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SAE TECHNICAL
PAPER SERIES

Effects of Subzero Treatments on the

Bending Fatigue Performance of
Carburized SAE-4320 and SAE-9310 Steels

Seung-Cheal Jung
Hyundai Motor Co.

D. J. Medlin and G. Krauss

Colorado School of Mines

Reprinted from: New Steel Products and Processing for Automotive Applications
(SP-1172)

The Engineering Society

=for Advancing Mobility international Congress & Exposition
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February 26-29,1996

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Effects of Subzero Treatments on the

Bending Fatigue Performance of
Carburized SAE-4320 and SAE-9310 Steels
Seung-Cheal Jung
Hyundai Motor Co.

D. J. Medlin and G. Krauss

Colorado School of Mines

Copyright 1996 Society of Automotive Engineers, Inc.

ABSTRACT austenite, phosphorus segregation and

carbide formation on austenite grain
The effects of subzero treatments on boundaries, and coarse carbide
the bending fatigue performance of structures, may influence the bending
carburized gear steels were investigated fatigue performance of gas-carburized
by cantilever bending fatigue testing. steel components (1, 2). Retained
Specimens were machined from SAE-4320 and austenite is invariably present in the
SAE-9310 bar stock steel, gas-carburized, high-carbon-containing case
quenched, tempered at 175OC, subzero microstructures of carburized steels, and
cooled t o -73OC and -196OC, and tempered high volume fractions may adversely
at 17S°C. Bending fatigue specimens were affect the wear resistance, high-cycle
characterized by light metallography to bending fatigue resistance, and
determine microstructure and prior dimensional stability (3,4). The latter
austenite grain size, x-ray diffraction effect is due to the strain-induced
for residual stress and retained austenite transformation of retained austenite to
contents, microhardness testing, and martensite (5) during cyclic mechanical
scanning electron microscopy t o evaluate loading in service, and the attendant
fatigue crack initiation, propagation and volume expansion when the austenite is
overload. Refrigeration treatments caused replaced by the martensite. On the other
additional transformation of retained hand, retained austenite may be
austenite and increased surface hardness beneficial for low-cycle bending fatigue
and compressive residual stresses. Bending resistance, rolling contact fatigue
fatigue endurance limits for the SAE-4320 resistance, or fracture resistance due to
specimens were determined t o be 1310 MPa the increase in residual compressive
for the as-carburized condition, 1170 MPa stresses formed from retained austenite
for the -73OC condition, and 1280 MPa for to martensite transformations during
the -196OC condition. Endurance limits for service.(6-8).
the SAE-9310 specimens were determined to The amount of retained austenite in
be 1170 and 1070 MPa for the as-carburized the case of a carburized steel component
and -73OC conditions, respectively. The may be reduced by reheating, by
lower endurance limits of the subzero tempering, or by subzero cooling or
treated specimens are attributed to refrigeration treatments (1,2). Subzero
retained austenite to martensite treatments effectively reduce retained
transformation and the formation of austenite contents, thereby increasing
microcracks in the carburized case layer case hardness and subsequent dimensional
due to subzero treatments. The importance stability of engineering components, and
of tensile residual stresses in the are commonly used for aerospace
austenite remaining after subzero cooling applications (9). However, several
is also discussed. investigations have shown that subzero
treatments decrease the bending fatigue
INTRODUCTION performance of carburized components (10-
12). Also, it has been shown that subzero
Many processing and microstructural cooling treatments may cause significant
factors, including case depth, residual reductions in the fracture toughness of
stresses, surface oxidation, retained high-carbon steel martensitic
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TABLE 1 - Chemical com~ositions(wt%l for SAE-4320 and SAE-9310 steels

Steel C Mn P S Si Ni Cr Mo Cu A1 N

4320 0.17 0.60 0.010 0,018 0.21 1.68 0.48 0.20 0.22 0.032 0.012
9310 0.10 0.60 0,011 0.019 0.28 3.11 1.31 0.13 0.19 0.032 0.011

TABLE 2 - Heat Treatment Processing for the bending fatigue specimens

microstructures (13). In view of these The purpose of this investigation

potential adverse effects of refrigeration is to evaluate the effect of subzero
treatments on the performance of cooling on the microstructure and bending
carburized steels, Parish and Harper fatigue of two gas-carburized alloy
recommend that they be used only with steels. SAE-4320 and SAE-9310 steels were
caution, and if subzero cooling treatments chosen for the investigation, and after
are used, that tempering should be carburizing and quenching, all specimens
performed before and after the cooling were subjected to tempering both before
treatment ( 1 ).
Several explanations have been
and after subzero cooling treatments in
order to minimize potential adverse
proposed for the decrease in mechanical effects on the case microstructures of
performance observed after subzero cooling the carburized specimens.
of carburized steels. One explanation
attributes decreased performance to EXPERIMENTAL PROCEDURE
microcrack formation which develops as
martensite plates form and impinge during SPECIMEN PREPARATION AND HEAT
subzero cooling (14). The microcracks may TREATMENT -
Table 1 shows the chemical
form within martensite plates, at the compositions of the SAE-4320 and 9310
interface of martensite plates and the steels examined in this study. Modified-
matrix retained austenite, or at austenite Brugger cantilever bending fatigue
grain boundaries. Fine austenite grain specimens were machined from forged bars
sizes, and therefore fine martensitic with the longitudinal axis of the
microstructures, reduce sensitivity to specimen oriented parallel t o the rolling
martensitic microcracking (15). Another direction of the bar, see Figure 1. The
explanation is based on the measurement of specimen geometry has a reduced
residual tensile stresses in the retained cantilever section to simulate the root
austenite of case microstructures during of a gear tooth and the edges on the
subzero cooling treatments (4,11,12). Such tensile side of the specimen are rounded
tensile stresses would locally offset the to avoid high-carbon build-up during gas
overall compressive residual stresses in a carburizing (16,17). The fatigue
carburized case and enhance crack specimens were mechanically ground with
formation during fatigue or impact loading. 320 grit paper and chemically polished in
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a HF-HZ02-HZO solution prior to

carburlz~ngin an effort to reduce
possible surface roughness effects (17).
Table 2 shows the heat treatment
processing for the specimens. After
tempering, the specimens were divided into
three groups, "A", "B" and "C" Group "A" .
specimens did not experience any
additional processing. Group "B" specimens
were subzero cooled to -73OC and tempered
at 17S°C for 60 minutes. Group "C"
specimens were subzero cooled to -196OC
and tempered.
FATIGUE TESTING - The bending
fatigue properties were evaluated with a
Baldwin displacement-controlled fatigue
machine which operated at 30 Hz. A
minimum/maximum stress ratio of R=0.1 was
utilized and fatigue evaluations were
suspended after 1 . 0 ~ 1 0cycles.
~ Figure 1. Cantilever bending fatigue
METALLOGRAPHY AND HARDNESS TESTING - specimen. All dimensions in millimeters.
Metallographic samples cut from selected
bending fatigue specimens were prepared by approximately 0.65mm. However, there is a
traditional metallographic techniques. hardness increase near the surface of
Case and core microstructures were over 40HV consistent with retained
revealed with a two percent nital etch. austenite to martensite transformation
The depth of surface intergranular due to subzero cooling. This will be
oxidation was measured on samples in the discussed later.
as-polished condition. The prior austenite Figure 3 shows the microhardness
grain size was determined in accordance profiles for the as-carburized and
with ASTM E112-88, after etching in a subzero cooled to -73OC SAE-9310 specimen
saturated picric acid and hydrochloric sets. The specimen set subzero cooled
acid solution in which sodium- to -196OC was not included in this study
tridecylbenzene was used as a wetting due processing complications. Both of
.
agent ( 18) these specimen sets exhibit similar case
Microcracks were examined with light depths of approximately 0.50mm. However,
and scanning electron microscopy (SEM). the near surface hardness of the subzero
Fatigue fracture surfaces were examined by cooled specimen set is much higher, 60
light macroscopy and SEM to characterize HV, and is also attributed to retained
fatigue initiation and propagation austenite transformation which occurred
mechanisms. Vickers hardness testing was during subzero cooling.
used with a 500 gr load for 10 seconds.
X-RAY DIFFRACTION - Retained
METALLOGRAPHIC CHARACTERIZATION
The surface alloy-oxidation which
-
austenite and residual stress profiles of occurred during gas carburizing on the
representative samples were measured with SAE-4320 and SAE-9310 specimens is shown
traditional x-ray diffraction techniques in Figures 4(a) and 4(b), respectively.
with chromium radiation (19,20). The The depth of oxidation is approximately
volume fraction of retained austenite was 5-10pm. The corresponding etched
calculated by the ratio of four microstructures in Figures 5(a) and 5(b)
diffraction peaks: martensite (211) and show the dark-etching non-martensitic
(200) and austenite (220) and (200). microstructures in the oxidized surface
Residual stress levels were also layer for the SAE-4320 and SAE-9310
determined by measuring the martensite steels, respectively. These
(211) peak shift. microstructures reflect a decrease in
hardenability caused by reduced alloying
RESULTS elements in solution, such as chromium
and silicon, because of oxide formation.
MICROHARDNESS PROFILES -
Figure 2 More non-martensitic microstructures are
shows the microhardness profiles for the evident in Figure 5(b) for the SAE-9310
three SAE-4320 specimen sets: as- specimen due to higher silicon and
carburized, carburized and subzero cooled chromium contents. Below the oxidized
to -73OC, and carburized and subzero layer the microstructure consists of
cooled to -196OC. All three specimen sets tempered plate martensite and retained
exhibit a similar case depth of austenite,
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Microhardness Profiles for SAE-4320 Specimens

L . - . . l . . . . l . . . - l . . . . I . . . . .
Po SAE-4320
As-Carburlzed
A Carb. & Subzero -73C .
Carb. & Subzero -196C -

0 0.5 1 1.5 2 2.5

Depth Below the Surface (mm)

Figure 2. Microhardness profiles for the

SAE-4320 cantilever bending fatigue
specimens.

Microhardness Profiles for SAE-9310 Specimens

4
.A
SAE-9310
As-Carburlzed
-
A Carb. & Subzero -73C .

?% 4 A
-

'e Figure 4. Unetched microstructure

Bb showing surface alloy-oxidation on (a)
48 ~ Q W W P ~ B ~ B B ~ SAE-4320 and (b) SAE-9310 specimens.
Light micrographs. -
: . . . . I . . . , I . . . . ' . . . . I . . . . %

0 0.5 1 1.5 2 2.5

Depth Below the Surface (mm) RESIDUAL STRESS AND RETAINED
AUSTENITE- The retained austenite
Figure 3. Microhardness profiles for the profiles for the SAE-4320 and SAE-9310
SAE-9310 cantilever bending fatigue specimens are shown in Figures 8(a) and
specimens. 8(b), respectively. The as-carburized
SAE-4320 specimens have a maximum
retained austenite content subsurface of
The prior austenite grain structures almost 15%. Both subzero cooling
from the case and core of the SAE-4320 treatments decrease the entire retained
specimen are shown in Figures 6(a) and austenite profile. The specimen set
6(b), respectively. The specimens have an subzero cooled to -196OC has a maximum
average case ASTM grain size number of retained austenite content of only 10%.
10.1 and a core ASTM grain size number of Figure 8(b) shows that subzero cooling
10.7. Figures 7(a) and 7(b) show the prior decreased the retained austenite content
austenite grain structure of the case and from 22% down to approximately 10% in the
core for the SAE-9310 specimens. These SAE-9310 specimen set.
specimens have an average grain size of The transformation of retained
ASTM 9.4 for the case and ASTM 9.6 for the austenite to martensite resulted in an
core. increase in the residual compressive
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Figure 5. Non-martensitic microstructures Figure 6. Prior austenite grain

on the surface of (a) SAE-4320 and (b) boundaries from the (a) case and (b) core
SAE-9310 specimens. Light micrographs with of SAE-4320 specimen. Light micrograph
2% nital etch with DDBS-Na etch (see text).

stress state in both sets of steels. profiles.

Figure 9(a) shows an increase of almost 70 BENDING FATIGUE PERFORMANCE The-
results of the cantilever bending fatigue
MPa in the residual compressive stress
state in the SAE-4320 specimens due to evaluations are shown in Figures 11 and
subzero cooling t o -73OC and a compressive 12 for the SAE-9310 and SAE-4320 specimen
increase of almost 140 MPa due to subzero sets, respectively. The SAE-4320 as-
cooling to -196OC. The SAE-9310 specimens carburized specimen set exhibited an
had an increase in the compressive stress endurance limit of 1310 MPa. The subzero
state near the surface of almost 170 MPa cooling treatments lowered the endurance
and an even larger compressive increase limits to 1170 and 1280 MPa for the -73OC
subsurface (150pm) of almost 275 MPa. The and -196OC subzero cooled specimens sets,
transformation of retained austenite due respectively.
to subzero cooling is responsible for the The SAE-9310 as-carburized specimen
increase in residual compressive stresses, set had an endurance limit of 1170 MPa,
as well as an increase in hardness while the -73OC subzero cooled set had an
previously shown in Figures 2 and 3. endurance limit of 1070 MPa. In both
Figure 10 shows the carbon profiles steels, the subzero cooling lowered the
for the SAE-4320 and SAE-9310 steels. Both endurance limits of the specimens, as
gas-carburized steels show similar carbon well as the low cycle portion of the
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Retained Austenite Profiles

SAE-4320 Specimens

-
+As-Carburized
-A- Carb. & Subzero - 7 3 C

-+ Carb. & Subzero - 1 9 6 C I

I I
0
0 200 40 0 600 800
Depth Below the Surface (microns)

Retained Austenite Profiles

SAE-9310 Specimens
30 L I I I 1
+As-Carburized
--a- Carb. & Subzero -73C

Figure 7. Prior austenite grain

boundaries from the (a) case and (b) core
of SAE-9310 specimen. Light micrograph
with DDBS-Na etch (see text).
0 200 400 600 800
fatigue curves. Depth Below the Surface (microns)
FRACTOGRAPHY - A typical fracture
surface from a specimen is shown in Figure Figure 8. Retained austenite profile for
13 via SEM imaging. The tension side of (a) SAE-4320 and (b) SAE-9310 specimens
the specimen is shown on the top of the determined by x-ray diffraction.
fractograph and two fatigue crack
initiation sites are apparent on this
fracture surface. Figures 14(a)-(e) show size for the carburized case, unstable-
the typical sequence of fatigue crack intergranular overload occurs through the
propagation or "stages" exhibited on these case and into the case/core interface, as
specimens. The fatigue cracks initiate by shown in Figure 14(b). Because the carbon
intergranular fracture in and below the level at the case/core interface is much
oxide layer. This phase is referred to as lower, the fracture toughness of the core
Stage I. Stage I1 is the stable- is much higher, therefore intergranular
transgranular-fatigue-crack growth region overload through the case is inhibited
which encompasses most of the fatigue life and subsurface stable-secondary-fatigue
of these specimens. Both Stages I and I1 crack growth resumes. This is shown in
are shown in Figure 14(a). Once the Figure 14(c) and is described as Stage
fatigue crack obtains the critical flaw IV. Figure 14(d) shows the change in
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Residual Stress Profiles Carbon Profiles

SAE-4320 Specimens
20

0 200 400 600 800

Depth Below the Surface (microns) 0 1 2 3
Depth Below the Surface (mm)
Figure 10. Carbon profiles for the SAE-
Residual Stress Profiles 4320 and SAE-9310 specimens.
SAE-9310 Specimens
20 Bending Fatigue of SAE-4320 Specimens
100 Closed symbol represents suspended test

2000
A Carb. & Subzero -73C
o Carb. & Subzero -196C

-400
-60
0 200 400 600
Depth Below the Surface (microns)
800
150 1 .................................... J1000
Figure 9 . Residual stress profiles for 1 0' lo4 lo5 10' lo7 10'
(a) SAE-4320 and (b) SAE-9310 specimens Number of Cycles
determined by x-ray diffraction. Figure 11. Bending fatigue results for
the SAE-4320 specimens.
crack propagation from stable-secondary-
fatigue to ductile overload. Final ductile Bending Fatigue of SAE-9310 Specimens
Closed symbol represents suspended test
overload is shown in Figure 14(e) and is ...... . . ....",
signified as Stage V. All stages of
fatigue crack propagation in the
"I
-0 ........................

As-Carburlzed 2000
cantilever bending fatigue specimens have
been evaluated and discussed in a previous
study (21).
Figure 15 shows microcracks that are
typical in the carburized case of the
subzero cooled specimens. Both the -73OC
and -196OC SAE-4320 specimen sets
exhibited more microcracks than the as-
carburized specimens. Figure 16 shows the
microcrack density per depth in the SAE-
4320 specimens. At approximately 100
microns all the specimens have a maximum
microcrack density. However, both sets of 10' lo4 lo5 10' 10' 10'
subzero cooled specimens have twice the Number of Cycles
microcrack density when compared to the Figure 12. Bending fatigue results for
as-carburized processed specimens. the SAE-9310 specimens.
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Figure 13. SEM fractograph of the entire

fracture surface of a SAE-4320 specimen.
Fatigue fracture initiated at the top
surface.

DISCUSSION formation in the near surface layers

found in this study, and ultimately lower
The results presented above confirm the bending fatigue performance.
that subzero cooling lowers fatigue Carburized steels with fine
performance of carburized steels. This austenite grain size exhibit superior
decrease in fatigue performance occurs bending fatigue performance as shown in
even when specimens are tempered before Figure 17. This figure shows the bending
and after subzero cooling. The subzero fatigue endurance limits of as-carburized
cooling results in a transformation of and subzero cooled SAE-4320 and SAE-9310
some retained austenite in the carburized steels from this study, along with
case and leads t o increased near surface similar gas-carburized SAE-4320 steels
hardness and residual compressive from previous studies (22,23), as a
stresses, as shown in Figures 2,3,8, and function of austenite grain size. This
9. However, metallographic evaluation figure clearly indicates the significance
shows subzero cooling develops increased of specifying heat treatments, such as
microcracking in the near surface layer. reheat treatments, that will result in
These cracks could lead to enhanced fine austenite grain structures and
fatigue crack initiation and propagation, increased bending fatigue performance.
which accounts for the reduced fatigue Heat treatment specifications and
performance. This is shown in Figures 11 some commercial heat treaters recommend
and 12. Several investigations (11-13), tempering both before and after subzero
including the recent study by Grosch and cooling in order t o diminish the
Schwarz ( 4 ) , have shown that the retained detrimental effects on bending fatigue
austenite in the case of subzero cooled performance (1,9). However, the bending
components can develop residual tensile fatigue results shown in Figures 11 and
stresses. Usually case residual stresses, 12 indicate that traditional tempering
because of the large martensite volume operations performed before and after
fraction, are measured from the tempered subzero cooling will not completely
martensite peaks. As a result, the peaks diminish the adverse effects attributed
from the retained austenite have very low to subzero cooling, and ultimately result
intensity, and are rarely measured. in decreasfng the endurance limit by
However, these tensile stresses may approximately 10%.
locally contribute t o the microcrack
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Figure 14. SEM fractographs showing

typical fracture surfaces of SAE-4320
specimen. (a) Stages I and I1
intergranular initiation and stable
transgranular growth, (b) Stage I11
intergranular overload in case, (c) Stage
IV secondary fatigue, (d) transition
between Stages IV and V, and (e) Stage V
ductile overload in core.
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Comparison With Previous Studies

ASTM Grain Size N u m b e r
8 9 10 11 12 13 14
1600 I I I I I I a

-
-
Research Investigation
X Hyde (22)
+ Cohen (23)
Carb 4320
Subzero 4320 .
Carb 9310
A Subzero 8310
I . . . . I . . .

Figure 15. SEM micrograph showing 8 10 12 14 16 18

microcracks in the case of SAE-4320 Grain Size, m m -112
specimen, 2% nital etch.
Figure 17. Bending fatigue endurance
Microcrmk Observation Range
limit verses prior austenite grain size
/ I ' r . - , ~ ~ - . , T
".
l r . , . I I I
for this study and previous studies.

31 The transformation of retained

austenite t o martensite from
subzero cooling caused significant
additional microcrack formation,
SAE 4920 which together with localized
0-0 Ar.Carburlzed tensile stresses in the austenite,
A-A Car.+ Subzero -730C may be responsible for the reduced
0-0 Car.+ Subzero -18doC bending fatigue performance.

4) Standard tempering before and after

subzero cooling did not completely
remove the detrimental effects
associated with subzero cool
processing.
0 100 200 SO0 400 500 600

Depth below Surface (micron)

ACKNOWLEDGEMENTS
Figure 16. Microcrack density versus
depth for SAE-4320 specimens. The authors thank The Timken
Company and Mr. John Dossett of Midland
Metal Treating for their assistance with
CONCLUSIONS this investigation.
1) The subzero cooled SAE-4320 and SAE-
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