The Effect of Heat Treatment on Microstructure and

Cryogenic Fracture Properties in 5Ni and 9Ni Steel

J. R. STRIFE AND D. E. PASSOJA

Heat treatments were utilized in 5Ni and 9Ni steel which resulted in the development of
tempered microstructures which contained either no measurable retained austenite (<0.5
pct) or approximately 4 to 5 pct retained austenite as determined by X-ray diffraction.
Microstructural observations coupled with the results of tensile testing indicated that the
formation of retained austenite correlated with a decrease in carbon content of the matrix.
Relative values of K t c at 77 K were estimated from slow bend precracked Charpy data using
both the COD and equivalent energy measurements. In addition, Charpy impact properties
at 77 K were determined. In the 9Ni alloy, optimum fracture toughness was achieved in
specimens which contained retained austenite. This was attributed to changes in yield and
work hardening behavior which accompanied the microstructural changes. In the 5Ni alloy,
fracture toughness equivalent to that observed in the 9Ni alloy was developed in grain
refined and tempered microstructures containing <0.5 pct retained austenite. A decrease in
fracture toughness was observed in grain refined 5Ni specimens containing 3.8 pct retained
austenite due to the premature onset of unstable cracking. This was attributed to the
transformation of retained austenite to brittle martensite during deformation. It was
concluded that the formation of thermally stable retained austenite is beneficial to the
fracture toughness of Ni steels at 77 K as a result of austenite gettering carbon from the
matrix during tempering. However, it was also concluded that the mechanical stability of the
retained austenite is critical in achieving a favorable enhancement of cryogenic fracture
toughness properties.

THE need for materials to contain liquefied gases has
steadily increased in recent years. Low carbon ferritic
nickel alloy steels have been developed for use in
cryogenic structural applications with costs being min-
imized by selecting the appropriate nickel content for
the intended service temperature range. In general, 9Ni
steel has received wide acceptance for liquefied natural
gas and nitrogen tankage due to its relative ease of
production and good weldability. Recently, ~,25Ni steel
has been proposed as a lower cost replacement for 9Ni
steel in such applications and therefore is an alloy of
considerable interest.
Austenite retention after heat treatment has been
considered to play a key role in achieving low temper-
ature toughness in Fe-Ni alloys since the development
of low carbon 8 to 10 pct nickel steels for cryogenic
service by Brophy and Miller? Marshall, et a[ 4 sug-
gested that retained austenite increased low temperature
toughness in 9Ni steel by scavenging carbon and other
deleterious elements from the ferritic matrix. More
recently, Norstrom 5 found that cementite precipitation
was eliminated as a result of retained austenite for-
mation in 9Ni steel and that this produced a cor-
responding decrease in the DBTT. A mechanism other
than a scavenging effect seems to be supported by
recent reports 6,7 in low carbon, titanium gettered Fe-Ni
alloys. The presence of retained austenite in such
systems was shown to have beneficial effects on tensile
J. R. STRIFE, formerly with Union Carbide Corporation, Tarry-
town, NY, is now Research Scientist at United Technologies Research
Center, East Hartford, CT 06108. D. E. PASSOJA is Senior Research
Scientist, Union Carbide Corporation, Central Scientific Laboratory,
Tarrytown, NY 10591.
Manuscript submitted July 23, 1979.
ISSN 0360-2133/80/0811-1341500.75/0
METALLURGICAL TRANSACTIONS A 9 1980 AMERICAN SOCIETY FOR METALS AND
THE METALLURGICAL SOCIETY OF AIME
ductility, Charpy impact toughness, and the DBTT.
Schwartz 8 has suggested that low temperature toughness
increases as a function of retained austenite in 9Ni steel
due to a TRIP mechanism operative at the crack front.
Sarno, et al ~ concluded that retained austenite con-
tributes to toughness in 5Ni steel by depleting the
matrix of interstitials and by simply increasing the
amount of fcc phase which possesses higher resistance
to cleavage fracture.
Other results have been reported which are somewhat
contradictory. Pampillo and Paxton 9 reported a bene-
ficial effect of retained austenite on tensile ductility but
no effect on impact properties in maraging steels.
Hwang, et al 7 reported that retained austenite improved
tensile elongation and Charpy impact energy at cryo-
genic temperatures in fine grained 12Ni titanium
gettered alloys but produced a decrease in K t c . Samples
containing retained austenite showed increased suscep-
tibility to unstable crack propagation. Finally, Ooka, et
allo found no quantitative relationship between retained
austenite and low temperature toughness.
It is evident from this brief review that the influence
of retained austenite on the material toughness meas-
ured by various methods is complex and not well
understood. In addition, in many previous studies the
effect of reduced strength due to tempering of the
martensitic structure has been neglected in interpreting
the role of retained austenite. A program was instituted
in our laboratory to define the microstructural mech-
anism responsible for high toughness in Ni steels by
first considering quench and temper treatments in both
5Ni and 9Ni steel, and then by considering the more
complicated 3-step heat treatments in 5Ni steel. In
particular, an attempt was made to clarify the role of
VOLUME 11A, AUGUST 1980--1341
martensite tempering in conjunction with retained aus-
tenite formation in both alloys.
EXPERIMENTAL PROCEDURE
Materials
Conventionally heat treated 5Ni and 9Ni plate ap-
proximately 13 mm in thickness was received from the
A R M C O Steel Corporation. The chemical compositions
as determined in our laboratory are listed in Table I.
Microstructural Characterization
Specimens to be investigated optically were mounted
in epoxy and polished using standard metallographic
techniques. Specimens to be used for observation by
transmission electron microscopy were prepared from
sections cut parallel to the fracture surface of Charpy
specimens. Disks of 3 mm diam were spark machined
from the sections and chemically thinned in a dual
submerged jet polisher using a chromic-acetic electro-
lyte. The thin foils were examined in a JEOL electron
microscope operated at 200 KV.
Quantitative measurement of the amount of retained
austenite was determined by X-ray diffraction methods.
The peak pair technique of Durnin and RidaP ~was
adopted and a standard procedure using a copper X-ray
tube and graphite monochromator was implemented.
Samples for X-ray measurement were polished metallo-
graphically and deeply etched to remove the disturbed
metal resulting from polishing. In general, three deter-
minations of retained austenite content were made for
each heat treatment. The relative integrated areas under
the austenite peaks indicated that any texture effects
were minimal. The accuracy of this technique was
estimated as + 0.5 pct.
Heat Treatment
To establish heat treating parameters, the critical
temperatures were determined from dilatometric meas-
urements on specimens which had been austenitized at
1173 K and water quenched. The A c, and A c, temper-
atures were defined as the first deviations from linear
thermal expansion behavior. These were determined as
923 and 1073 K for the 5Ni steel, and 863 and 1013 K
for the 9Ni steel.
In the 9Ni alloy, austenitizing was performed at
1116 K to remove the effects of prior heat treatment
log tempering time. The amount of retained austenite
observed after heat treating exhibits a maximum as a
function of time. The time at which the amount of
retained austenite is maximized at a given tempering
temperature decreases as the tempering temperature
increases. This result can be understood by considering
that the initial austenite which forms will be rich in
alloy content. As the time at the tempering temperature
increases, austenite continues to grow but the solute
redistributes itself over a larger volume of austenite.
Thus, the alloy content of the austenite at the tempering
temperature decreases causing the stability of the aus-
tenite to decrease as the time at temperature increases.
At some point, the austenite stability is reduced to a
level which, when cooled to low temperature, will
readily transform to martensite, resulting in a decrease
in the volume of austenite retained at low temperature.
As the tempering temperature increases, austenite
growth increases concomitantly, and the austenite sta-
bility is reduced for shorter aging times. Tempering
temperatures of 863 and 813 K were selected for the 9Ni
alloy from these data to produce tempered martensitic
microstructures with and without retained austenite.
Time at temperature was limited to the linear portions
of these curves to prevent formation of untempered
martensite on quenching.
The heat treatment for 5Ni steel as developed by
A R M C O L2 is a relatively complex three-step treatment
which involves !) austenitizing and water quenching,
2) reheating into the A c,-Ac, range to form a lamellar
structure and water quenching, 3) reheating to just
above the A c, and air cooling or quenching. The final
microstructure is composed of ferrite, tempered marten-
10
9
uJ 893K
I---
8
I,g
I-r 7
/ / 1 3 K
rgJ 6
z_ 5
<
I-
4
3

2 /
and to produce a martensite packet size of approxi- o I | I I
o lO 10 2 10 3 10 4 10 5
mately 10 ttm. A series of tempering treatments was TEMPERING TIME [MINUTES]
implemented in order to alter the formation of retained Fig. 1--Pet retained aus,!.enite v s tempering time for 9 pet Ni steel
austenite. The data obtained from these treatments are quenched from 1116 K and tempered at the indicated temperatures
plotted in Fig. 1 as percent retained austenite at 77 K v s followed by quenching to 77 K.

Table I. Composition of the Alloys, Wt Pct

Nominal Ni C N Mn Mo Si AI S P Fe
5Ni 5.05 0.085 0.017 0.52 0.28 0.21 0.046 0.009 0.022 bal
9Ni 9.10 0.084 0.035 0.54 0.065 0,19 0.038 0.011 0.026 bal

1342--VOLUME 11A, AUGUST 1980 METALLURGICAL TRANSACTIONS A

site, and retained austenite. For the purposes of this
investigation, an austenitizing treatment of 1 h at
1158 K was selected. This produced a martensite packet
size of approximately 10/~m. The changes which
occurred in the microstructure during reheating were
then investigated. Reheating at 873 K resulted in no
detectable austenite growth, and thus represented a
quenched and tempered structure. In specimens re-
heated 1 h at 923 K, initial austenite growth from the
martensitic packet boundaries was observed. Approx-
imately 2 pct was retained after quenching. At pro-
gressively higher temperatures, more extensive austenite
growth was observed, but this austenite was not stable
at 77 K. For a reheating treatment of 1 h at 1008 K,
approximately 50 pct of the microstructure had de-
composed to austenite at the reheating temperature
resulting in the formation of a refined lamellar grain
structure. No retained austenite was detected after
quenching in this microstructure. Based on these results,
two step quench and temper treatments utilizing
tempering temperatures of 923 and 873 K were defined
with the objective Of producing tempered martensitic
microstructures with and without retained austenite. In
addition, three step treatments using a second step of
1 h at 1008 K and third step tempering at 923 and 873 K
were designated to produce refined tempered micro-
structures with and without retained austenite.
Mechanical Testing
Mechanical properties at 77 K were determined using
an INSTRON servohydraulic testing system equipped
with a cryostat to maintain liquid nitrogen temperature.
Tensile properties were determined using round tensile
specimens having a 25.4 mm gage length and 6.4 mm
gage diam. Testing was performed at a strain rate of
10-3 S-I.
Fracture toughness parameters at 77 K were deter-
mined via slow bend testing of fatigue precracked
Charpy specimens. Standard size Charpy blanks were
machined in the transverse orientation (crack growth
direction normal to the plate rolling direction) and were
fatigue precracked at room temperature according to
the proposed British standard) 3 Although such simple
dimensions do not provide valid plane strain conditions,
the plane strain fracture toughness, Ktc, may be esti-
mated from the plots of load vs crack opening dis-
placement (COD) in the following manner. The crack
tip opening displacement, 6, is obtained from the
relation:
= K2( 1 - p:) + 0.4(W - a) V
2oyE 0.4W + 0.6a + Z
where K is the stress intensity associated with three
point bending, ~4p is Poisson's ratio, Oyis the yield
strength, E is Young's modulus, W is the specimen
depth, a is the crack length, Z is the distance of the clip
gage from the test piece surface, and V is the plastic
component of the clip gage opening displacement. K~c
may then be estimated from the relation:
GIC = oy~ = ~K~c (1 _ p2)or
METALLURGICAL TRANSACTIONS A
= [ oySE ]1/2
K;c tl -
In addition to this procedure, the equivalent energy
approach 15for estimating Kzc from nonlinear load-
displacement curves was utilized. In this approach, the
plane strain fracture toughfiess, Ktc, is estimated from
the relation:
egsf(a/w) (A1~ 1/2
K IEC= B w3/2 k~ ]
PQ is the 5 pct secant load, 14s is the span width,f (a/w)
is the geometric shape factor defined by ASTM speci-
fication, a is the crack length, w is the specimen depth,
and B is the specimen thickness. A ~is the area under
the load-displacement curve up to the maximum load
and A 2 is the area under the curve to the load Pc"
Experimental evidence7,16suggests that the equivalent
energy approach provides an accurate estimate of Ktc
in similar materials.
The Charpy impact properties were also determined
at 77 K using standard size Charpy V-notch specimens
machined with the notch orientation transverse to the
plate rolling direction. The impact tests were conducted
in accordance with ASTM standards? 2
RESULTS AND DISCUSSION
Microstructure
To investigate the effect of retained austenite for-
mation on carbide precipitation in 9Ni steel, two
tempering treatments were selected. These were 1 h at
813 K (<0.5 pct retained austenite) and 1 h at 863 K
(5.2 pct retained austenite). Shown in Fig. 2 are optical
micrographs of polished and etched specimens for these
two tempering treatments. Extensive carbide precipi-
tation is observed at the martensite packet boundaries
as well as in the packet interiors for the specimen
containing <0.5 pct retained austenite, Fig. 2(a). In the
specimen containing 5.2 pct retained austenite, Fig.
2(b), the carbide precipitation is much less extensive.
The retained austenite appears as globules on the
packet boundaries.
The microstructures for an as-quenched specimen
and these two tempering treatments were also char-
acterized using transmission electron microscopy. In the
as-quenched structure, heavily dislocated martensite
laths were grouped in parallel arrays and no carbide
precipitation was observed. On tempering for 1 h at
813 K, partial dislocation recovery and widespread
carbide precipitation occurred. A typical structure is
shown in Fig. 3(a). The dislocation density varied from
lath to lath, and carbides were observed as films at lath
boundaries (A) and as precipitates in lath interiors (B).
Such observations are typical of tempered martensites.
On tempering for 1 h at 863 K, Fig. 3(b), recovery was
more advanced and some relatively dislocation free
grains appeared. The general lath structure still
remained, but the structure was more equiaxed. Much
less carbide precipitation was observed and in partic-
ular, the carbide films as observed in Fig. 3(a) no longer
existed. These observations coupled with the optical
VOLUME 11A, AUGUST 1980-- 1343
Fig. 2--Optical micrographs of quenched and tempered 9 pct Ni
steel. (a) Tempered 1 h at 813 K. Note widespread carbide
precipitation. (b) Tempered 1 h at 863 K. Carbide precipitation and
retained austenite globules are seen primarily at the martensite
packet boundaries.
microscopy results suggest that retained austenite acted
as a sink for carbon in the 9Ni alloy.
In the 5Ni steel, tempering at 873 K (<0.5 pct
retained austenite) produced a microstructure which
was indistinguishable from the 9Ni alloy tempered at
813 K. An optical micrograph of a polished and etched
specimen, Fig. 4(a), shows extensive carbide precipi-
tation both at the packet boundaries and in grain
interiors. Observations in TEM showed that the as-
quenched martensitic structure was identical to that in
9Ni and that tempering at 873 K resulted in partial
dislocation recovery and extensive carbide precipita-
1344--VOLUME 11A, AUGUST 1980
Fig. 3--Transmission electron micrographs of the structure observed
in quenched and tempered 9 pct Ni steel. (a) Tempered for 1 h at
813 K. Note carbide film at lath boundaries (A) and carbide
precipitation in lath interiors (B). (b) Tempered for 1 h at 863 K. Note
the presence of some relatively dislocation free grains and carbide
precipitation.
tion. Tempering treatments at 923 K which produced
retained austenite were also investigated. It was dis-
covered, however, that the austenite which formed at
the tempering temperature was relatively unstable, so
that a maximum of 2 pct was retained on quenching in
liquid nitrogen. An optical micrograph for a sample
tempered 6 h at 923 K, Fig. 4(b), illustrates the fact that
austenite present at the tempering temperature effec-
tively gettered carbon from the ferritic matrix. Note
that no carbide precipitation is observed in the grain
interiors. The packet boundaries are covered with
patches of untempered martensite transformed on
METALLURGICAL TRANSACTIONS A
Fig. 4--Optical micrographs of quenched and tempered 5 pct Ni steel.
(a) Tempered 24 h at 873 K. Note widespread carbide precipitation.
(b) Tempered 6 h at 923 K. The packet boundaries are decorated with
untempered martensite. No carbide precipitation is observed.
quenching from the tempering temperature.
As was previously discussed in the experimental
procedure section, a heat treatment of 1 h at 1158 K,
water quench, followed by 1 h at 1008 K, water quench,
produced a refined lamellar grain structure in the 5Ni
alloy. After this treatment, the structure consisted of
approximately 50 pct tempered ferrite and 50 pct fresh
martensite. As a third step in heat treatment, specimens
were reheated for 1 h at 873 K to produce a tempered
structure, and 1 h at 923 K for development of retained
austenite in combination with tempering. X-ray meas-
urement showed that these treatments produced %0.5
pct and 3.8 pct retained austenite respectively. Obser-
vations in light microscopy, Fig. 5, showed that these
METALLU RGICAL TRANSACTIONS A
Fig. 5--Optical micrographs of 5 pct Ni steel representative of three
step heat treatments. (a) 1 h 1158 K, wq, 1 h 1008 K, wq, 1 h 873 K,
wq. <0.5 pct retained austenite detected. (b) 1 h 1158 K, wq, 1 h
1008 K, wq, 1 h 923 K, wq. Retained austenite was 3.8 pct.
treatments both produced a very refined microstructure
which appeared partially lamellar and partially
equiaxed. The average grain size determined from TEM
micrographs of these microstructures, Fig. 6, was less
than 1/~m. This represents an order of magnitude
reduction in grain size when compared to the quenched
and tempered microstructure, Fig. 4(a), since the effec-
tive grain size in the quenched and tempered micro-
structure is the martensite packet size which was
determined to be 8/~m.
The microstructural features associated with the three
step treatments were also investigated using TEM.
Shown in Fig. 6(a) is a representative micrograph for a
specimen tempered 1 h at 873 K as the third step.
VOLUME 11A, AUGUST 1980-- 1345

Fig. ~-Transmission electron micrographs of the structure observed
in 5 pct Ni steel for three step heat treatments 9 (a) 1 h at 873 K for the
third step. Carbide precipitation designated by arrows. Grain bound-
ary precipitate consisting of elongated carbide and possibly retained
austenite at A. (b) 1 h at 923 K for the third step. Both elongated and
equiaxed grains are seen with little evidence of carbide precipitation9
Extensive carbide precipitation was observed as des-
ignated by arrows on the micrograph. In addition, a
laminar precipitate was observed at some grain bound-
ary locations as shown at position A on the micrograph.
The morphology and contrast suggest that these are two
phase precipitates consisting of elongated carbides
coupled with films of retained austenite. Although
confirming electron diffraction evidence was not ob-
tained, the possibility that these are retained austenite
films must be considered since austenite distributed in
this manner at low volume fractions (~0.5 pct) would
go undetected using the X-ray diffraction techniques
1346--VOLUME 11A, AUGUST 1980
;~ i\.
Fig. 7--Transmission electron micrographs of the 5 pct Ni steel
showing retained austenite resulting from a three step heat treatment
utilizing 1 h at 923 K for the third step. (a) Bright field micrograph.
(b) Dark field micrograph using austenite diffraction spot as the
operating reflection. Retained austenite is located at the ferrite
boundaries9
described previously. In the specimens tempered 1 h at
923 K, Fig. 6(b), very little carbide precipitation was
observed, but retained austenite was readily docu-
mented using darkfield techniques. Figure 7(a) is a
brightfield micrograph and Fig. 7(b) the corresponding
darkfield micrograph using an austenite diffraction spot
as the operating reflection9 It can be seen that patches
of austenite decorate the ferrite grain boundaries. Thus,
it is apparent from a comparison of the microstructures
associated with the three step treatments that retained
austenite formation has effectively gettered the carbon
in the 5Ni alloy.
METALLURGICAL TRANSACTIONS A
 Cryogenic Tensile Properties 1400

The cryogenic tensile properties determined for the 1200

--D

alloys and their respective heat treatments are listed in A g

Table II. In the 9Ni alloy, the yield strength decreased

1000
as a function of increased tempering time or temper-
ature, while the ultimate tensile strength was relatively g.
IE 8O0
constant. Yield points were observed on all the tensile
curves. The difference between the upper and lower W
I:c
TEMPER TREATMENT
6O0 A. 9Ni 1 HR. 813K, wq
yield point decreased with increased tempering tem- u) B. 9Ni 1 HR. 863K. wq
perature such that the yield point was barely detectable C.
D.
5Ni
5Ni
1 HR.
1 HR.
1008K, wq, 1 HR. 873K, wq
1008K, wq, 1 HR. 923K, wq
400
in those specimens tempered at 863 K. This is illustrated
in Fig. 8. It is also evident that greater work hardening
200
occurs in the 863 K tempered specimen.
In the 5Ni alloy, a similar trend of decreasing yield
strength with increased tempering temperature or time % I
0.02
I
0.04
I
0.06
I
0.08
I
0.10
I
0.12
I
0.14 0.16
was observed. However, considerably greater softening STRAIN
occurred in the 5Ni alloy for the same increment of Fig. 8--Engineering stress-strain behavior up to the ultimate tensile
increased tempering temperature as was utilized in the strength demonstrating differences in yield and work hardening
9Ni alloy. For specimens tempered 1 h, a 50 K increase behavior at 77 K as a function of heat treatment.
in tempering temperature decreased the yield strength
263 MPa in the 5Ni alloy and only 139 MPa in the 9Ni
alloy. It may also be seen that equivalent yield strengths testing correlated with decreased evidence of carbide
are obtained in the 5Ni alloy for both the simple and precipitation. Since the formation of retained austenite
two step tempering treatments at the same final is concurrent with these observations, the conclusion
tempering temperature. Apparently the expected effect that thermally stable austenite formed during tempering
of grain size on yield strength was negated by the effectively getters carbon from the matrix is supported.
introduction of a duplex microstructure of ferrite and
tempered martensite by the two step temper. Yield
Cryogenic Fracture Properties
points were observed on the tensile curves for those
specimens tempered at 873 K, but they were not ob- The values of the fracture toughness parameter, K,c,
served for those tempered at 923 K. There were also calculated from slow bend testing of precracked Charpy
significant differences in the ultimate tensile strengths specimens at 77 K are presented in Table III. It is
achieved as a function of tempering treatment. A emphasized that these are not valid Ktc since the
consistent pattern of increased ultimate tensile strength specimen dimensions do not provide plane strain con-
in specimens containing retained austenite was ob- ditions during testing. The critical stress intensity fac-
served. Coupled with the much lower yield strengths tors,/('COD EE for fracture as defined by the crack
-~,c and K,c,
and relatively equivalent ultimate tensile strains, it is opening displacement and equivalent energy methods
clear that those specimens containing retained austenite respectively are both listed in Table III. The intent in
exhibit a significantly greater degree of work hardening both methods is to allow the definition of a critical
as shown in Fig. 8. These factors suggested that some stress intensity factor for fracture in alloy systems
degree of austenite to martensite transformation oc- exhibiting considerable plasticity prior to stable or
curred during tensile deformation at 77 K in those unstable crack extension. It is evident that although the
specimens containing retained austenite. methods yield different K,c values for a given
Finally, it is noted that the tensile test results are tempering treatment, the relative ranking of the Kzc
consistent with the microstructural observations dis- values with heat treatment is equivalent using either
cussed in the previous section. Diminished or complete method. The primary difference in the data is that a
elimination of a yield point phenomenon in tension larger range in Kic values is calculated using the COD

Table II. Tensile Properties at 77 K

Tempering %~ OUTS CUTS C/ Pct Retained

Alloy Treatment* (MPa) (MPa) Pet Pet Austenite
9Ni 1 h 813 K 1137 1161 9.8 22.2 (0.5
9Ni 24 h 813 K 1058 1125 13.0 25.6 4.1
9Ni 1 h 863 K 998 1157 12.4 24.3 5.2
5Ni 1 h 873 K 1118 1147 8.1 19.7 (0.5
5Ni 24 h 873 K 995 1056 13.2 26.0 (0.5
5Ni 1 h 923 K 855 1158 13.7 26.4 1.9
5Ni 1 h 1008 K, 1 h 873 K 1113 1110 13.0 26.4 (0.5
5Ni 1 h 1008 K, 1 h 923 K 859 1236 12.3 23.3 3.8
* Water quenching after each step.

METALLURGICAL TRANSACTIONS A VOLUME 11A, AUGUST 1980--1347

 matically increased. The specimens final tempered at
Table III. Values of the Fracture Toughness Parameter, Ktc, at 873 K containing <0.5 pet retained austenite exhibited
77 K Calculated from Slow Bend Precracked Charpy Data K~c values equivalent to those achieved in 9Ni spec-
imens containing 5.2 pct retained austenite. The energy
Tempering Ktc (MPa v-m) Pet Retained absorbed, although greatly improved, did not achieve
Alloy Treatment* Equiv. Energy COD Austenite the levels observed in 9Ni due to limited crack exten-
9Ni 1 h 813 K 177 210 <0.5 sion after maximum load was reached as shown in Fig.
9Ni 24 h 813 K 179 221 4.1 10. This dramatic change in fracture properties in the
9Ni 1 h 863 K 189 231 5.2
5Ni alloy could be attributed to the grain refinement
5Ni 1 h 873 K 99 87 <0.5 achieved by the intercritical heating at 1008 K and/or
5Ni 24 h 873 K 102 99 <0.5 the possible formation of fine retained austenite films at
5Ni 1 h 923 K 108 113 1.9
5Ni 1 h 1008 K, 1 h 873 K 190 226 <0.5
grain boundary locations during the final temper at
5Ni 1 h 1008 K, 1 h 923 K 130 156 3.8 873 K. However, the fact that both groups of 5Ni
specimens receiving the two step and three step heat
* Water quenching after each step.
treatments were final tempered at 873 K leads us to
conclude that the primary factor in improving the
toughness parameters measured was the grain refine-
method. Specifically, the upper end of the range is ment achieved by the intercritical tempering. In the
expanded indicating that the contribution of plasticity specimens tempered at 923 K where extensive retained
is of greater magnitude in the COD analysis. austenite formation occurred, inferior fracture proper-
In the 9Ni alloy, the data indicate that formation of ties to those determined for specimens tempered at
retained austenite produces a small increase in Ktc.
Significant differences were noted, however, in the
load-COD and load-displacement curves. In specimens
tempered I h at 813 K which contained no measurable
retained austenite, ductile crack extension was much
less than that observed in those specimens containing
15
~ / ~ '
1 HR. JB13K.wq

~ 1 HR. 863K. wq
retained austenite (Fig. 9). The net result was that the
9Ni specimens containing retained austenite exhibited
considerably more energy absorption as measured by
area under the load-displacement curve. These data are 10
listed in Table IV. The energies measured were cor- z

rected for crack length using the ductile fracture <[

equation developed for dynamic tear testing of steels. Is o
These results for the 9Ni alloy can be attributed to the
decreased yield strength and increased work hardening I
behavior associated with those tempering treatments I I

resulting in the formation of retained austenite.

In the 5Ni alloy, specimens quenched and tempered
exhibited brittle behavior with no ductile crack exten-
sion prior to catastrophic failure. This resulted in !
considerably lower fracture toughness and very low I
energy absorption when compared to quenched and I
L
tempered 9Ni as shown in Tables III and IV. This is o I I I i----""
1.0 2.0 3.0 4.0
observed since the alloy content of 5Ni is insufficient to CROSSHEAD DEFLECTION, mm
lower the DBTT below 77 K in this microstructure. In Fig. 9--Load-deflection behavior observed during slow bend testing
5Ni specimens receiving the two step temper treatment, at 77 K of precracked Charpy specimens of 9 pct Ni steel. Note
the fracture toughness and energy absorbed were dra- limited crack extension in specimen tempered at 813 K.

Table IV. Fracture Energy at 77 K

Tempering Slow Bend Charpy Impact Pet Retained

Alloy Treatment* 0oules) (joules) Austenite
9Ni 1 h 813 K 29.3 136 <0.5
9Ni 24 h 813 K 34.1 14l 4,1
9Ni 1 h 863 K 37.1 144 5.2
5Ni 1 h 873 K 4.0 17 <0.5
5Ni 24 h 873 K 4.2 28 <0.5
5Ni 1 h 923 K 6.2 37 1.9
5Ni 1 h 1008 K, 1 h 873 K 23.9 158 <0.5
5Ni 1 h 1008 K, 1 h 923 K 15.8 128 3.8
* Water quenching after each step.

1348--VOLUME 11A, AUGUST 1980 METALLURGICAL TRANSACTIONS A

873 K were measured. This was due to the premature
onset of unstable crack propagation as demonstrated in
Fig. 10. This phenomenon could be attributed either to
the transformation of retained austenite to martensite
during loading, or to the presence of brittle martensite
due to partial transformation of austenite on quenching
from the tempering temperature. Since the tensile test
results showed that grain refined 5Ni specimens
containing retained austenite had significantly lower
yield points and greater work hardening rates than
those that did not, it is concluded that the mechanism of
deformation induced martensite formation was respon-
sible for the decrease in fracture properties observed.
This indicates that the mechanical stability of the
retained austenite formed plays a key role in deter-
mining the low temperature fracture toughness.
Cryogenic Impact Properties
To further quantify the fracture behavior, Charpy
impact testing was performed at 77 K. This test rep-
resented fast fracture from a blunt notch whereas the
slow bend fracture toughness testing represented slow
crack propagation in the presence of a sharp notch. The
CVN properties determined are listed in Table IV. The
same trends observed in slow fracture were observed in
Charpy impact. Tempering of the 9Ni steel for 1 h at
813 K resulted in impact properties which were slightly
improved by treatments which introduced retained
austenite. In the 5Ni alloy, simple tempering resulted in
some gains in impact properties, but the levels achieved
were minimal compared to similar treatments in the 9Ni
alloy. Refinement of the structure by the two step
temper treatment resulted in dramatic increases in
impact properties to a level exceeding that obtained in
the 9Ni alloy. Introduction of retained austenite by
tempering at 923 K resulted in a decrease in impact
properties of the refined structure. Note that this
behavior was identical to that observed in the slow bend
testing and indicates that mechanically unstable
retained austenite decreases fracture toughness under
either slow crack growth or impact conditions.
SUMMARY AND CONCLUSIONS
Heat treatments were established over a narrow
temperature range in 5Ni and 9Ni steel which allowed
the development of tempered structures which con-
tained either no measurable retained austenite (<0.5
pct) or approximately 4 to 5 pct retained austenite as
determined by X-ray diffraction. It was demonstrated
that the formation of austenite during tempering effec-
tively gettered carbon from the matrix and eliminated
carbide precipitation. It was also observed that 5Ni steel
was sensitive to overtempering which resulted in the
transformation of the austenite to martensite on cooling
from the tempering temperature.
The results of tensile testing at 77 K showed that the
yield strength decreased as the tempering temperature
or time increased. Yield points were observed in the
tensile curves for those specimens containing no meas-
urable retained austenite (<0.5 pct) while yield points
were greatly diminished or eliminated for those spec-
METALLURGICAL TRANSACTIONS A
15 ~ 1 HR. 1008K, wq, 1 HR, 873K, wq
1 HR. 1008K, wq, 1 HR. 923K, wq
z lo / !
I i
"1
!
I,,-.~ L,.,
I I I -'-I
0 1 .O 2.0 3.0 4.0
C R O S S HEAD DEFLECTION, m m
Fig. l~-Load-deflection behavior observed during slow bend testing
at 77 K of precracked Charpy specimens of 5 pct Ni steel. The two
step tempering treatments utilized are indicated on the curves. Note
the early onset of unstable cracking in the specimen final tempered at
923 K.
imens which contained retained austenite. Significant
variations were observed in the ultimate tensile
strengths, but a consistent pattern of increased ultimate
tensile strength in specimens containing retained aus-
tenite was observed. Since the variation in ultimate
tensile strain was minimal, greater work hardening was
present in those samples containing retained austenite.
This was attributed to the transformation of austenite to
martensite during tensile deformation.
The fracture toughness parameter, Kzc, at 77 K was
calculated from slow bend precracked Charpy data
using both the equivalent energy and COD concepts. In
the 9Ni alloy, optimum properties were observed in the
specimens containing retained austenite. Both a slight
increase in Kzc and significant increase in energy
absorbed were correlated with the formation of retained
austenite during tempering. These effects were attrib-
uted to the decreased yield strength and increased work
hardening exhibited by the specimens containing
retained austenite. In the 5Ni alloy, equivalent fracture
properties to those observed for the 9Ni alloy were
developed in specimens which were grain refined and
tempered to contain <0.5 pct retained austenite. Infe-
rior properties were observed in grain refined specimens
containing 3.8 pct retained austenite due to the pre-
mature onset of unstable cracking.
The results of Charpy impact tests at 77 K correlated
with the fracture toughness testing. Maximum impact
properties were observed in 9Ni specimens containing
retained austenite, and in 5Ni specimens grain refined
and tempered which contained <0.5 pct retained
austenite. A decrease in impact properties was observed
in grain refined 5Ni specimens containing 3.8 pct
retained austenite.
VOLUME 11A, AUGUST 1980--1349
 The net result of these observations leads us to
conclude that the formation of thermally stable retained
austenite in these Ni steels has an inherently favorable
impact on fracture toughness by acting as a sink for
carbon during tempering. However, the mechanical
stability of the retained austenite is a key factor in
achieving favorable results. Too low of an austenite
stability can result in unstable cracking which leads to
significantly reduced fracture properties.
ACKNOWLEDGMENT
This work was funded by the Central Scientific
Laboratory of the Union Carbide Corporation. The
work was performed at Union Carbide's Central Sci-
entific Laboratory, Tarrytown, NY.
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1350--VOLUME 11A, AUGUST 1980
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METALLURGICAL TRANSACTIONS A