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Nagarajan Govindan
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Arunachalam Rajadurai
Krzysztof Junik
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Received 6 July 2006; received in revised form 14 June 2007; accepted 16 July 2007
Abstract
The effect of cryogenic treatment on the distribution of residual stress in the case carburized steel (En 353) was studied using X-ray diffraction
technique. Two types of cryogenic treatment: shallow cryogenic treatment (193 K) and deep cryogenic treatment (77 K) were adopted, as a
supplement to conventional heat treatment. The amount of retained austenite in conventionally heat-treated, shallow cryogenically treated and
deep cryogenically treated samples was found to be 28%, 22% and 14%, respectively. The conventionally heat-treated, shallow cryogenically
treated and deep cryogenically treated samples in untempered condition had a surface residual stress of 125 MPa, 115 MPa and 235 MPa,
respectively. After tempering the conventionally heat-treated, shallow cryogenically treated and deep cryogenically treated samples had a surface
residual stress of 150 MPa, 80 MPa and 80 MPa, respectively. A comparative study of the three treatments revealed that there was an increase
in the compressive residual stress in steel that was subjected to cryogenic treatment prior to tempering. The experimental investigation revealed
that deep cryogenically treated steel when subjected to tempering has undergone a reduction in compressive residual stress. Such stress relieving
behaviour was mainly due to the increased precipitation of fine carbides in specimens subjected to DCT with tempering.
2007 Elsevier B.V. All rights reserved.
Keywords: Case carburized steel; Cryogenic treatment; Grinding; Residual stress; Retained austenite
1. Introduction
Scientists and engineers have been successful in improving
the impact and fatigue properties of metals by intentionally
introducing residual stresses into the surface of these materials. Residual stress exists in an elastic solid body in the absence
of, or in addition to, the stresses caused by virtue of load or
temperature or both. Such stresses can arise from deformation
during cold working, in welding from weld metal shrinkage,
and in changes in volume due to thermal expansion. In recent
years, there has been a considerable interest in the properties and
development of compressive residual stress. Knowledge of the
nature of residual stresses is of paramount importance since they
can lead to creep failure, fatigue and stress corrosion cracking in
sensitive materials. Mack Alder and Olsson [1] have observed
0921-5093/$ see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2007.07.035
that after case hardening, the gear tooth would experience compressive residual stresses, which are beneficial in maintaining
an appreciable endurance limit. But these beneficial stresses are
counter acted by detrimental tensile residual stresses in the core.
The explanation of this phenomenon is based on the uneven volumetric expansion in the core and at the surface layer during
phase transformation. Hence, it is an important consideration in
the heat treatment of steel.
Various methods are used to improve the behaviour of steel.
Carburizing is one of the prevalent methods used for this purpose. It is a thermo chemical diffusion process used to produce a
hard wear resistant case. Due to carburization, the percentage of
carbon in the case will increase to the carbon potential applied.
Carburizing is beneficial to the component but the increase in
carbon content leads to retention of austenite after hardening,
which is not desirable. In some steels, those with higher carbon
content and alloy steels, the martensite finish temperature (Mf ) is
below 273 K, which means that at the end of the heat treatment,
there is as much as 515% of austenite remaining [2].
230
with the metal. Molinari et al. mentioned that carbide precipitation occurs with a higher activation energy thus leading to
a higher nucleation rate and in turn to finer dimensions and a
more homogeneous distribution. A new phenomenon referred as
tempered martensite detwining was observed. Deep cryogenic
treatment can strongly reduce the wear rate of the hot work
tool steel. This result was interpreted on the basis of increased
toughness, because in the presence of delamination the ability
of materials to oppose crack propagation can really increase
the mechanical stability on the wear surface and the load bearing capacity. Therefore, even if the deep cryogenic treatment
does not influence the hardness, it increases both toughness
and wear resistance [5]. Barron conducted preliminary tests
to determine the effect of cryogenic treatment on lathe tools,
end mills, zone punches and concluded that an increase in tool
life from 50% to more than 200% was observed for the tools
which had been soaked in liquid nitrogen for 12 h [6]. Fanju
Meng et al. have studied the effect of cryogenic treatment on
the wear behaviour of Fe12CrMoV1.4C tool steel. The
results have shown a dramatic increase in wear resistance especially at high sliding speeds [7]. Microstructural analysis of the
sample after cryogenic treatment has shown fine carbide precipitates of size in the range of 10 nm, which are characterized
as -carbide. This formation of -carbides helps to improve
the wear resistance. Mohan Lal et al. [8] studied the effect of
cryogenic treatment on T1 type-high speed material and found
that soaking at 203 K can attain the maximum hardness of 67
HRC.
The effect of cryogenic treatment on the residual stress
behaviour of En 353 prior to tempering and after tempering is
not yet reported. Hence the present study deals with the measurement of residual stress distribution, which in turn helps to
know whether cryogenic treatment helps in improving the life
of the component.
3. Experimental
3.1. Sample preparation
Commercially available 30 mm diameter bar stock of En 353
raw material was procured. In order to confirm the composition of the material procured, elemental analysis was carried
out using optical emission spectroscope (OES), the results of
which are shown in Table 1. The raw sample conforms to the
chemical requirements of En 353 specifications, as far as the
constituents are concerned. It was also found that weight percentage of carbon has increased from 0.16 to 0.75 in the case
Table 1
Chemical composition of the untreated En 353 steel (weight %)
Sample description
Carbon
Silicon
Nominal composition
0.120.18
0.10.35
0.61.0
Raw material
0.16
0.21
0.68
0.75
0.20
0.67
0.011
0.013
0.013
0.035
0.022
Chromium
Nickel
Molybdenum
0.00250.05
0.751.25
1.01.5
0.080.15
0.028
0.76
1.19
0.10
0.021
0.022
0.011
0.002
0.76
1.19
0.09
0.007
0.006
0.020
231
(1)
232
Table 2
Experimental inputs for residual stress analysis
Miller indices hkl
Diffraction angle ( )
Angular resolution ( )
Poissons ratio
Exposure time (s)
Penetration depth (m)
Youngs Modulus (GPa)
211
156.4
0.029
0.3
4
4
200
CHTUT
CHTT
SCTUT
SCTT
DCTUT
DCTT
28.1
28.5
22.0
22.8
14.9
14.3
3.5
6.1
7.6
5.9
5.8
4.1
Mf = Ms 215
(2)
(3)
233
234
as cracks during the subsequent grinding operation. The intensity of cracks visible is different for all the samples and can
be related to the amount of untempered martensite available,
which is highly brittle in nature. The presence of grinding cracks
in SCTUT and DCTUT is more when compared to CHTUT.
This could be attributed to the conversion of retained austenite to martensite at low temperatures. The cracks visible in the
tempered specimen can be related to the fine carbide precipitation. As cryogenic treatment facilitates fine carbide precipitation
during tempering, no visible cracks are observed in SCTT and
DCTT specimen. This clearly indicates that the toughness of
the matrix holding the carbides has improved. Low temperature
conditioning of martensite accelerated the precipitation of fine
235
to the specimen subjected to DCT. The decrease in the temperature increases the lattice defects and thermodynamic instability
of the martensite, which drives the carbon and alloying elements to nearby defects. These clusters act as nuclei for the
formation of fine carbides on subsequent tempering. The intensity of carbide precipitation depends on the extent to which the
specimens are cooled below room temperature. The large relaxation of residual stress in DCTT specimens indirectly reflects
about the amount of carbide precipitation. Based on relaxation
phenomenon it is concluded that DCTT exhibit the maximum
carbide precipitation than SCTT and CHTT specimens. This
has reflected in an earlier study on the improved wear resistance
obtained for En 353 after deep cryogenic treatment with tempering [14]. The study clearly shows that En 353 when subjected
to deep cryogenic process has attained the maximum compressive stress (235 MPa) before tempering. This aids the carbide
precipitation during the subsequent tempering process resulting
in large relaxation (80 MPa).
Acknowledgements
Fig. 7. Optical photograph showing the influence of grinding on DCTUT specimen.
The authors wish to thank the support of Ministry of Science and Computerization, Poland, towards residual stress
measurements. The authors also gratefully acknowledge M/s.
Chennai Metco Private Limited, for extending their metallurgical facilities for the successful completion of the work.
The authors gratefully acknowledge the financial support from
Department of Science and Technology, India, under FIST program (SR/FST/ETI-053/2002) for setting up a state of the art
cryogenic treatment facility, which enabled for the successful
completion of the project.
References
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5. Conclusion
The study confirms that cryogenic treatment (i.e. shallow
cryogenic treatment and deep cryogenic treatment) should be
followed by tempering. Untempered specimens of shallow cryogenic treatment and deep cryogenic treatment have surface
cracks, which is not beneficial to the life of the component.
The retention of residual stress in samples subjected to conventional heat treatment and shallow cryogenic treatment, followed
by tempering can lead to better fatigue properties, as compared
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