350 bainites and martensites exhibit a large response to strain-tem-
pering treatments. For both steels, small deformations (up to 3 per cent) pro-
duce large strengthening effects. Yield strengths close to 400,000 psi have been
obtained by the application of strain-tempering treatments (50 per cent defor-
mation) to both Hll martensite and bainite. Increasing the carbon content in
43XX steels enhances the strengthening response to strain-tempering.
The increments in strength developed by deformation processes, both before
and after transformation to either bainite or martensite, are found to be ap-
proximately additive when the individual processes are combined.
Significant improvements in the and experimental steels. In addition,
strength of low-alloy steels have been straining and subsequent tempering of
achieved by the application of mechan- as-quenched or tempered martensite can
ical deformation either before or after also lead to exceptionally high strength
the formation of martensite. Ausforming, levels. The reported ductility and re-
the deformation of austenite prior to sistance to brittle fracture at these im-
transformation into martensite, has been proved strength levels have, in general,
shown to develop yield strengths over been equal to or less than that developed
300,000 psi in a number of commercial by the conventional heat treatment.
1
Instructor and professor, respectively, De- In the search for methods to improve
partment of Metallurgy, Massachusetts Insti- the strength, and possibly the ductility
tute8 of Technology, Cambridge, Mass. and fracture toughness of low-alloy steels,
Project director, ManLabs, Inc., Cambridge.
Mass. the utilization of bainitic structures
172
KALISH ET AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 173

TABLE 1—CHEMICAL COMPOSITIONS.


Element, %
Steel
c Mn Si Cr Mo Ni V p s
Hll. 0.39 0.25 1.00 5.25 1.39 0.54 0.111 0.007
4350. 0.52 0.65 0.22 0.88 0.26 1.82 0.008 0.006

(a) Hll
(6) 4350
FIG. 1—Isothermal Transformation Diagrams.

in conjunction with thermomechanical response of certain low-alloy steels to


treatments should not be overlooked, thermomechanical treatments involving
Copyright bythe
Accordingly, ASTM Int'l objective
primary (all rights reserved);
of the Mon Dec 7 13:15:25
transformation EST 2015These proc-
to bainites.
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present investigation is to evaluate the esses involve deformation of the steels
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174 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

(a) 500 F
(5) 550 F
(c) GOOF
(d) 650F
Etchant—modified picral.
FIG. 2—Light Micrographs of Hll Bainite Transformed for 4 hr (X1500).

either before or after the bainitic reac- the following considerations: (1) the com-
tion. The parameters measured are positions are such that the steels may be
strength, ductility, and fracture tough- deformed as metastable austenite and
ness. then transformed to bainite, (2) the
tempering behaviors of the alloys in the
MATERIALS AND TRANSFORMATION conventionally heat-treated condition are
CHARACTERISTICS well denned, and (3) the influence of
Alloy Selection: thermomechanical treatments involving
the martensitic reaction has previously
The low-alloy
Copyright steelsInt'l
by ASTM studied in this
(all rights in- Mon
reserved); beenDecstudied (1-5)
7 13:15:25 EST.3 Two
2015 low-alloy steels
vestigation are listed byin Table 1. These
Downloaded/printed 3
The boldface numbers in parentheses refer
materials were
University selected on
of Washington the basis
(University of to thepursuant
of Washington) list of references
to Licenseappended to No
Agreement. thisfurther
paper.reproductions
KALISH EX AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 175

(a) 500 F
(6) 550 F
(c) 600 F
(d) 650 F
Plastic replicas shadowed. Etchant—modified picral.
FIG. 3—Electron Micrographs of Hll Bainite Transformed for 4 hr (X15.000).

that meet these requirements are Hll The steels were obtained as consuma-
and AISI 4340. Results obtained in a ble-electrode, vacuum-melted 2-in.-wide
preliminary investigation of Hll sug- strip in two thicknesses, 0.250 and 0.140
gested that further study of this steel in. The thicker stock was used for experi-
would be fruitful. It was also decided that ments involving deformations of more
AISI 4350 would be more desirable than than 20 per cent reduction.
AISI 4340 for present purposes because
the additional carbon provides a lower Transformation Characteristics:
Ms temperature and Int'l
Copyright by ASTM thus(all
a wider range MonExperimental
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EST 2015
of high-strength bainites
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withUniversity
the lower carbon material.
of Washington on the
(University of Washington) transformation
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No further
176 STRUCTURE AND PROPERTIES OP ULTRAHIGH-STRENGTH STEELS

the two steels. Figure 1 shows the iso- reacted for 4 hr at these temperatures,
thermal-transformation diagrams for Figs. 2 and 3 respectively, illustrate that
Hll and 4350. The results of this investi- stoppage of the reaction at each of these
gation essentially agreed with the previ- temperatures does not represent 100 per
ously published diagram for the Hll cent transformation to bainite.
steel, shown in Fig. l(a). The diagram of The bainite morphology in the Hll
the 4350 steel, shown in Fig. 1(6), was steel changes, and the structure coarsens
obtained by interpolation between those as the reaction temperature is raised. In
of 4340 and 4360. the case of the 500-F reaction, the bainite
is acicular and resembles lower bainite.
S giis 555 n
F, a portion of ce
the the M
structure must consist of martensite
formed on quenching to 500 F; this mar-
tensite is then tempered during the
subsequent 4-hr hold. The structure also
contains retained austenite together with
some untempered martensite formed on
the quench from 500 F to room tempera-
ture. Isothermal transformation at 550 F
develops a bainite which cannot defin-
itely be identified as either upper or
lower bainite. Some regions of the
bainite contain coarse carbides oriented
approximately parallel to the long axis
of the plates, as in upper bainite, while
other areas of the structure contain
Carbon replica shadowed. Etchant—modified bainite plates with fine carbides oriented
picral.
FIG. 4—Electron Micrograph of 4350 Bainite at an angle of approximately 60 deg to
Transformed at 550 F for 4 hr (X 15,000). the plate axis. The remainder of the
structure appears to consist of retained
TABLE 2—Ma TEMPERATURES austenite. It is probable that small quan-
OF THE STEELS.
tities of both untempered and tempered
Ma Temper- Austenitizing
Steel ature, F Temperature, F martensite are also present. The trans-
formations at both 600 and 650 F pro-
Hll 555 1850 duce upper bainite, untempered marten-
4350 515 1550
site, and retained austenite as the final
structure.
For the purposes of this study, the It was found that the bainitic reaction
time for reaching the end of transforma- in 4350 reaches completion within 4 hr
tion at various reaction temperatures had for temperatures from 550 to 800 F. The
to be determined. In Hll, the bainitic microstructure of 4350 developed by
transformation was studied at 50-F transformation to bainite at 550 F (4 hr)
intervals between 500 and 700 F. It ap- is illustrated in the electron micrograph
pears that no bainite forms at 700 F. of Fig. 4. In agreement with the isother-
within 16 hr. However, stoppage of the mal-transformation diagram, Fig. 1(6),
reaction at 500, 600, and 650 F is reached the reaction appears to be complete, with
in times up to by
Copyright
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(all
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product
Mon
being
Dec
lower7 bainite.
13:15:25 EST
micrographs of specimens
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 177

were determined by the Greninger- t'1 = pretempering temperature (to be


Troiano metallographic technique, and followed by deformation of either
the results are given in Table 2. martensite or bainite), and
Vs- = retempering temperature, follow-
EXPERIMENTAL PROCEDURES ing deformation of either marten-
Eight basic thermal or thermome- site or bainite.
chanical treatments were employed in
Thermal Treatments:
this investigation, and are shown sche-
matically in Figs. 5 and 6. A list of sym- Processes B and M in Fig. 5 refer to
bols, most of which appear in these the formation of bainite or martensite,

FIG. 5—Schematic Representation of Thermal and Thermomechanical Treatments

figures and are used throughout this respectively, without any deformation
paper, are defined as follows: being introduced during the heat treat-
2° = austenitizing temperature, ment cycle. Bainite was formed by aus-
tb = bainite-reaction temperature, tenitizing for 30 min in salt at some tem-
td = austenite - deformation tempera- perature, ta, hot quenching into salt at
ture, the appropriate bainite-reaction tem-
tq = quench temperature, perature, /*, holding to the end of trans-
rt = room temperature, formation, tf , and oil quenching to room
In = liquid nitrogen, temperature, rt. Martensite was formed
hq = hot quenched, by air cooling Hll or oil quenching 4350
oq = oil quenched, from /°. Both processes B and M are
ac = air cooled, followed by a double-temper ing treat-
b
tf =Copyright
time forbybainite formation at t , ment (1 + 1 hr at /O in salt baths and
ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
t1 =Downloaded/printed
tempering temperature,
by
then air cooling to room temperature.
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178 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

Deformation of Austenite: each pass and then transferred to the air


Processes AB and AM in Fig. 5 in- furnace at & for 2 min. It was found that
volve the deformation of austenite be- the 4350 steel had to be deformed in one
fore transformation to either bainite or pass because of the narrow time and
martensite. Specimens were hot quenched temperature limits of the metastable
from J° into a salt bath at the desired austenite bay region. The experiments
deformation temperature, td. After 5 min involving austenite deformation were re-
in the salt, the material was rapidly stricted to a constant per cent reduction
transferred to an adjacent air furnace for in thickness of 50 per cent. Following the
2 min at the same temperature, t?, in final deformation pass, the specimens
order to allow the salt to drain and were either hot quenched to tb in order to

FIG. 6—Schematic Representation of Thermomechanical Treatments.

evaporate off. Previous experience in this form bainite or oil quenched to form mar-
connection had shown that rolling a dry tensite. Processes AB and AM were
specimen from an air furnace was easier completed by double-tempering (1 + 1
than rolling a specimen covered with salt. hr at /«)•
The specimen was then reduced by roll-
ing in a 2-high 15-in. mill. In the case of Strain-Tempering Martensite and Bain-
Hll, the reduction in thickness was ite:
achieved in 4 passes, with most of the Processes BS and MS in Fig. 6 refer to
deformation occurring during the first straining bainite and martensite, respec-
two passes and the final two passes used tively. After the formation of bainite or
primarily to straighten the blank. Be- martensite, the structures were single-
cause of a drop in temperature during the tempered 1 hr at some temperature, ttl
rolling operation,
Copyright by ASTMspecimens
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7 13:15:25 EST performed
turned by P for 3 min after
to the salt pot at
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KALISH EX AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 179
desired extent of deformation. Following tures between room temperature and
the deformation, the structures were re- liquid nitrogen.
tempered 1 hr at t12; lfl was not neces-
sarily the same as tt2. Mechanical Testing:
The hardness and unnotched tensile
Combinations of Thermomechanical Treat- properties of most of the bainitic and
ments:
tempered martensitic structures were de-
Processes ABS and AMS in Fig. 6 termined. The parameters obtained were
combine deformation of the parent yield strength (0.2 per cent offset), ulti-
austenite phase with straining of the mate tensile strength, per cent elongation

ta = 1850 F, tf = 4 hr, f« = rt, t* = 550 F.


FIG. 7—Tensile Properties of Hll as a Function of Bainite Reaction Temperature, f>, for Process B.

subsequently formed transformation (measured in a 2-in. gage length) and


product (either bainite or martensite). per cent reduction in area.
A precracked subsize Charpy impact
Refrigeration Treatments: test (6) was chosen for evaluating fracture
For various treatments, it was desira- toughness. This test has been found to
ble to introduce subcooling in order to be relatively easy to perform and evalu-
minimize or determine the influence of ate. The parameter measured was the
retained austenite on the properties. For energy per unit area required to propa-
this purpose refrigeration in liquid nitro- gate a crack under the conditions of the
gen was employed after the quench from test.
either /°, /** or i6, and also after the first The dimensions of the subsize Charpy
tempering treatment. Some treatments specimen were 2.165 in. in length, 0.394
also Copyright
requiredbyvariations inrights
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subcoolingMon Decin. in width,
7 13:15:25 and 0.080 in. in thickness.
EST 2015
temperature, tq, in the
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180 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

ta = 1850 F, tb = 550 F, = 4 hr, ta = rt or ln.


FIG. 8—Mechanical Properties of Hll as a Function of Tempering Temperature, tl, for Process B.

in the specimen after heat treatment, and tensile properties of Hll as a function of
then a precrack (about 0.015 in. in length bainite-reaction temperature, process B,
and extending through the specimen are shown in Fig. 7. A tempering tem-
thickness) was produced in a fatigue ap- perature, /', of 550 F was employed in
paratus specifically developed for the this series of tests. The ultimate tensile
purpose. strength is found to be independent of tb
in the temperature range of 450 to 650 F
EXPERIMENTAL RESULTS AND and has a value of approximately 270,000
DISCUSSION OF Hll psi. However, the yield strength changes
Bainite and Martensite—No Deforma- rapidly with ^ above 500 F. The decrease
tion (Processes
Copyright B andInt'l
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13:15:25 EST increases from
Bainite-Reaction Temperature,
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 181

coarsening of the bainite, as illustrated the refinement of the bainitic plate size
in Figs. 2 and 3. The increase in yield presumably accounts for the higher yield
strength for £* = 650 F is due to the strengths obtained at tb below 550 F.
limited amount of bainite formed and a However, in order to develop a small
corresponding increase in the quantity of bainitic plate size and avoid appreciable
martensite, as shown in Fig. 3(d). The martensite formation, a /* of 550 F was

ta = 1850 F, f* = rt or In.
FIG. 9— Mechanical Properties of HI 1 as a Function of Tempering Temperature, tl, for Process M.

elongation, measured in a 2-in. gage selected for further experiments on the


length, increases somewhat as tb de- bainitic structures.
creases, while the reduction in area re- Tempering Temperature, t*—The me-
mains essentially constant. chanical properties of Hll as a function
It should be noted that specimens of tempering temperature for process
transformed at 450 and 500 F contain B (f> = 550 F) are presented in Fig. 8.
significant amounts of martensite in addi- The effect of quench temperature, tq
tion Copyright
to the bainite since
by ASTM Int'l the M
(all rights s tempera-
reserved); (roomEST
Mon Dec 7 13:15:25 temperature,
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ture Downloaded/printed
is 555 F. Thisby factor together with gen, In) is illustrated. The ultimate tensile
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182 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

strength displays a marked secondary tempering temperature increases is par-


strengthening reaction independent of tially associated with the transformation
tq, reaching a maximum value of 324,000 of retained austenite.
psi at a tempering temperature of 1000 F. The ductility, as measured by tensile
The yield strength for tempering tem- elongation, is unaffected by tq and has a

f° = 1850 F, tb = 550 F, f« = 550 F, <« = rt or In.


FIG. 10—Mechanical Properties of Hll as a Function of Isothermal Transformation Time, ts ,
for Process B.

peratures of 900 F and below varies be- value of about 12 per cent for t* between
tween 115,000 and 150,000 psi. Temper- 550 and 900 F. The ductility falls to 6
ing in the temperature range of 1000 to per cent for /' values between 1000 and
1100 F develops a yield-strength level of 1100 F. The reduction in area values vary
230,000 to 245,000 psi. With a In quench between 15 and 35 per cent with a mini-
an increase in yield strength of about mum at a tl of 900 F. The impact energy
40,000 psi occurs for t* below 1000 F. is low over the entire range of /'.
TheCopyright
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mechanical be-
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 183

havior of Hll as a function of tl for be compared to martensite with a yield


process M. Refrigeration in liquid nitro- srength of 212,000 psi.
gen produces significant increases in both Isothermal Transformation Time, tj—
yield and ultimate strength for /' below The mechanical properties of Hll
approximately 900 F. Corresponding de- bainite as a function of t/ at 550 F are
creases in ductility and toughness are ob- shown in Fig. 10. These data include the
served. The effects associated with the effect of subsequent tempering, 1 + 1 hr
In treatment can be attributed to the at 550 F. The influence of subcooling in

Etchant—modified picral.
FIG. 11—Light Micrograph of Hll Isothermally Held at 550 F for 15 min and Quenched to Room
Temperature (X1500).

transformation of retained austenite to liquid nitrogen is also illustrated. It is


martensite on refrigeration. found that the bainitic transformation
Below a t* of 1000 F, martensite is seen essentially stops within 4 hr. The forma-
to possess a higher strength and tough- tion of bainite is accompanied by a
ness and lower ductility than the tem- marked loss in yield strength from the
pered bainites. On the other hand, for /' 240,000 psi level (tempered martensite)
above 1000 F (up to 1200 F), the bainite to approximately 120,000 psi, concurrent
has higher strength than the martensite with an improvement in ductility values.
but equivalent ductility and toughness. Light microscopy shows that a small
After an 1100-F temper the bainite has amount of bainite forms during the first
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
a yield strength of 236,000 psi which may 15 min at 550 F (Fig. 11). Although this
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184 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

tf = 1850 F, ^ = 900 F, deformation = 50 per centi


FIG. 12—Progress of Martensitic Reaction in Hll for Deformed and Undeformed Austenite.

ta Copyright
= 1850 F, by
f* = 900 F,
ASTM deformation
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FIG.Downloaded/printed
13—Tensile Properties
by of Hll as a Function Bainite Reaction Temperature, P, for Process
AB. University of Washington (University of Washington) pursuant to License Agreement. No further reprod
KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 185

structural change has no effect on the tenite deformation and subsequent bain-
tensile properties, a significant decrease ite formation in the vicinity of M„, it is
in toughness is observed. This is evi- important to know the effect of deforma-
dently a case where a small amount (see tion on the progress of the martensitic
Fig. 11, approximately 5 per cent) of one reaction. Figure 12 illustrates the degree

ta = 1850 F, i" = 900 F, deformation = 50 per cent, tb = 550 F, t = 4 hr, <« = rt or In.
FIG. 14—Mechanical Properties of HI 1 as a Function of Tempering Temperature, tl, for Process
AB.

constituent in a mixed structure can play of martensite formation from both de-
a controlling role in determining fracture formed and undeformed austenite as a
toughness. function of quench temperature. Aus-
tenite deformation of 50 per cent was
Austenite Deformation Prior to Trans-
found to depress the Ms slightly, but
formation (Processes AB and AM}:
significantly altered the shape of the
Bainite-Reaction Temperature,
Copyright by ASTM P—In
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transformation curve. EST 2015
Downloaded/printed by
order to study processes involving aus- Figure 13 depicts the tensile properties
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186 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

of Hll as a function of the bainite-reac- as a function of tempering temperature


tion temperature for process AB. The for process AB where fl is 550 F. The
In treatments markedly improve the yield trends in mechanical properties are
strength for all bainite-reaction tempera- rather similar to those observed in the
tures. Variation of /* and tq produce a absence of austenite deformation, as
number of interesting combinations of shown in Fig. 8. However, the strengths
strength and ductility. For example, obtained are now much greater. Also, the
a tb of 550 F, refrigeration in liquid nitro- effect of In treatments on the yield
gen, and subsequent tempering at 550 F strength is more pronounced in this case.
develops a yield strength of 250,000 psi, For all values of t* up to 900 F, and with

ta = 1850 F, td = 1000 F, deformation = 50 per cent, <« = rt.


FIG. 15—Tensile Properties of Hll as a Function of Tempering Temperature, tl, for Process AM.

an ultimate strength of 350,000, an a In quench, one obtains yield strengths


elongation of 11 per cent, and an a re- over 200,000 psi, ultimate tensile
duction in area of 27 per cent. This may strengths of 340,000 psi, and elongation
be compared with the properties of con- values between 9 and 11 per cent. Tem-
ventionally heat treated Hll, that is, pering above 900 F produces marked sec-
yield strength of 240,000 psi, ultimate ondary strengthening, which may be as-
strength of 315,000 psi, and an elongation sociated with the conditioning and
of about 5^ per cent. Thus, a fl of 550 F subsequent elimination of the retained
is used for further experiments involving austenite. The impact-energy values are
bainite formation out of deformed aus- low and seem insensitive to /' or tq.
tenite. The effect of tl on the tensile properties
lrights reserved); Mon Dec 7 13:15:25 EST 2015
Tempering Temperature, t —Figure 14 of Hll martensite produced by process
Copyright by ASTM Int'l (all
shows the mechanicalbyproperties of Hll AM is shown in Fig. 15. These ausformed
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 187

properties display higher strength and tq between rt and In. This suggests that
lower ductility than was obtained by the retained austenite is relatively un-
process AB (Fig. 14) for tl less than stable in the vicinity of room tempera-
1000 F. However, at the higher values of ture, and undergoes some conversion to
tl, the bainitic structures exhibit superior martensite during room-temperature ten-
strength. For example, on tempering at sion testing of process AB specimens.
HOOF, process AB develops a yield This situation could account for the
strength of 260,000 psi and an ultimate unusually large difference between the

ta = 1850 F, V1 = 900 F, deformation = 50 per cent, tb = 550 F, tf = 4 hr, tl = 550 F.


FIG. 16—Mechanical Properties of Hll as a Function of Quench Temperature, /«, for Process AB.

tensile strength of 300,000 as compared yield and ultimate strengths of the


to a yield strength of 240,000 psi and an bainitic structures.
ultimate tensile strength of 275,000 ob- Isothermal Transformation Time, tj—
tained by ausforming. Both processes The effect of bainite-reaction time at
produce elongations of about 5 per cent 550 F in process AB on the mechanical
for this tempering condition. properties of Hll are depicted in Fig. 17.
When the quench temperature, tq, is The parameters most sensitive to both
varied, a change in properties is obtained // and tq are the yield strength and
as given in Fig. 16. In this series ft is elongation. With tq at rt, the yield
and t* isby550
550 FCopyright F. The
ASTM Int'l yield strength
(all rights strength
reserved); Mon Decdecreases andESTthe2015elongation
7 13:15:25
increases continuouslyby with decreasing increases when tf is greater than about
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188 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

ta = 1850 F, td = 900 F, deformation = 50 per cent, tb = 550 F, <« = rt or In, t* = 550 F.


FIG. 17—Mechanical Properties of Hll as a Function of Isothermal Transformation Time, tf ,
for Process AB.

15 min. However, when tq is at In, the retained austenite is eliminated, for ex-
yield strength and elongation do not ample by employing high tempering
begin to change until t/ is more than 1 hr. temperatures such as 1 100 F.
These data, together with the temper-
ing series, Fig. 14, indicate that the Deformation of Bainite (Process BS^:
formation of bainite in Hll is accom- Per cent Deformation—The mechanical
panied by the retention of austenite. properties of Hll as a function of per
Evidently, this austenite is a controlling cent reduction in thickness for process
factor in determining the yield strength BS are presented in Fig. 18. The bainite
and elongation characteristics. The in- was formed at 550 F, pretempered /" at
herent properties of the bainite cannot 550 F, strained by rolling at room tem-
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015 t2
,be evaluated until essentially
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 189

Deformation of only 3.5 per cent followed yield strength of 370,000 psi, an ultimate
by retempering raises the yield strength tensile strength of 370,000, and an
from 120,000 to 275,000 psi, and de- elongation of 3 per cent. The per cent
creases the elongation from 12 to 5 per reduction in area remains at approxi-
cent. There is also a small improvement mately 25 per cent for deformations up

<M

t" = 1850 F, tb = 550 F, tf = 4 hr, *« = rt, ttl = 550 F, ttz = rt or 550 F.


FIG. 18—Mechanical Properties of Hll as a Function of Per Cent Reduction of Thickness for
Process BS.

in the ultimate tensile strength from to 10 per cent and then gradually de-
275,000 to 285,000 psi. Further deforma- creases to a level of 15 per cent for the
tion beyond 3.5 per cent increases the higher reductions.
yield strength slightly faster than the The degree of strengthening attributed
ultimate tensile strength, so that the to the deformation of the tempered
yield-to-ultimate ratio approaches
Copyright by ASTM unity.
Int'l (all rights bainite
reserved); Monand
Dec that portionEST
7 13:15:25 associated
2015 with
A deformation of 50 perbycent develops a the retempering at 550 F have been
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190 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

separated by testing specimens without


retempering, that is, with t& = rt. The
results are included in Fig. 18. An incre-
ment in yield strength of approximately
40,000 psi is produced by the retemper-
ing, and is independent of the amount of
strain for reductions between 4 and 50
per cent.
The effect of straining 10 per cent and
subsequent retempering on the micro-
structure of tempered bainite is illus-
trated by the light micrographs of Fig.
19. The structure in Fig. 19(a) consists
essentially of tempered bainite and re-
tained austenite. Straining 10 per cent
decreases the amount of retained austen-
ite, shown in Fig. 19(6), and subsequent
retempering appears to eliminate the
austenite almost entirely, Fig. 19(c).
A more detailed description of the in-
fluence of deformation and retempering
on the microstructure of Hll bainite has
been obtained by electron microscopy,
but the details will not be reported here.
Apparently, the straining causes some
re-solution of the carbides, and the subse-
quent retempering results in a precipita-
tion of fine carbides which is responsible
for the 40,000 psi increment in yield
strength.
The effect of deformation on tempered
martensite (process MS) will be discussed
in another section.
Pretempering Temperature, ttl and Re-
tempering Temperature, tt2—The influence
of pretempering temperature on the
mechanical properties of Hll for process
BS is illustrated in Fig. 20 for deforma-
tions of 10 and 35 per cent reduction in
thickness. The trends in mechanical
(a) Tempered at 550 F properties are similar for both degrees of
(b) Pretempered at 550 F and strained 10 per
cent deformation. The strength is unaffected
tl
(c) Pretempered at 550 F, strained 10 per by variations in t from rt to 800 F.
cent, and retempered at 550 F. However, a marked strengthening peak
Etchant—modified picral. occurs between 900 and 1000 F. A defor-
FIG. 19—Light Micrographs of Hll Bainite mation of 35 per cent with a ttl of 550 F
Transformed
Copyrightat by
550ASTM
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(X2000).
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 191

ta = 1850 F, tb = 550 F, tf = 4 hr, f« = rt, deformation = 10 or 35 per cent, tt2 = 550 F.


FIG. 20—Mechanical Properties of HI 1 as a Function of Pretempering Temperature, ttl, for
Process BS.

but this is increased to 395,000 psi by where the elongation increases from less
employing a tn of 1000 F. The hardening than 4 to 14 per cent, concurrent with a
response is accompanied by minima in yield strength of 285,000 psi and an
elongation, reduction in area, and impact ultimate strength of 300,000 psi.
energy. The development of alloy car-
bides on tempering in the vicinity of Combinations of Thermomechanical Treat-
1000 F considerably enhances the ments (Processes ABS and A MS):
strengthening obtained by strain-temper-
ing this steel. It should be noted that the It has been shown that one can obtain
virtual coincidence of the yield strength strength improvements in Hll by defor-
and ultimate tensile strength in this mation of austenite before transforma-
series indicates that the stable elonga- tion to either bainite or martensite, or by
tions are negligible. deformation applied after transforma-
The experiments on varying the retem- tion. The possibility of combining these
pering temperature, tt2, are summarized deformation processes affords the oppor-
in Fig. 21. A striking effect is found for tunity of achieving even greater strength
10 per cent deformation and ttz ofreserved);
Copyright by ASTM Int'l (all rights
1000 F Monlevels.
Dec 7 As
13:15:25 EST 2015
a result, experiments were per-
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192 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

formed to determine the changes in proximately additive to the strengthen-


properties developed in each step of such ing increment obtained by austenite de-
combined treatments. formation prior to the bainitic reaction.
A comparison of the tensile properties As a matter of fact, the amount of
of Hll bainite subjected to various ther- strengthening obtained by 10 per cent
mal and thermomechanical treatments is bainite deformation is not essentially al-

ta = 1850 F, tb = 550 F,f t= 4 hr, <« = rt, ttl = 550 F, deformation = 10 or 35 per cent.
FIG. 21—Mechanical Properties of Hll as a Function of Retempering Temperature, ttz, for
Process BS.

illustrated in Fig. 22. Treatments 1 tered by 50 per cent prior deformation


through VI have been discussed individu- of the austenite. Similarly, retempering
ally in the preceding sections. Treat- after the bainite deformation step in
ments VII and VIII (process ABS) process ^4J55 produces a significant im-
demonstrate the strengthening advan- provement in strength. It may be noted
tage of combining the two deformation that In treatments have no effect in proc-
processes. A comparison of treatments esses involving deformation of the tem-
VII Copyright
and V shows
by ASTMthat
Int'lthe
(all strengthening
rights reserved); Monpered bainiteEST(treatments
Dec 7 13:15:25 2015 V through
obtained by bainite bydeformation is ap- VIII). Process ^455, including re temper-
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 193

ing at 550 F, gives the highest yield gains obtained by combining austenite
strength in this series with a value of deformation with subsequent straining of
365,000 psi. martensite. As in the work on bainite, it
In general, it appears that the elonga- is found that the strengthening effects
tion decreases as the yield strength in- from processes AM and MS are essen-

FIG. 22—Comparison of Tensile Properties of Hll Bainite Subjected to Various Thermomechani-


cal Treatments.

creases. However, process AB with a In tially additive. Process AMS, treatment


quench, treatment IV, shows an interest- IV, develops a yield strength of 390,000
ing combination of properties. For this psi. However, at this exceptionally high
situation, the yield has been improved to yield strength value, the elongation is
250,000 psi, while the elongation has 1.5 per cent.
decreased only slightly to a value of Up to the present time, further opti-
Copyright
10 per cent. by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25
mization EST 2015
of the deformation and temper-
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Figure 23 depicts bythe strengthening ing variables has not been carried out.
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194 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

EXPERIMENTAL RESULTS AND bainite with increasing tb. The per cent
DISCUSSION OF AISI 4350 elongation is essentially constant over
the entire range of tb studied here.
Bainite with No Deformation (Process The effect of tempering temperature,
E): tf, on the bainite formed at 550 F is given
in Fig. 25. A small strengthening peak is
The effect of the bainite-reaction tem- observed at 600 F. For tl values above
perature, /*, on tensile properties is 700 F the yield strength drops below

FIG. 23—Comparison of Yield Strength of Hll Martensite Subjected to Various Thermomechani-


cal Treatments.

shown in Fig. 24. The strength decreases 200,000 psi with a very large increase in
with increasing reaction temperature up impact energy.
to a temperature of 750 F, whereas the
reduction in area and impact-energy Austenite Deformation Prior to Trans-
values go through a maximum between formation (Processes AB and AM):
b
650 and 700 F. At a t of 800 F, the reac- In contrast to the results obtained on
tion is still underway in 4 hr, as shown in Hll, process AB applied to 'AISI 4350
Fig. 1. This allows martensite to form on results in only small gains in strength,
quenching from lb with a resultant in- approximately 5,000 to 10,000 psi, over
crease in strength. Metallographic ob- process B. This is the case even though
Copyright
servations by ASTMaInt'l
indicate (all rights reserved);
coarsening tb is
of the Mon Dec 7 13:15:25
varied fromEST to 750 F (t* = 550 F)
5502015
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KA.LISH ET AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 195

and when /' is varied from rt to 1100 F to determine the influence of austenitiz-
(/6 = 550 F). Austenite deformation ing temperature, ta, on processes M and
prior to bainite formation produces a AM. The results are summarized in
slight decrease in both elongation and Table 3. Changing p from 1550 to 2100 F
impact energy. has little effect on the mechanical proper-
The strengthening developed by proc- ties obtained in process AM, and is in

ta = 1550 F, t} = 4 hr, tl = 550 F.


FIG. 24—Mechanical Properties of 4350 as a Function of Bainite Reaction Temperature, tb,
for Process B.

ess AM (ausforming) as a function of tl is agreement with the findings of Justusson


shown in Fig. 26. The tensile properties and Schmatz (7) on a 0.32 per cent
for process M are included in this figure in carbon, 3.0 per cent chromium, and 1.5
order to indicate the changes attributable per cent nickel steel. This is further con-
to the austenite deformation. The yield firmation of the fact that austenite grain
strength increment varies from 40,000 to size, which determines the maximum
22,000 psi as tl is increased from 400 to martensitic plate size, does not control
HOOF. the strength of ausformed low-alloy
Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
Some experiments were also performed
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steels. In contrast, the strength achieved
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196 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

ta = 1550 F, tb = 550 F,f t= 4 hr,«« = rt.


FIG. 25—Mechanical Properties of 4350 as a Function of Tempering Temperature for, tl, Process B.

by regular hardening and tempering, tion in area and impact energy go


process M, decreases progressively as the through a maximum at about 650 F as in
austenitizing temperature is raised. the case of process B (Fig. 24). The
Deformation of Bainite and Martensile elongation has a constant value of 4 per
cent over the transformation tempera-
(Processes BS and MS):
ture range investigated. There is no
Bainite-Reaction Temperature, tb—The obvious distinction between upper and
mechanical properties of strain-tempered lower bainites in their response to this
4350 as a function of tb are illustrated in strain-tempering treatment.
Fig. 27. An increment in yield strength of Pretempering Temperature, tn, and
approximately 50,000 psi is found, com- Retsmpering Temperature, tK—The ten-
pared with by
Copyright process B, (all
ASTM Int'l over the
rights entireMonsile
reserved); Decproperties of 2015
7 13:15:25 EST 4350 as a function of
of tb from 550 to
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range by 800 F. The reduc- tn and tK for process BS are summarized
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 197

<° = 1550 F, td = 1050 F, deformation = 50 per cent, i« = rt.


FIG. 26—Tensile Properties of 4350 as a Function of Tempering Temperature, tf, for Processes
M and AM.
TABLE 3—EFFECT OF AUSTENITIZING TEMPERATURE ON THE TENSILE
PROPERTIES OF 4350 FOR PROCESSES M AND AM.
Process ttt. F Yield Strength, psi Ultimate Tensile Elongation,
Strength, psi %
M
[1550 232 000 281 000 4.9
((« = rt, V = 550 F) 1 1700 229 000 278 000 3.7
1900 218 000 263 000 4.2
[2100 210 000 254 000 4.7
A.M
1550 270 000 308 000 4.5
(if1 = 1050 F, austenite deforma- 1700 265 000 308 000 3.3
tion = 50% 1900 263 000 307 000 3.1
<« = RT, t( = 550 F 2100 266 000 306 000 3.9

in Figs. 28 and 29, respectively. The yield obtainable on tempering of unstrained


strength is maximum for a value of ta and bainite, as shown in Fig. 25. For example,
/ <2 = 550 F. The yield-to-ultimate straining 10 per cent and retempering at
strength ratio is approximately unity 900 F results in a yield strength of about
when /'2 is 550 F. This ratio decreases 200,000 psi, a reduction in area of 48 per
slowly as t12 is either decreased or in- cent, and an elongation of 7 per cent.
creased from 550 F. Per cent Deformation—The effect of the
The yield strength is found to sustain degree of deformation on processes BS
higher levelsby ASTM
Copyright on retempering at high
Int'l (all rights reserved); Mon and 7MS
Dec for EST
13:15:25 43502015
are illustrated in Fig.
2
temperatures (/' up
Downloaded/printed by to HOOF) than is 30. The strain-tempering curves of Hll
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198 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

ta = 1550 F, tf = 4 hr, t" = rt, tn = 550 F, deformation = 10 per cent, t12 = 550 F.
FIG. 27—Mechanical Properties of 4350 as a Function of Bainite Reaction Temperature, tb, for
Process BS.

ta = 1850 F, #> = 550 F, ft = 4 hr, t« = rt, deformation = 10 per cent, t'2 = 550 F.
FIG. 28—Tensile
Copyright Properties
by ASTM Int'l (all of 4350reserved);
rights as a Function
Mon Decof7 Pretempering Temperature, /", for Proc-
13:15:25 EST 2015
ess BS.
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ta = 1550 F, t* = 550 F, t/ = 4 hr, f« = rt, t" = 550 F, deformation = 10 per cent.
FIG. 29—Tensile Properties of 4350 as a Function of Retempering Temperature, ttz, for Process BS.

Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
FIG. 30—Yield Strength of 4350 and Hll as a Function of Per Cent Deformation for Processes
BS and MS.
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199
FIG. 31—Comparison of Yield Strength at 4350 Martensite Subjected to Various Thermo-
mechanical Treatments.

ttl = 400 F, deformation = 10 per cent.


Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
FIG. 32—Influence of Carbon Content on Strain Tempering Response of 43XX Martensites.
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS OF BAINITES 201

bainite and martensite are included for tempering is undoubtedly due to the
comparison purposes. In all cases, con- retained austenite present, rather than
spicuous strengthening is found as a to the bainite itself. The Hll structures
result of small deformations of the order strain-temper to higher strength levels
of 3 per cent. For deformations of 5 to 50 than do the 4350 structures. For any

FIG. 33—Comparison of the Response of Hll Bainite and Martensite to Various Thermal and
Thermomechanical Treatments.

per cent, both materials display an given amount of deformation, the


essentially linear increase in strength process MS develops higher strength in
with increasing deformation. each material than does process BS.
Bainite has a greater strengthening
response than does martensite at very Combinations of Thermomechanical Treat-
low deformations, but the martensite ments (Processes ABS and A MS):
strengthens at a somewhat greater rate In view of the small strengthening
for Copyright by ASTMofInt'l
higher amounts (all rights reserved);
deformation. The Mon Dec 7 13:15:25
improvement EST 2015
obtained by austenitede-
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initial sensitivity of bainite to strain- formation prior to bainite formation in
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202 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

the 4350 steel, process AB versus process achieves an increment of 78,000 psi.
B, there seems to be no advantage to Once again, it is observed that, as the
employing a combination treatment. In strength of martensite is improved, the
other words, one would obtain practically ductility tends to decrease.
the same results for process ABS as for
process BS in this material. E/ect of Carbon Content on Process
However, combination treatments can MS:
be applied advantageously to marten- A supplementary series of experiments

FIG. 34—Comparison of the Response of 4350 Bainite and Martensite to Various Thermal and
Thermomechanical Treatments.
sites in the 4350 steel. Figure 31 shows was performed to explore the influence of
the almost additive nature of the yield carbon content on the strain-tempering
strength increments associated with each response of 43XX martensites. Some
thermomechanical treatment. For ex- data were available for carbon contents
ample, treatments II and IV, processes of 0.12 and 0.20 per cent (8) arid carbon
AB and MS, produce yield-strength contents of 0.35 and 0.43 per cent were
increments of 38,000 and 50,000 psi, added to the program. The results of
respectively, and
Copyright by combining
ASTM thesereserved);
Int'l (all rights treat- Mon
these
Dec experiments
7 13:15:25 EST involving
2015 process MS
ments in treatment VI,
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KALISH ET AL ON THERMOMECHANICAL TREATMENTS or BAINITES 203

that the strength improvements for both Finally, a comparison may be made
straining and retempering increase with between the two steels investigated. Hll
increasing carbon content. has been shown to be much more respon-
sive than 4350 to all of the thermome-
GENERAL COMPARISONS chanical treatments investigated.
AND CONCLUSIONS
CONCLUSIONS
General Comparisons:
The results of this work can be sum-
The response of Hll and 4350 to marized as follows:
various thermal and thermomechanical 1. The mechanical properties of Hll in
treatments is shown in Figs. 33 and 34, the martensitic or bainitic condition are
respectively. These data are presented so strongly affected by refrigeration in
that a direct comparison may be made liquid nitrogen when tempered at tem-
between bainite and martensite after peratures below 1000 F. This indicates
analogous processing conditions. The the important influence of retained
processes considered in these figures austenite.
involve either (1) no deformation, (2) 2. Hll bainite formed at 550 F
austenite deformation, or (3) transforma- exhibits a large secondary strengthening
tion-product deformation (strain-tem- when tempered between 1000 and 1100 F.
pering). Under these conditions, with a This effect is mainly attributable to the
550 F-temper, it is seen that the marten- elimination of austenite, which is re-
sites always have greater strengths than tained in large amounts when bainite is
the bainites in both Hll and 4340. How- formed.
ever, the bainites generally have superior 3. After tempering at the highest tem-
ductility. In Hll the differences between pering temperatures, 1000 to 1200 F, Hll
martensitic and bainitic properties are bainite has higher strength than does
most striking for treatments involving martensite, accompanied by equivalent
either no deformation or austenite defor- ductility and toughness. Bainite tem-
mation. In 4350, the ductility differences pered at 1100 F has a yield strength of
are small, but the strength variation is approximately 235,000 psi as compared
significant for all processes. to approximately 212,000 for martensite
An interesting comparison may be at the same temperature.
made between austenite deformation 4. The appearance of only a very
processes and strain-tempering processes. small amount of bainite in Hll (trans-
Deformation of either bainite or marten- formation times up to 15 min) is accom-
site (strain-tempering) always develops panied by a marked decrease in fracture
much higher strengths for a given toughness.
amount of deformation than does austen- 5. Austenite deformation in Hll of
ite deformation followed by transforma- 50 per cent depresses M8 by about 5 F,
tion to either bainite or martensite. This and significantly alters the shape of the
may be seen for Hll in Fig. 33 by com- martensite range curve.
paring treatments V and VI with IX and 6. Austenite deformation in Hll re-
X, and for 4350 in Fig. 34 by comparison sults in considerable strengthening of the
of treatments III and IV with V and VI. subsequently formed bainite, and liquid
The strain-tempering treatments always nitrogen refrigeration is then found to
produce lower ductilities than is ob- have a large effect on tempering up to
tained with the austenite deformation 900 F. A strengthening peak occurs on
Copyright by ASTM Int'l (all rights reserved); Mon Dec
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204 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

strengths being higher than is obtained to strain-tempering treatments. As in the


on similar tempering of ausformed Hll. case of Hll, small deformations (up to 3
7. Hll bainites and martensites ex- per cent) result in large strengthening
hibit a large response to strain-tempering effects.
treatments. Small deformations (up to 3 12. Increasing carbon content in
per cent) produce large strengthening 43XX steels produces increasing incre-
effects. Retempering produces an essen- ments in strength due to strain-temper-
tially constant strength increment ing.
(40,000 psi) for bainites strained between 13. The application of deformation
5 and 50 per cent. processes, both before and after marten-
8. Maximum strengthening by strain- site formation in 4350, results in a
tempering of Hll bainites is obtained by strengthening which is approximately
pretempering at 1000 F and retempering additive when the individual processes
at 400 F. are combined.
9. The increments in strength devel-
oped by deformation processes both A cknowledgments:
before and after transformation to
either bainite or martensite are found to The authors appreciate the support of
be approximately additive when the the Metals Branch of the Materials
individual processes are combined. Division, Bureau of Naval Weapons,
10. Austenite deformation in 4350 has Department of the Navy. They also
little effect on the strength of subse- acknowledge the cooperation of T.
quently formed bainite. However, such Kearns and G. Yoder, under whose cog-
deformation does enhance the strength nizance this investigation was conducted.
properties of martensite. J. Davis, H. Tushman, and R. Wright
11. Both bainitic and martensitic assisted in various experimental aspects
structures in 4350 exhibit a large response of the program.

REFERENCES
(1) W. R. Warke and A. R. Elsea, "Methods of (5) E. T. Stephenson and M. Cohen, "The
Strengthening the Ultrahigh Strength Effect of Prestraining and Retempering on
Steels," Defense Metals Information Center, AISI type 4340," Transactions, American
Memo 149, April, 1962. Society for Metals, Vol. 54, 1961, p. 72.
(2) V. F. Zackay, N. M. Justusson, and D. J. (6) G. M. Orner and C. E. Hartbower, "Sheet
Schmatz, "Deformation of Metastable Fracture Toughness Evaluated by Charpy
Austenite . . . An Interim Report on a New Impact and Slow Bend," Welding Journal
Process," Metal Progress, Vol. 80, September, Research Supplement, September, 1961.
1961, p. 68. (7) W. M. Justusson and D. J. Schmatz, "Some
(3) P. J. Fopiano, S. Das Gupta, and D. Kalish, Observations on the Strength of Martensite
"Effect of Mechanical and Thermal Proc- Formed from Cold-Worked Austenite,"
essing on High Strength Steels," Watertown
Transactions, American Society for Metals,
Arsenal Laboratories, Final Technical Report
No. 320.4/4-3, June, 1962. Vol. 55, 1962, p. 640.
(4) E. B. Kula and J. M. Dhosi, "Effect of (8) S. V. Radcliffe, M. Schatz, G. Orner, and G
Deformation Prior to Transformation on the Bruggeman, "The Flow Tempering of High
Mechanical Properties of 4350," Transac- Strength Steel," ManLabs, Inc., Watertown
tions, American Society for Metals, Vol. 52, Arsenal Laboratories, Final Technical Report
1960, p. 321. No. 320.4/3-1, April, 1962.

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DISCUSSION

M. HILL, S. PASCOVER, AND S. J. conclusion in the case of solid solution


MATAS1—We would like to compliment strengthening elements such as silicon,
the authors on having contributed some nickel, and cobalt.
excellent experimental information to However, we feel that any conclusions
the complex field covering the role of with respect to the susceptibility of a
thermomechanical treatments in im- given alloy steel to strengthening by
proving the strength, ductility and, in the deformation of austenite and subse-
some instances, toughness of steels. They quent transformation to bainite (process
have elegantly shown that by superim- AB), cannot be clearly established from
position of various strengthening mecha- the data in this paper, since Hll did not
nisms steels can approach a high strength clearly transform to bainite. The pres-
level of 400 ksi. For 4350 and Hll this ence of the mixed structure seems to so
amounted to a tripling of strength (120 greatly complicate the issue that the Hll
ksi to 360 ksi). and 4350 cannot be readily compared.
By the less elaborate superimposition The TTT curves and photomicrographs
of straining on the hot-cold working of a presented can be interpreted as showing
0.60 per cent carbon and 5 per cent nickel that a substantial portion of the austenite
steel we were able to double the strength transformed to martensite rather than
from 290 to 530 ksi while retaining some bainite.
ductility. Using the authors' thermo- The data presented in this paper indi-
mechanical treatments, however, it is cate that a substantial improvement can
conceivable that the 530 ksi may be be produced in the toughness of 4350
greatly exceeded with this 0.60 per cent at a given strength level by deformation
carbon and 5 per cent nickel steel, per- of austenite followed by transformation
haps even approaching the million ksi to bainite (process B) rather than mar-
goal. tensite. Similar results have been re-
One of the goals of the authors' work ported by R. F. Heheman et al. In all
was to determine if the response to ther- cases the improvement was minor. How-
momechanical work was a function of the ever, our work2 indicates that if a 9 per
alloy content of the steel. Their work cent nickel and 4 per cent cobalt steel
appears to confirm other recent work in- is treated in a similar fashion, an appre-
dicating that steels with higher amounts ciable increment of toughness may be
of manganese, chromium and molyb- obtained from a bainitic rather than a
denum are more susceptible to thermo- martensitic structure. The differences in
mechanical working than steels with behavior between these two types of
smaller amounts of these elements. steels may be ascribed to the solid solu-
Earlier work permitted a firm conclusion tion elements acting to improve fracture
only in the case of carbon, with no resistance.
The authors probably adopted isother-
1 Copyright by ASTM Int'l (all rights reserved); Mon Dec 7 13:15:25 EST 2015
Research metallurgists, Research Center,
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205
206 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

mal deformation of austenite for the sake the difference in response of bainite in
of convenience and clear-cut experi- Hll and 4350 to pre-austenite deforma-
mentation. However, whether the prod- tion. Since 4350 steel contained little re-
uct is to be bainite or as in our hot-cold tained austenite and responded only
working process, martensite, it may be slightly to bainite formation after prior
more practical for production purposes to austenite deformation, is it possible that
follow an athermal course. Almost equal the better results obtained in the Hll are
properties result if deformation begins in caused by variations in the amount of
the normal hot working range and con- martensite in the structure, or do the
tinues by any path which avoids trans- authors feel that there is a fundamental
formation until the temperature is difference in the bainite contained in the
reached for bainite or martensite forma- two steels?
tion. D. KALISH, S. A. KULIN, AND M.
It seems that this paper will be of great COHEN (authors' closure)—The authors
utility in the search for high-strength wish to thank the discussers for their
steels. helpful comments.
ERIC B. KuLA3—The authors are to be The results obtained by Hill, Pascover,
congratulated for this very thorough and Matas on 0.60 per cent carbon-5 per
study of the effects of various thermo- cent nickel and 9 per cent nickel-4 per
mechanical treatments applied to bain- cent cobalt steels certainly indicate
itic structures. Their findings, which paths for future investigations. In fact,
show that bainite behaves the same as the authors are presently engaged in
martensite in that it is strengthened studying the influence of thermome-
when cold worked and aged or when it is chanical treatments on the properties of
formed from a cold worked austenite, are the 9 per cent nickel-4 per cent cobalt
important. Also, their results that the steel.
strengthening contributions from de- As suggested by Dr. Kula, the differ-
forming, both before and after trans- ence in the strengthening response of
formation, are approximately additive, 4350 and Hll to austenite deformation,
indicates that very high strengths can be when followed by transformation to
obtained by such combinations of treat- bainite, may be partially attributed to
ments. This is not incompatible with the presence of retained austenite. Re-
current ideas on the strengthening cent experiments4 have shown that 33
mechanisms involved during thermo- per cent austenite is retained in Hll with
mechanical treatments. process AB, td = 550 F, deformation =
In previous investigations on the me- 50 per cent. Approximately half of this
chanical properties of bainite, the pres- austenite converts to untempered mar-
ence of retained austenite, as well as tensite during the tension test and causes
tempered and untempered martensite the large separation of yield and ultimate
in the structure, has always been a com- tensile strengths shown in Fig. 14 for the
plicating factor. The authors have very rt quench condition. Subcooling in liquid
aptly demonstrated the effect of reducing
nitrogen causes a substantial increase in
the amount of retained austenite in Hll
yield strength because 11 per cent aus-
steel by refrigeration on the mechanical
properties. This brings up the question of
4
D. Kalish, S. A. Kulin, and M. Cohen,
3
Supervisory physical metallurgist, U. S. "Bainitic Structures and Thermomechanical
ArmyCopyright
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DISCUSSION ON THERMOMECHANICAL TREATMENTS or BAINITES 207

tenite is thereby converted to untem- to strain tempering, Fig. 30. The implica-
pered martensite. In either case, the mar- tions of these results are that the addi-
tensite that forms from the deformed tional alloying elements in Hll affect the
austenite should have the high yield nature of the bainite and martensite or
strength typical of ausformed (process at least alter the response of these micro-
AM) martensite. constituents to thermomechanical treat-
This argument does not preclude the ments.
possibility that there may be a funda- Unfortunately the multiphase struc-
mental difference between the bainites in tures that form, in the various treatments
4350 and Hll. A difference does seem to investigated, do not allow a direct com-
exist between the martensites in these parison between the bainites in 4350 and
two alloys, as indicated by the response Hll.

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ULTRAHIGH-STRENGTH STEEL FASTENERS

BY A. C. HOOD1 AND R. L. SPROAT1

SYNOPSIS
Bolts with tensile strengths as high as 300,000 psi are being produced and
reliably used. The manufacturing and application of these bolts are a challenge
owing to the basic design of threaded fasteners.
There are severe stress concentrations caused by the notches of the threads
and the abrupt change in cross section of the head-to-body fillet area. In order
to maximize both notch toughness and fatigue strength, large fillet radii are
used in both of these critical areas.
For additional fatigue strength, the head-to-shank fillet radius is prestressed
and the threads are rolled after heat treatment.
The material selected for bolting must have a high degree of notch toughness
as well as strength. H-ll hot-work die steel has the greatest application for
bolts with tensile strengths over 220,000 psi. Corrosion-resisting materials such
as A-286 and Inconel 718, which are cold worked prior to aging, are also used.
Care must be exercised during the heat treatment of the bolts to prevent car-
burization or decarburization, both of which reduce fatigue strength. Stresses
caused by grinding are removed by retempering prior to fillet stressing and
thread rolling.
Alloy steel bolts are coated for corrosion protection with electroplating or
vacuum-deposited cadmium. Through the use of these methods, hydrogen
embrittlement is avoided.
Application and environmental conditions greatly affect the life of a bolt in
actual usage. Fatigue failures may be caused by corrosion. The performance of
the bolt is influenced by the configuration of a nut or tapped hole. The design
of the joint and conditions of tightening must also be considered.

The development of a number of high- fasteners which will take the same loads
strength structural steels over the past without failure.
several years is in keeping with the Although high-strength steel fasteners
demand for materials that will withstand preceded the use of ultrahigh-strength
the high stresses imposed by lighter steels in other applications, except
weight designs and higher performance perhaps landing gear structures, the
requirements of both conventional air- challenge has been one of maintaining
craft and aerospace vehicles. this availability of fasteners when
It is natural that utilization of these material needs required them.
materials prompts a requirement for Another requirement has been that
1
Manager, research and development, and the resulting hardware should not be of
director, engineering and development, re- such new and unique design that it would
spectively, Standard Pressed Steel Co., Jenkin-
town, Pa. require a whole new fastening technology
208
HOOD AND SPROAT ON ULTRAHIGH-STRENGTH STEEL FASTENERS 209

The bolt is subjected not only to high


tension loads, but to shear, bending, and
fatigue. Depending on the design and
characteristics of surrounding structural
materials, it often must carry loads in
FIG. 1—A Twelve-Point External Wrenching excess of those imparted to the adjacent
Aircraft Bolt. structure. Being made of steel, it is
Thread exposure of f-20, 200,000-psi bolts subject to all the problems inherent in
measured from shank thread runout to point of
thread engagement. steel, such as corrosion, heat treat

FIG. 2—Effect of Thread Engagement on Bolt Tensile Strength.


The stress required to achieve 65,000-cycle fatigue life for bolts with rolled threads after heat
treatment peaks is slightly below 200,000 psi tensile strength.

to assemble the high-strength steels into variables, hydrogen embrittlement, and


useful structures. notch sensitivity.
The design of a bolt tends to make it Fortunately, the bolt may be tested
difficult to utilize the full strength in its entirety, without resorting to the
potential of materials. Basically, the method of testing metal specimens to
bolt is a bar with a series of notches at predict the properties of the bolt.
one end, a non-uniform cross-section, a The combination of stresses imposed
diameter
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as shown in Fig. 1. so complex that the material property
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210 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

approach offers little guide to bolt engagement of internal and external


properties. Bolts are therefore tested as threads.
specimens to provide tensile, shear, Another factor affecting the tensile
fatigue, and even impact data. strength of a bolt is the number of
threads exposed between the runout
TENSILE STRENGTH thread and the point where the first nut
The tensile strength of the base ma- thread is engaged. In Fig. 2 the tensile
terial is the initial criterion for its use in strength drops as a function of the num-
a fastener. The tensile strength of a ber of threads exposed (I).2 In aircraft
bolt made from a material must be as bolting, where thread length is generally
near as possible to the strength of the short, the tensile strength is measured at
ASTM specimen in order to merit three exposed threads.
further consideration. A number of comparative studies have
While it is desirable to utilize a ma- been made of material and bolt strength,
in an effort to establish an empirical
TABLE 1—HIGH-STRENGTH BOLTING method for calculation of thread area
MATERIALS. (2—4). The resulting bolt area has been
Material at Various Tensile Strengths, psi chosen from these investigations and
further reference to bolt tensile strength
220,000 260,000 300,000 will be on this basis.
H-ll" H-ll" Vasco Jet SELECTION or BOLTING MATERIALS
MA"
MIL-S-7108A0 4340° Maraging High-strength bolting has been cate-
Steel, 325 gorized into tensile strength levels of
A-2860 Inconel 718 Ausformed
220,000, 260,000, and 300,000 psi. Table
H-ll
15-7 Mo Waspaloy 1 shows ultrahigh-strength alloys which
Mar aging are capable of achieving bolt strengths
Steel, 300
AFC 77 of these magnitudes. Their selection as a
0
bolting material, however, is not gov-
Currently used as bolting. erned by strength alone.
Other factors affecting the selection of
terial of high yield strength, the term a high-strength material include thread
bolt yield strength has little meaning, tensile strength, fatigue endurance,
since there is no reference either to uni- range of temperature stability, fabricabil-
form cross section or fixed gage length. ity, susceptibility to hydrogen embrittle-
For this reason, subsequent discussion ment, and resistance to corrosion and
of ultrahigh-strength steel fasteners will stress-corrosion. The important aspect
be in terms of bolt ultimate tensile of the above, however, is that the selec-
strength. tion be made on the basis of bolt prop-
The tensile strength of a bolt cannot be erties and not limitations imposed by
accurately predicted from the notch material data. To cite a specific example,
properties of the base material, although note in Table 2 the properties of both
these values often serve as a guide in material and notch strength. It is not
the screening of high-strength steels. until the tension-tension fatigue life of
The stress-concentration factor of a bolts made from both materials can be
multiple-notched specimen may. be cal- compared that a separation can be made.
culated, but it is not the same as the 2
The2015boldface numbers in parentheses refer
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HOOD AND SPROAT ON ULTRAHIGH-STRENGTH STEEL FASTENERS 211

Another possible choice at this strength chromium content and resistance to


level would be AISI 8740 steel. Figure 3 hydrogen embrittlement.
illustrates, however, that the fatigue An advantage of H-ll steel at the
resistance of this alloy peaks at a strength 220,000 and 260,000 psi strength level is
level slightly below 200,000 psi (5). its retention of strength at elevated
Fatigue is not the only criterion for temperature, which enables it to be used
selection. Resistance to hydrogen em- for 900-F bolting with only a slight loss
brittlement would again enable a separa- in strength at that temperature (8,9).

TABLE 2—MATERIAL AND BOLT PROPERTIES OF 4330 MODIFIED,


4340, AND H-ll STEELS.
Property 4330 Modified 4340 H-ll

BOLTS HEAT THEATED FROM 180,000 TO 200,000 PSI

Material UTS, psi 201,100 196,000 197,700


Material yield strength, psi 190,200 184,000 158,200
Elongation in 4 diameters, % 13.5 11.9 15.5
Reduction of area, % 53.0 42.3 47.7
Notch-to-smooth ratio, Kt6 1.2 1.4 1.4
Bolt UTS, psi 204,300 199,000 198,000
Fatigue-cycles, maximum stress, 93,000 psi 71,000 59,500 321,100

BOLTS HEAT TREATED FBOM 220,000 TO 250,000 PSI

Material UTS, psi 242,800 229,000 236,800


Material yield strength, psi 208,800 210,500 199,400
Elongation in 4 diameters, % 12.6 10.9 13.5
Reduction of area, % 49.4 41.6 48.3
Notch-to-smooth ratio, Kt6 1.2 1.2 1.3
Bolt UTS, psi 238,100 230,700 239,000
Fatigue-cycles, maximum stress, 115,000 psi 20,400 174,000 417,600

BOLTS HEAT TREATED FROM 260,000 TO 290,000 PSI

Material UTS, psi ... 289,000 288,000


Material yield strength, psi ... 229,800 243,700
Elongation hi 4 diameters, % ... 9.0 12.1
Reduction of area, % ... 29.2 41.4
Notch-to-smooth ratio, KtQ ... 1.0 1.1
Bolt UTS, psi ... 290,000 288,400
Fatigue-cycles, maximum stress, 135,000 psi. . ... 24,000 700,000

tion to be made. The data in Fig. 4 show A need for a high-strength, high-
a comparison of H-ll and 4340 steels, temperature stainless bolting material
using notch tension specimens under a exists. Alloys sometimes considered for
sustained load of 90 per cent of notched use as high-strength bolts are A-286,
ultimate strength (6). All alloy steels in Inconel 718, and Waspaloy. Since heat
aircraft are plated. Therefore, , the treatment alone will not provide these
possibility of hydrogen embrittlement strengths, the alloys are cold worked
cannot be overlooked. The above data prior to aging to raise the aged material
have recently been confirmed in part by strength. A combination of corrosion
Beck and Jankowsky v(7), who note a resistance and high cryogenic toughness
Copyright
strong relationship bybetween ASTM
increased Int'l (all their application
has prompted rights reserved);
in areas Mo
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212 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

FIG. 3—Fatigue Strength Versus Bolt Strength of AISI 8740 Material.


Test specimens heat treated to Re 50, cadium fluoborate plated, and baked at 375 F for 23 hr
were subjected to a sustained load at 90 per cent of their notched tensile strength. Tension speci-
mens had a notch stress concentration factor of Kt = 4.9.

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HOOD AND SPROAT ON ULTRAHIGH-STRENGTH STEEL FASTENERS 213

FIG. 4—Comparison of Hydrogen Embrittlement Susceptibility of 4340 and H-ll Steels.


Improvement from cold working and thread form design approach endurance stress of H-ll
smooth bar.

TABLE 3—MATERIAL AND BOLT PROPERTIES OF H-ll AND


MARAGING STEEL, 300.
H-ll Maraging Steel, 300
Room -320F Room -320 F
Temperature Temperature

SPECIMEN

UTS psi 279,000 302,000 283,000 354,000


Yield strength psi 240,000 263,000 272,000 327 000
Elongation, *% 11.5 10.2 10.7 10.0
Reduction of area, % 42.0 39.0 53.3 44.3
Charpy impact ft-lb° 5.0 1.5 5.7 3.4

BOLT

UTS, psi 280,000 297,000 279,000 352,000


Fatigue-cycles, maximum stress 135,000 psi. 100,000 65,000 43,000 25,000
Tension impact, ft-lb, 1-28 bolt 50 37 50 44
0
Subsize specimen per ASTM E 23, Type W.

such as the liquid gas section of rocket with properties developed by heat
engines. They have also been considered treatment alone. The alloy is essentially
for elevated temperature structures, an iron base, chromium-cobalt-molyb-
where it is necessary to match the coeffi- denum material. Limited data on bolting
cients of expansion of both bolt and joint has shown it to have a nominal ultimate
materials. strength of 294,000 psi at room tem-
A new alloy (10), AFC77, shows perature, falling off to 246,000 psi at
promise of providing
Copyright by ASTM a Int'l
stainless 900 F (n).
high- reserved);
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strength bolting material
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214 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

bolts in the 260,000-psi category. Al- Steel Co., was selected. The factors
though their notched strength, Kt = 6, governing the selection of fastener
is higher than that of H-11 at this materials were considered and one or
strength level (1.5 at 276,000 psi versus another of many alloys was rejected.
1.1 at 288,000 psi for H-11) (12), they Since the development of a 300,000-
offer no particular advantage over H-11 psi fastener, new materials have shown
and actually have some disadvantages. promise; the comparative properties of
The resistance to temperature is lower three alloys are shown in Table 4. A few
for these steels as a result of a lower aging words are necessary to describe the last
temperature. two materials in more detail. Maraging
Susceptibility to hydrogen embrittle- 325 steel is a higher titanium modifica-
ment of maraging steels appears to be tion of the maraging steel series, and
greater than that of H-11. Notched limited data indicate that it may be
tension specimens, Kt = 4.9, of the capable of achieving sufficient properties
maraging steel (300) were cadmium- as a fastener to warrant its use in this
fluoborate plated and not baked. They capacity. However, further research will
failed during loading to 90 per cent of be necessary before it is regarded as

TABLE 4—ULTRAHIGH-STRENGTH BOLTING MATERIALS.


Property Vasco Jet MA Maraging 325 Ausformed H-11

UTS psi 311,600 344,000 371 000


Yield strength, psi. 252 000 332,000 305 000
Elongation % 84 10 0 12 0
Reduction of area. % 31.7 48.5 47.0
Bolt UTS, psi. 307,800 330,000 360,000

notched ultimate tensile strength. H-11 suitable. The ausformed H-11 data show
steel under the same conditions still had thread properties only, since techniques
not failed after 550 hr, when the test have not as yet been developed to fabri-
was terminated. cate heads on ausformed steels at this
The one possible area where maraging strength level. The highest thread prop-
steels may offer an advantage is in the erties to date, 392,000 psi, have been
area of cryogenic applications. Note in obtained on ausformed Vasco Jet MA
Table 3, however, that fasteners of H-11 (13). It is for this reason that ultrahigh-
tested at —320 F stand up quite well. strength bolting with a strength as high
Only when the Charpy impact values of as 400,000 psi may be practical in the
the two materials are compared, how- future. To provide some perspective to
ever, does the maraging steel show a the problem, however, it is necessary to
superiority at the lower temperature. consider that threads must be rolled
It would be recommended for use at after heat treatment to achieve both'
— 320 F on the basis of current knowl- tensile strength and high fatigue life in
edge. the bolt. Quench and temper treatments
The selection of a bolting material for will not produce bolts at this strength
300,000 psi narrows the choice consider- level because of high notch brittleness.
ably. It was only after several years of Accomplishing the thread rolling on a
research that Vasco Jet MA, a modified steel whose hardness is Re 63 is a large
tool Copyright
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by ASTMby Vanadium
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HOOD AND SPROAT ON ULTRAHIGH-STRENGTH STEEL FASTENERS 215

FIG. 5—Effect of Bolt Design on Endurance Limit Stress of 220,000-psi H-ll Bolts.
Bolts are tested in tension-tension fatigue at loads cycling between 10 and 100 per cent of maxi-
mum load.

FIG. 6—Endurance Limit as a Function of Bolt Tensile Strength.


Uncontrolled atmospheres resulting in carburization or decarburization reduces bolt fatigue
life. The bolts were tested in tension-tension fatigue at loads cycling between 5,250 and 52,500 psi.
Bolt Copyright by rolled
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Int'l heat
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216 STRUCTURE AND PROPERTIES or ULTRAHIGH-STRENGTH STEELS

BOLT DESIGN AND PROCESSING fatigue tests are normally run with the
To produce reliable bolts of the load varying between a maximum stress
strength levels indicated above, it is and 10 per cent of that maximum stress.
the function of bolt design and process- This choice parallels as nearly as possible
ing to maintain as great a percentage the worst condition of bolt fatigue,
of the base material properties as pos- namely, a loose bolt and nut. For con-

FIG. 7—Fatigue Life of AISI 4037 Steel Bolts as a Function of Carbon Content of Heat Treating
Atmosphere.
Failure occurred in 30 min.

sible. Bolts must be designed to mini- venience, only the maximum stress is
mize stress raisers, such as sharp notches usually reported.
and abrupt changes in cross sectional The development of maximum endur-
areas. Processing should be controlled ance limit stress in bolting has been
to prevent metallurgical damage and to going on for several years. A history of
create beneficial residual stresses in this development can be considered for
critical areas. the 220,000-psi bolt. The tension-tension
Since bolts are subjected to tension- fatigue endurance limit for a smooth
tension fatigue in application, bolt tests bar of H-ll is estimated at 130,000 psi.
are conducted
Copyright toby simulate
ASTM this
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(all rights The endurance
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HOOD AND SPROAT ON ULTRAHIGH-STRENGTH STEEL FASTENERS 217

thread rolled before heat treatment is vestiges of carburization or decarburiza-


20,000 psi. The S-N curves of Fig. 5 tion, but also to remove surface imper-
illustrate what has been necessary to fections present in the raw material,
restore a large proportion of this fatigue establish finished dimension, and create
life. Stressing of the thread roots by a smooth surface finish. Grinding of
rolling threads after heat treatment hardened steel can result in grinding
nearly tripled the fatigue endurance
stress. Increasing of thread root radius
added another increment to reach 85,000
psi (14). This is the fatigue level of the
existing 220,000 psi bolting on the mar-
ket today. Recent research on minimiz-
ing stress concentration peaks in the
engaged thread has resulted in a high
fatigue thread form which has raised
the endurance stress to 105,000 psi.
Needless to say, it has been necessary to
cold work the head-to-shank fillet area
as well, since this became the critical
point of failure as soon as threads were
rolled after heat treatment. The ultimate
goal continues to be that of restoring all
the fatigue endurance lost when the
transition was made from a smooth bar
to a bolt.
Another means of increasing fatigue
endurance has been to increase bolt
strength as shown in Fig. 6. The result
is that the 300,000-psi bolt has an en-
durance stress of 125,000 psi. It should
be pointed out, however, that this result
has been achieved only with the large-
radius thread form and rolling of threads
after heat treatment.
The manufacture of ultrahigh-strength FIG. 8—Stress-Alloy Cracking of a Cadmium
bolts must be closely controlled in order Plated Bolt Exposed to 700 F and a Stress Equal
that the properties anticipated by design to 90 Per Cent of the Ultimate Strength of the
are retained in the final product. The Bolt.
influence of surface carbon on tension
tension fatigue can be appreciable, as burns and high tension stresses or cracks.
shown in Fig. 7 (10), and both carburized The high tension stresses alone can pro-
and decarburized surfaces must be duce premature fatigue failure or re-
eliminated. duced tolerance for hydrogen. A stand-
In spite of raw-material control and ard practice therefore is to temper all
heat-treat atmosphere vigilance, the bolt blanks after grinding at a tempera-
body, underhead, and thread roll di- ture of 25 F below the original tempering
ameter are all ground after heat treat- temperature.
ment. This isbynotASTM
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218 STRUCTURE AND PROPERTIES OF ULTRAHIGH-STRENGTH STEELS

common in high-strength bolting. Cad- It can be seen that ultrahigh-strength


mium is the normal plate, but aluminum bolts are made under conditions predi-
has been used on occasion. Although cated by bolt properties and not neces-
cadmium fiuoborate plating followed by sarily by material or design character-
baking for 23 hr at 375 F is currently istics utilized for other structures. In
used on 220,000-psi bolting, the pro- addition, environmental conditions can
posed military 220,000-psi bolt requires affect bolt fatigue just as they affect
vacuum cadmium plating. This is an material fatigue. The endurance limit
added precaution in spite of the reduced stress in 90 per cent moisture has been

FIG. 9—Effect of Protective Coating on the Fatigue Life of 220,000 psi H-11 Bolts in 90 Per Cent
Moisture Environment.

susceptibility of H-11 steel to hydrogen reduced from 85,000 psi to 80,000 psi,
embrittlement. Steel bolting at 260,000 as shown in Fig. 9. Studies of this phe-
psi and 300,000 psi is vacuum cadmium nomenon have resulted in the develop-
plated as a standard practice. Elevated- ment of a protective coating. The coat-
temperature exposure of cadmium-plated ing has not only restored fatigue life to
bolts under load at a temperature at or its original level but increased the en-
close to the melting point of cadmium durance stress to 120,000 psi.
(610 F) has resulted in stress-alloy crack- With all that can be provided in the
ing, as shown in Fig. 8. This has neces- ultrahigh-strength steel bolt, its life in
sitated the use of a nickel-cadmium the structure is also affected by joint
diffused plate for high-temperature design and proper tightening. Utilization
bolts. Aluminum has been used for the of this hardware requires a proper under-
sameCopyright
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standing of these factors.
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HOOD AND SPROAT ON ULTRAHIGH-STRENGTH STEEL FASTENERS 219

REFERENCES

(1) W. Schlicting, "Effect of Tensile Strength (7) W. Beck and E. Jankowsky, "Delayed
vs. Thread Engagement of Socket Head Brittle Failure in Cadmium Plated Steels,"
Cap Screws," SPS Lab Report No. 707, Metals Progress, Vol. 84, No. 2, August,
November 10, 1961. 1963.
(2) Gregory W. Gries, "Area Determination (8) Thomas C. Baumgartner, "EWB TM9
for Tensile Strength of Socket Head Cap External Wrenching Bolt, EWN TM9
Screws; Sizes #0-80, #1-72, #2-56, #3- Flexloc Locknut," SPS Lab Report No. 86,
48, #4-40, and #5-40," SPS Lab Report May 7, 1957.
No. 796, March 27, 1962. (9) A. W. Dickens, "Evaluation of SPS EWB
(3) Gregory W. Gries, "Area Determination 926 Bolts and SPS FN926 Locknuts,"
for Tensile Strength of Socket Head Cap SPS Lab Report No. 283, June 8, 1960.
Screws with Threads Rolled Before and (10) A. Kasak, V. K. Chandhok, J. H. Moll,
After Heat Treat; Sizes #6-40, #10-32, and E. J. Dulis, "Development of High-
and ^-20 at Strength Levels of 160,000, Strength Elevated-Temperature Corrosion-
180,000, and 200,000 psi," SPS Lab Report Resistant Steel," Crucible Steel Company
No. 835, July 10, 1962. of America, ASD Contract No. AF33(657)-
(4) Gregory W. Gries, "Area Determination 8458, November 1, 1962.
for Tensile Strength of Socket Head Cap (11) J. Glackin, "Bolt and Material Evaluation
Screws; Sizes #6-40 and #10-32 with Hi- of AFC 77 Material to 1200°F," SPS Lab
Life, HiR 75%, and HiR 55% Thread Note No. 822, April 22, 1963.
Forms, Rolled Thread Before and After (12) D. E. McGarrigan, "Susceptibility of Vasco
Heat Treat," SPS Lab Report No. 858, Max 300 to Hydrogen Embrittlement."
August 23, 1962.
SPS Lab Note No. 845, June 17, 1963.
(5) Thomas C. Baumgartner, "Basic Design
(13) J. Glackin, "Progress Report on Aus-
and Manufacturing of Aircraft Fasteners
for Use Up to 1600°F," SPS Lab Report formed Material from Ford Motor Com-
No. 2300, December 17, 1958. pany," SPS Lab Report No. 759, February
(6) J. Laurilliard, "Hydrogen Embrittlement 21, 1962.
of 4340 Material Compared to SPS-M-107 (14) E. Gowen, Jr., "Test Data of 220,000 and
Material," SPS Lab Note No. 581, Novem- 260,000 psi SPS Hi-Life Bolts," SPS Lab
ber 28, 1961. Report No. 998, May, 1963.

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DISCUSSION

A. R. JOHNSON1—It was a pleasure to J. T. BiNGHAM2—The authors' data


read the history behind the development on 19 per cent maraging steel, indicating
of ultrahigh-strength fasteners, since it fatigue life lower than H-ll, and their
clearly shows how persistent efforts to data on cadmium plate embrittlement
optimize processing and design can with the same results, are open to ques-
achieve maximum performance from tion. Extensive testing of various sizes
ultrahigh-strength materials like Vasco- of bolts made from several heats of
Jet 1000 and Vascojet M-A. In this materials by our company have shown
connection, Figs. 5 and 6, showing the more favorable results. Successful pro-
incremental gains in fatigue strength duction of parts does require close and
with improvements in design and proc- precise control of forming and processing
essing, are particularly interesting. as mentioned by the authors.
It is encouraging to note that the E. J. DuNN3—In bolting applications,
authors see some promise in the new are transverse properties important?
18 per cent nickel maraging steels as A. C. HOOD AND R. L. SPROAT (authors1
ultrahigh-strength fasteners. There are closure)—A. R. Johnson's comments are
some very definite advantages inherent indeed appreciated. With regard to his
in these steels; for example, their tough- question on Charpy impact values shown
ness at cryogenic temperatures, which in Table 3, the original paper showed
the authors have pointed out. In addi- Charpy values for a subsize specimen
tion, however, the simplest heat treat- per ASTM E 23, Type W. Subsequent
ment, 2 hr age at 900 F, and relatively tests, shown below, indicate values essen-
small dimensional change on aging, tially the same as those noted by John-
—0.0004 in./in., should be helpful from son:
a manufacturing standpoint. I would
H-ll Maraging Steel 300
like to point out that Charpy V-notch
impact tests run at the Vanadium-Alloys Room -320° F Room -320° F
Steel Company laboratory on a cali- Charpy Im-
brated impact tester have shown con- pact, full
siderably higher impact strength for the size 13.5 3 16.6 10.7
maraging (300) steel than those reported
by the authors in Table 3—18 ft-lb at The authors are grateful to J. T.
room temperature and 10 ft-lb at —320 Bingham for commenting on the work
F. On the basis of these test results, the of his company in the area of high-
maraging steel might be expected to strength bolts. Numerous attempts at
show substantially greater resistance to SPS to achieve a fatigue life in the
shock loadingbythan other steels. maraging steel bolt comparable-to H-ll
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bolts of the same strength level and
1 2
University
Manager ofof Washington
research, Washington)Hipursuant
(University ofSteel
Vanadium-Alloys Shear Corp., Torrance,
to License Calif. No further reproductions
Agreement.
3
Co., Latrobe, Pa. Westinghouse Corp., Blairsville, Pa.
220
DISCUSSION ON ULTRAHIGH-STRENGTH STEEL FASTENERS 221

design were not successful. This was satisfactory, providing proper precau-
based on tests run with threads rolled tions are taken with respect to hydrogen.
after heat treatment, customary for It is the authors' contention that steels
high-strength bolting. In addition, rotat- of the strength level of which the marag-
ing-beam fatigue tests of H-ll and ing steels are capable should be vacuum-
maraging steels run by Vanadium Alloys cadmium plated to avoid the pick-up of
Steel Co.4 resulted in a lower endurance hydrogen completely. It is generally
limit stress for the maraging steel. accepted that susceptibility to hydrogen
The tests on hydrogen embrittlement embrittlement increases with increase in
of maraging steel notched specimens, tensile strength.
Kt = 4.9, was not intended to indicate Generally speaking, the transverse
that maraging steel fasteners could not properties of a material are not the
be electroplated. Rather, it was an ex- major factor affecting the properties of
periment to establish whether the marag- a bolt.
ing steels are susceptible to hydrogen, Longitudinal material properties con-
and if so, to what degree. Numerous trol the properties of bolting. However,
bolt products are made everyday which bolt manufacturing operations, such as
are cadmium plated, and the results are upsetting and thread rolling, are affected
4
Private communication with D. Yates, Va- by the transverse properties of the raw
nadium Steel Co. material.

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tHIS PUBLICATION IS ONE OF MANY
issued by the American Society for Testing and Materials
in connection with its work of promoting knowledge
of the properties of materials and developing standard
specifications and tests for materials. Much of the data
result from the voluntary contributions of many of the
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Over the years the Society has published many tech-
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on request.

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