Cryogenics 45 (2006) 747–754

www.elsevier.com/locate/cryogenics

Enhancing the wear resistance of case carburized steel (En 353) by

cryogenic treatment
A. Bensely *, A. Prabhakaran, D. Mohan Lal, G. Nagarajan
Department of Mechanical Engineering, Anna University, Sardar Patel Road, Chennai 600 025, Tamilnadu, India

Received 1 September 2004; received in revised form 20 September 2005; accepted 12 October 2005

Abstract

All mechanical components that undergo sliding or rolling contact are subject to some degree of wear. So wear is an important tri-
bological phenomenon while studying the failure of components. The observed frequent failure of crown and pinion due to wear and
fatigue lead to this study on effect of cryogenic treatment on the wear resistance of case carburized steel (En 353). This paper deals with
the pin on disk wear test without lubrication as per ASTM standard, designation: G 99-95A. The test was carried out for three different
load conditions and seven sliding speeds for the samples, which has undergone three different treatment conditions namely conventional
heat treatment (CHT), shallow cryogenic treatment (SCT) and deep cryogenic treatment (DCT). It has been found that the wear resis-
tance has been considerably increased due to shallow cryogenic treatment and deep cryogenic treatment includes much more improve-
ment in wear resistance when compared to conventional heat treatment. Also it is concluded that for better wear resistance, it is advisable
to go for deep cryogenic treatment. The results are consistent with the previous studies reported in the literature on cryogenic treatments
for other materials.

2005 Elsevier Ltd. All rights reserved.

Keywords: Case carburized steel; Cold treatment; Cryogenic treatment; Material processing; Wear

1. Introduction industries in USA, China and other developed countries

have adopted the process in their production line itself to
Cryogenic treatment has been used to improve wear improve wear resistance and dimensional stability of their
resistance of materials because it enhances the transforma- components, which have an edge over the competitors.
tion of austenite (soft phase of iron) to martensite (a hard Since the mechanism is yet to be understood, some of the
phase of iron). It is a one-time permanent treatment pro- beneficiaries do not attribute the benefits achieved by cryo-
cess and it affects the entire cross-section of the material genic treatment even though it is added to the regular heat
usually done at the end of conventional heat treatment pro- treatment. So in general cryogenic treatment is still in the
cess but before tempering. Also it is not a substitute process dormant level. Further there are different levels of treat-
but rather a supplement to conventional heat treatment ment temperatures. In order to avoid confusion, cryogenic
process. In the production sector, cryogenic treatment is treatment has been classified into shallow cryogenic treat-
not yet added to the regular heat treatment cycle for the ment (SCT) and deep cryogenic treatment (DCT) depend-
components they manufacture. This is due to the lack of ing upon the temperatures in which the material is treated.
knowledge of the treatment, unexplained mechanism, ben- The common practice for shallow cryogenic treatment is to
efits with respect to materials and research articles. How- keep the specimens in a mechanical freezer at 193 K for 5 h
ever a number of aerospace, automotive and electronic and then exposed to room temperature. But in deep cryo-
genic treatment the materials are slowly brought down
*
Corresponding author. Tel.: +91 44 2220 3262; fax: +91 44 2220 3269. from room temperature to 77 K at 1.26 K/min, held at
E-mail address: [email protected] (A. Bensely). the same temperature for 24 h and subsequently brought

0011-2275/$ - see front matter
2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.cryogenics.2005.10.004
748 A. Bensely et al. / Cryogenics 45 (2005) 747–754

Nomenclature

ASTM American standard for testing and materials SAE the society of automotive engineers
CHT conventional heat treatment SCT shallow cryogenic treatment
DCT deep cryogenic treatment V linear velocity in mm/s
F load in N WL wear rate of pin in mm3/s
Hv Vickers hardness in N/mm2 WR wear resistance
k non-dimensional wear coefficient
L sliding distance in mm

back to room at 0.63 K/min. In order to achieve deep cold tionally heat-treated samples and yielded an extra life of
temperatures, materials cannot be directly kept in freezer at 3%, 10%, and 10.6% for M2, T1 and D3 steels, respectively
77 K similar to that of shallow cryogenic treatment because [4].
the temperature difference is very high and fast cooling will Meng and Tagashira studied the wear resistance and
lead to quench cracks. Hence this controlled process is microstructure of Fe–12Cr–Mo–V-1.4C tool steel both
achieved using computerised controls in a well-insulated with and without cryogenic treatment. The study reveals
treatment chamber with liquid nitrogen (LN2) as working that cryogenically treated samples show improvement from
fluid. The present work is a comparative study on the wear 110% to 600% through sliding wear test. The convention-
resistance improvement in samples through CHT, SCT, ally heat-treated and cryogenically treated specimens
and DCT using a pin-on-disk wear tester without lubrica- showed the largest and smallest wear volume at all sliding
tion and a microstructural analysis to know the effects of distance, respectively. From the microstructure of the steel
cryogenic treatment on En 353. it is reported that the improvement in wear resistance after
cryogenic treatment can be attributed to g-carbide precipi-
2. Literature survey tates [5].
However there are reports from metallurgist who are
Molinari studied the effect of DCT on mechanical prop- skeptic about cryogenic treatment [6,7]. The present work
erties of tool steels through field test and lab test on AISI deals with the study of effect of cryogenic treatment on
M2 and AISI H13, respectively. Cold treatment is done wear resistance of case carburized steel (En 353).
at 213 K to 193 K to improve surface hardness and thermal
stability. DCT is done at 148 K to 77 K, which improves 3. Statement of purpose
properties beyond the improvement obtained by normal
cold treatment. It is carried out using liquid nitrogen with The material selected for wear study is case carburized
a cooling rate of 20–30 K/h with a soaking time of 35 h. steel (En 353). This material has significant application in
Total duration of the treatment is 100 h and it reduces tool automotive industry. Typical applications of this material
breakage and wear, which resulted in 50% cost reduction are crown wheel, crown pinion, bevel pinion, bevel wheel,
[1]. timing gears, king pin, pinion shaft, differential turnion,
Collins and Dormer studied the effect of DCT on D2 etc. The gears especially crown wheel and pinion are one
cold work tool steel. Deep cryogenically treated steels give of the most stress prone parts of a vehicle, which are made
lowest wear rate compared to conventionally heat treated of En 353 steel. They are made as an assembly pair and if
steels. It is mentioned that in addition to the well-known one fails both are to be replaced together, which is quite
effect of transforming retained austenite to martensite, with expensive too. Observation of frequent failure of crown
the consequent increase in hardness. DCT has an influence wheel and pinion due to wear lead to this investigation.
on the characteristics of freshly formed martensite that on Wear for gears is defined as loss of material from contact-
tempering results in the precipitation and finer distribution ing surfaces of teeth. In an analysis of more than 1500 stud-
of carbides in the tempered microstructure, which conse- ies, wear has been identified as one of the most common
quently increases both toughness and wear resistance [2]. failure modes apart from tooth bending fatigue and tooth
Paulin mentioned that cryogenic treatment is an exten- bending impact [8]. The statistics on causes of gear failure
sion of conventional heat treatment, which converts reveals that about 13.2% of the gears fail due to wear and
retained austenite to martensite. Due to this the durability 16.2% due to faulty heat treatment. Wear processes greatly
of the component is increased [3]. reduce precision and the service duration of gears. Some of
Mohan Lal et al., made a comparative study on wear the factors influencing wear are toughness, environment,
resistance improvement of cryogenically treated samples type of loading, relative speeds of mating parts, lubricant,
with standard heat-treated samples through flank wear test temperature, surface finish, compatibility of mating parts
and sliding wear test. Cryogenic treatment imparts better and presence of foreign particles. Wear rate is generally
wear resistance throughout the section than the conven- known to decrease as the hardness of the materials
 A. Bensely et al. / Cryogenics 45 (2005) 747–754 749

increases, provided other factors remain constant. The on experimental investigations on En 353 to improve the
required wear resistance could be attained either by suit- wear resistance by adding cryogenic treatment to conven-
ably alloying or through manipulating the heat treatment tional heat treatment and also to study the microstructural
parameters. The present work deals with adding cryogenic changes.
treatment to conventional carburizing process to pro-
duce durable components. Carburization is a process, 4. Research methodology
which gives high wear resistance surface. However during
carburization the components are exposed to a rich carbon The experimental procedure adopted in the present
environment that causes retention of austenite after con- work is shown in Fig. 1. According to the flow chart
ventional hardening and tempering. The retained austenite the tests were carried out separately for three different
thus spontaneously transforms as a result of thermal and treatments.
mechanical stresses encountered during service. This results
in a variety of problems from dimensional instability to the 5. Experimental procedure
formation of grinding cracks to premature failure of com-
ponents. In order to alleviate this problem, it is advisable to 5.1. Sampling
add cryogenic treatment to the conventional heat treat-
ment, which imparts high dimensional stability, and wear After procuring the raw material, chemical analysis was
resistance. Case carburized steel when cryogenically treated done for the confirmation of the material composition.
is expected to show improvement in wear resistance. This This analysis was carried out in an optical emission spec-
can be due to the microstructural changes brought in by troscope (OES). In this spectroscope only conductive sam-
cryogenic treatment. Hence the present work is focused ples could be used. The spark analyser software is used in

Procurement of raw material

Chemical analysis to check

composition

Carburized at 1183 K for 5 hours

Air-cooled

Hardening at 1093 K for 30

minutes
Shallow cryogenic
treatment at 193 K
for 5 hours Quenching in oil at 313 K Deep cryogenic treatment

Tempering at 423 K for 1.5 hours

Dry sliding wear test Microstructural analysis

Analyzing benefits

Comparison and evolving

conclusion

Fig. 1. Flow chart for experimental procedure.

750 A. Bensely et al. / Cryogenics 45 (2005) 747–754

Table 1
Result of chemical analysis of En 353 raw material in weight %
Carbon (%) Silicon (%) Manganese (%) Phosphorus (%) Sulphur (%) Chromium (%) Nickel (%) Molybdenum (%)
0.17 0.19 0.92 0.018 0.031 1.09 1.05 0.11

estimating the elements in the sample. A sample of 20 mm specimen. The pin is positioned perpendicular and forced
diameter, 10 mm long was polished using 60-grit alumina against the revolving disk specimen with a required load.
paper. Spark is introduced on the specimenÕs polished sur- So the wear track on the disk is a circle, involving multiple
face. The surface of the sample is first ground flat and wear passes on the same track. The variable speed motor in
placed against the spark stand where it is flooded with the machine causes the disk specimen to revolve about the
argon and a rapid series of high current sparks are pro- disk center and the plane of the disk is held horizontally.
duced. A large quantity of the sample surface is evaporated Initially wear test was performed with lubrication (SAE
and emits light (photons). The signals are then recorded by 90) for 3 h but the wear loss was too small and could not
an optical spectrometer and finally OES provides a quanti- be quantified even with a precision electronic weighing bal-
tative elemental analysis of the metal sample. The result ance. Hence dry test was preferred for the study. The test
obtained by the chemical analysis for the raw material is was conducted for the samples of three different treatments
listed in Table 1. The tested sample conforms to the chem- namely CHT, SCT and DCT. The speed and load ranges
ical requirements of En 353 specifications, as far as the rad- were determined taking into account the capacity of the
icals are concerned. After confirming the material, the wear testing machine and the minimum amount of wear
material procured is machined according to machine loss which could be measured using the weighing balance.
requirement and subjected to appropriate treatments as The maximum capacity of the weighing balance used for
required for the tests. measuring the wear loss is 220 g with an accuracy of
In conventional heat treatment, the machined test sam- 0.001 g. Since the disk weighs 1450 g, the amount of wear
ples has to undergo carburization in liquid carburizing fur- could not be measured to an accuracy of 0.001 g. Hence
nace at 1183 K for 5 h followed by hardening at 1093 K for after each test only the mass loss of pin was considered
30 min, then oil quenching at 313 K and tempering at as the wear. During the test the temperature of the pin
423 K for 90 min. For shallow cryogenic treatment, the and disk interface was very high, so an air blower was used.
samples were heat treated as for CHT, but without temper- This reduces the temperature effects in the wear test per-
ing. Then the samples were directly kept in a mechanical formed. In order to ensure that the wear test is not
freezer at 193 K for 5 h and then exposed to room temper- performed continuously on the same track, which leads
ature and it is followed by tempering at 423 K for 90 min. to the removal of carburized layer, both the sides of the
The deep cryogenic treated samples were heat treated as for carburized disks were utilized for testing. Based on the pre-
CHT, but without tempering, in which the materials are liminary investigations on the machine, wear test para-
slowly brought down from room temperature to 77 K at meters were arrived, which are wear track diameter
1.26 K/min, held at the same temperature for 24 h and sub- 33–50 mm, sliding speed range 1.944–4.444 m/s, disk rota-
sequently brought back to room temperature at 0.63 K/ tion speed 550–850 rpm, normal load 60–80 N.
min. Then the samples were subjected to tempering at Hence tests were carried out for three different loads (60,
423 K for 90 min. Thus three sets of samples (i) CHT, (ii) 70, and 80 N), seven sliding velocity (1.94, 2.36, 2.78, 3.19,
SCT and (iii) DCT were taken for wear study. 3.61, 4.03, and 4.44 m/s) and for three different treatment
conditions (CHT, SCT and DCT). Wear results are
5.2. Dry sliding wear test obtained by conducting test for a selected sliding velocity
and load. Each specimen was tested for duration of 720 s
The amount of wear in any component will, in general, before arriving at the weight loss. The wear rate of each
depend upon a number of factors such as applied load, pin was calculated from the weight loss during this test
testing machine characteristics, sliding speed, sliding dis- duration. The amount of wear is determined by weighing
tance, environment and material properties. The measure- the specimen before and after the tests using a precision
ment and evaluation of wear are difficult as it depends on electronic weighing balance with an accuracy of 0.001 g.
several factors. However ASTM 99-95a describes a labora- Since the mass loss is measured, it is converted to volume
tory procedure for determining the wear of materials dur- loss using the density of the specimen. The results obtained
ing sliding [9]. In this test, materials are tested in pairs are reported as wear rate of pin (mm3/m) for the three dif-
under nominally non-abrasive conditions. Two specimens ferent treatments. A comparison has been made to identify
are required for the test a pin with a flat tip and a flat cir- the effects of each treatment on wear improvement. The
cular disk both are made of En 353 in the present work. test was repeated for a minimum of 3 times for each condi-
The size of the pin is 10 mm in diameter and 30 mm long tion. If the results were found deviating due to human
whereas the disk is 160 mm in diameter and thickness of error, machine error, improper fixing, etc. then it is
10 mm. The case depth of 1 mm is given for both the test repeated again till at least three consistent readings were
 A. Bensely et al. / Cryogenics 45 (2005) 747–754 751

Table 2 0.003
Vickers hardness of En 353 Load = 60 N
Type of treatment Hardness value (N/mm2) 0.0025
CHT 7318

Wear rate (mm3/m)

SCT 7573 0.002
DCT 7573
0.0015

obtained for every condition. This ensures better results. 0.001

The number of samples considered was sufficient to give
CHT
statistically significant results. The hardness test was car- 0.0005 SCT
ried out for the very same wear tested samples and the DCT

results are given in Table 2. 0

1.5 2 2.5 3 3.5 4 4.5 5
Sliding velocity (m/s)
5.3. Characterization by optical microscope
Fig. 2. Wear rate at 60 N load for three different treatment.
The changes in microstructure of the materials due to
cryogenic treatment are the main reason for the improved
mechanical properties of the steel. Hence microstructural 0.004
Load = 70 N
examination was carried out to identify the possible mech- 0.0035
anism brought in by cryogenic treatment on improving the
Wear rate (mm3/m)
0.003
wear properties. First the samples needed for the study
0.0025
were polished using emery paper of grit 80, 120, 200, 600
and 800. It is followed by polishing using diamond paste 0.002
on a rotating linen disk. Finally the samples are mirror fin- 0.0015
ished by polishing on velvet cloth using white kerosene as
0.001
coolant. These samples were etched with 2% nital and dried CHT
SCT
in air. Microstructural examination was carried out using 0.0005
DCT
optical microscope. 0
1.5 2 2.5 3 3.5 4 4.5 5
Sliding velocity (m/s)
6. Results and discussions
Fig. 3. Wear rate at 70 N load for three different treatment.
6.1. Wear resistance enhancement

The results obtained are represented as wear rate of pin 0.0045

Load = 80 N
for CHT, SCT and DCT in Figs. 2–4, respectively, for var-
0.004
ious loadings of 60, 70 and 80 N. The wear of any compo-
0.0035
nent is a complex function of load and sliding speed.
Wear rate (mm3/m)

Hence, these two variables were considered for the study 0.003
and the wear resistance [10] was calculated as a non-dimen- 0.0025
sional parameter incorporating the load, sliding distance,
0.002
volume loss and Vickers hardness.
0.0015
FV
WR ¼ ð1Þ 0.001 CHT
W LH v SCT
0.0005 DCT
where WR is the wear resistance, F is the load in N, V is the
0
linear velocity in mm/s, WL is the wear rate of pin in mm3/s 1.5 2 2.5 3 3.5 4 4.5 5
and Hv is the Vickers hardness in N/mm2. This wear resis- Sliding velocity (m/s)
tance is the reciprocal of wear coefficient (k). The improve- Fig. 4. Wear rate at 80 N load for three different treatment.
ment in wear resistance of cryogenically treated sample
over conventionally treated sample was evaluated and gi-
ven in Table 3. ments. It has been observed that the overall wear resistance
has been improved by 85% due to shallow cryogenic treat-
SCT
CHT
Improvement of wear resistance ¼ ð2Þ ment and 372% due to deep cryogenic treatment with
CHT respect to conventional heat treatment and while compar-
From Figs. 2–4, it is evident that the wear resistance has ing DCT with SCT the improvement was 152%. Previous
been improved due to shallow and deep cryogenic treat- studies on 52100, D-2, A-2, M-2 and O-1 alloys [10] show
752 A. Bensely et al. / Cryogenics 45 (2005) 747–754

Table 3
Improved wear resistance
Load (N) Sliding velocity (m/s) Wear resistance Improvement w.r. Improvement w.r. to SCT (%)
to CHT (%)
CHT SCT DCT SCT DCT DCT
60 2.778 6424 12,625 41,525 97 546 229
3.194 5559 9303 36,453 67 556 292
3.611 4562 7295 24,316 60 433 233
4.027 3549 5929 12,486 67 252 111
4.440 3240 4635 8375 43 158 81

70 2.778 4513 10,093 43,645 124 867 332

3.194 3892 7395 21,992 90 465 197
3.611 3264 6215 14,995 90 359 141
4.027 2706 5460 8830 102 226 62
4.440 2651 4218 7931 59 199 88

80 2.778 4023 8711 22,446 117 458 158

3.194 2988 6750 15,918 126 433 136
3.611 2838 5584 10,637 97 275 90
4.027 2679 4963 7975 85 198 61
4.440 2772 4144 6957 49 151 68

Average wear resistance improvement 85 372 152

that the wear improvement of samples treated at 83 K The effect of sliding velocity and load on wear is shown
(close to DCT) was approximately 2.6 times higher than in Fig. 5. On comparing Fig. 5(a)–(c), it is clear that wear
the wear resistance of sample treated at 188 K (close to has been found to increase almost proportionally with the
SCT). Also it was found that the improvement of wear applied load and sliding velocity for all the treatments.
resistance for the above alloys when treated at 188 K However for sliding velocity below 2.364 m/s, wear is
ranges by factors from 1.2 to 2.0 whereas the same alloys almost negligible for all the three loads irrespective of the
when treated at 83 K improves the wear resistance by fac- treatment the material has undergone. Whereas while
tors ranging from 2.0 to 6.6. Thus the present result is con- studying the wear behavior from 2.364 m/s up to
sistent with the published literature. 4.444 m/s, it is found that CHT experienced the maximum

Fig. 5. Influence of load and sliding velocity over dry sliding wear. (a) Conventional heat treatment, (b) shallow cryogenic treatment, (c) deep cryogenic
treatment.
 A. Bensely et al. / Cryogenics 45 (2005) 747–754 753

wear when compared to SCT and DCT. The test results

reveal that DCT experiences high wear resistance at all cir-
cumstances. Also while assessing the wear behavior at the
most severe condition of the test (i.e. maximum load,
80 N and maximum sliding velocity 4.444 m/s), it is
revealed that En 353 experienced a wear volume loss of
12.618 mm3, 8.157 mm3 and 4.859 mm3 for CHT, SCT
and DCT, respectively. This study confirms that DCT
can very well be employed for improving the wear resis-
tance. In general the decrease in wear resistance of the
material for all the three treatments at higher velocities
can be attributed to the increase in the temperature of
pin and disk due to friction.

6.2. Microstructure

In order to identify the mechanism for the wear resis-

tance improvement microstructural evaluation was made
using optical microscope. The microstructure of CHT,
SCT and DCT samples are shown in Figs. 6–8. The micro- Fig. 7. Microstructure of case in SCT sample at 100·.
structure of CHT sample reveals that enormous amount of
austenite is retained in the case of the material, which is evi-
dent from the white patches on the microstructure shown
in Fig. 6. The presence of retained austenite is undesirable
for a component under service. Moreover the hardness of
the CHT sample is less when compared to SCT and
DCT, which can be attributed to the poor wear resistance.
Fig. 7 reveals that all the austenite retained in CHT is con-
verted into martensite thereby increasing the hardness,
which resulted in improvement in wear resistance over
CHT. However while comparing the microstructure of
DCT with SCT, precipitation of carbides or distribution
of carbides is not visible in SCT samples. In addition to
the well-known effect of converting retained austenite to
martensite, DCT induced precipitation and finer distribu-
tion for carbides, which are solely responsible for the
improved wear resistance and hardness.

Fig. 8. Microstructure of case in DCT sample at 100·.

7. Conclusions

Deep cryogenic and shallow cryogenic treatment

imparts more wear resistance when compared to the con-
ventional treatment. Wear resistance has been improved
by 85% for SCT over CHT and 372% for DCT over
CHT. And also the wear resistance improvement of
DCT is 152% over SCT. Wear is found to increase line-
arly with load at constant sliding speeds and with sliding
Fig. 6. Microstructure of case in CHT sample at 200·. speed at constant loads. At low sliding speeds (i.e. 1.944
754 A. Bensely et al. / Cryogenics 45 (2005) 747–754

and 2.361 m/s), wear loss is very minimal (in the range of References
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120 F help
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