Journal of Materials Processing Technology 176 (2006) 4144

Effect of low temperature tempering prior

cryogenic treatment on carburized steels
M. Preciado , P.M. Bravo, J.M. Alegre
Department of Civil Engineering, University of Burgos, Av. Cantabria s/n, 09006 Burgos, Spain
Received 13 April 2005; received in revised form 20 January 2006; accepted 20 January 2006

Abstract
The effect of deep cryogenic treatment on the hardness and wear resistance of carburized steels used in gears was studied. The performance of
the deep cryogenic treatment on quenched and tempered (first stage of tempering) steels, increased the wear resistance but the hardness was only
increased in steels tempered at 200 C. To avoid the influence of the retained austenite, and considering this presence beneficial for its application
on gears, it was stabilized prior to performing the cryogenic treatment. It is suggested the possibility of creation of nuclei sites during the 200 C
tempering, where new segregations of carbon and alloying elements could cluster during the cryogenic treatment producing an increase in the
hardness.
2006 Elsevier B.V. All rights reserved.
Keywords: Deep cryogenic; Retained austenite; Carburization

1. Introduction
Case carburized steels can present a microstructural composition, which results in high superficial hardness and an increased
mechanical, fatigue and wear strength. The combination of these
properties is recommended for applications where high stress
and cyclic loading are involved, such as gears [1]. Case carburized steels present a very complex microstructure: close to
the surface, it is composed of high carbon tempered martensite, retained austenite and carbides. The retained austenite is a
very ductile phase, and its presence in the microstructure, has
been a controversial subject in controlling both wear and fatigue
behaviour. The presence of retained austenite in the carburized
case may decrease the wear resistance or the contact fatigue in
gears but it has also been suggested that due to the strain induced
ability of retained austenite to transform into martensite during
abrasion, the fatigue life can be improved by promoting crack
closure at the crack tip and reducing then the crack growth rate
[2].
Deep cryogenic treatment in the range of 125 to 196 C
improves certain properties beyond the improvement obtained
by normal cold treatment. There are several theories concern-

Corresponding author. Tel.: +34 947 258919; fax: +34 947 259485.
E-mail address: mpreciado@ubu.es (M. Preciado).

0924-0136/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2006.01.011

ing reasons for the effects of cryogenic treatment. One theory,

involves the more nearly complete transformation of retained
austenite into martensite. This theory has been verified by Xray diffraction measurements. Another theory is based on the
strengthening of the material brought about by precipitation of
submicroscopic carbides as a result of the cryogenic treatment.
Allied with this, is the reduction in internal stresses in the martensite that happens when the submicroscopic carbide precipitation
occurs [3].
In this work, two types of carburized steels has been subjected to a deep cryogenic treatment after tempering at different
temperatures, since it has been observed [4], that such treatment
improves the mechanical properties of tool steels, and the carbon
level in the carburized region becomes either equal to or higher
than the carbon level in the tool steels.
To avoid the influence of the retained austenite in the improvement of certain properties and considering its presence beneficial for gears application [5], it was stabilized by holding the
samples at room temperature during a long time. These experiments were aimed at the study of the effect of the treatment
on hardness and wear resistance. Although it is known that a
tempering treatment after the cryogenic cycle must be given,
in order to improve the impact resistance of the materials, the
samples were studied without such a treatment to evaluate only
the effects of the tempering and the cryogenic treatment on the
steels.

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M. Preciado et al. / Journal of Materials Processing Technology 176 (2006) 4144

Table 1
Chemical composition of the investigated steel (percentage by weight)
Steel

%C

%S

%Si

%Ni

%P

%Mn

%Cr

%Mo

1
2

0.150.21
0.110.17

0.035
0.035

0.150.40
0.150.40

3.003.50

0.035
0.035

0.600.90
0.300.60

0.851.15
0.801.10

0.150.25
0.200.30

Fig. 1. Cryogenic cycle.

2. Experimental procedure
The chemical composition of the gear materials prior to carburization is
given in Table 1.
The specimens were carburized at 920 C, quenched from 820 C and tempered at three different temperatures for 2 h: 160 C to obtain a surface hardness
of 61 HRC, 170 C for 58 HRC and 200 C for 56 HRC. To stabilize the retained
austenite, the samples were held at room temperature for more than 107 s [6].
They will be referred to as QT (quenched and tempered) and QTC (quenched
tempered and cryogenically treated) following the nomenclature of Molinari et
al. [4].
The cryogenic treatment consisted of a slow cool-down (1 C/min) from
ambient temperature to liquid nitrogen temperature. When the materials reached
approximately 190 C, were held at that temperature for 22 h. Finally, the
samples were allowed to warm up to room temperature. These samples were
kept inside another chamber to prevent the steels from being subjected to liquid
nitrogen and to eliminate the risk of thermal shock. Fig. 1 shows the cryogenic
cycle.
These heat-treated specimens were sectioned before the cryogenic cycle and
afterwards they were cold-mounted, polished and lightly etched in 2% Nital. The
hardness profiles were then drawn by using microhardness value (VHN) at different points from the sub-surface to the core. The specimens were then slightly
polished and etched with Beraha etching to point up the retained austenite.
Wear tests were carried out on a CSEM pin-on-disk trybotester using as
counterface material a 6 mm diameter alumina ball. Test conditions were set up
as 10 N of load and a total sliding distance of 174 m.

Fig. 2. Microhardness of Steel 1.

The tempering treatment at temperatures between 150 and

200 C is in the temperature range which produces the first
stage of tempering. In this temperature range, fine transition
carbides precipitate within the martensite crystals. These carbides decrease the carbon content of the martensite and thus
its hardness. After the cryogenic treatment, other carbides have
precipitated as a consequence of the low temperatures used, and
some properties of the material could be changed because of
their size and distribution. In a recent study about the microstructure of cryogenic treated tool steel [7], it was observed that the
volume fraction of carbides in the cryogenically treated sample was two times that in the non-cryogenically treated one
(although the samples of this steel were tempered after the cryogenic cycle). Besides, the distribution of these carbides was more
homogeneous and it was pointed out the possibility of a localized
diffusion process, possibly due to the clustering of carbon and

3. Results and discussion

As shown in Figs. 2 and 3, only the steels treated at 200 C (56
HRC) increased the hardness after the cryogenic treatment. This
increase is equivalent to the hardness level of the steels treated at
170 C. Nevertheless, this effect is not likely to be attributed to
the transformation from retained austenite into martensite but to
the presence of carbides inside the microstructure. The hardness
of a material is in directly correlated with the yield strength,
therefore these carbides may increase the strength at low strains.
However, in the steels treated at 170 and 160 C, any remarkable
increase in hardness was experienced.

Fig. 3. Microhardness of Steel 2.

M. Preciado et al. / Journal of Materials Processing Technology 176 (2006) 4144

43

Fig. 4. Optical micrographs showing the 160 C tempered steels with and without cryogenic treatment at 150 m from the surface (1000).

alloying elements to defects generated by microscopic internal

stresses during cooling. Assuming that in the 200 C tempered
samples the carbides would be bigger and present in higher
amount, these carbides could be likely to act as nuclei for the
new segregations formed during the cryogenic cycle and capable of increasing the microhardness. The absence of this effect
in the other two tempered samples suggested two possibilities:
either there was a critical carbide size from which the precipitation was not preferential at these sites or the volume fraction of
carbides at temperatures less than 170 C was not enough.
The microstructural evaluation of the carburized case (Fig. 4.)
revealed a microstructure composed of high carbon martensite,
retained austenite and carbides. Apparently these microstructures did not present variations in the amount of retained austenite (as expected) before and after the cryogenic treatment, and
this was less than 15% for the Steel 1 and about 15% for Steel 2
although these estimations were approximate due to the fact that
the amount of retained austenite was made by metallographic
evaluation with analysis of image near the surface (150 m).
The microstructures observed in the core of the QT specimens
of both steels were similar to those found in the core of QTC
specimens. This could be due to the absence of any retained
austenite and the low carbon content of the martensite.

The wear results are summarized in Fig. 5. It could be

observed that the wear resistance was always better in the QTC
samples than in the QT ones for both steels. Nevertheless, Steel
2 presented a higher wear resistance than Steel 1 for all the heat
treatments studied.
The effect of the deep cryogenic treatment for the wear resistance must be sought in the submicroscopic microstructure of

Fig. 5. Wear rate of heat treated steels.

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M. Preciado et al. / Journal of Materials Processing Technology 176 (2006) 4144

the steels. The precipitation of fine carbides as a result of the

cryogenic treatment could be responsible for the improved wear
resistance in both steels. Alloying will increase the abrasion
resistance of a metal only if the strengthening mechanism leads
to increase strength at high strains [8], and this could give an
explanation for the better behaviour of Steel 2. The precipitation
of fine carbides is also a strengthening mechanism and, during
the high strains produced in the wear tests, this precipitation
plays an important role.
Looking at the microhardness values it could have been
thought that the QTC 200 C samples would present the same
wear behaviour that the QCT 170 C, as their hardness were
the same and also the heat treatment, but the precipitates which
increased the microhardness in the QTC 200 C were not effective for improving the wear resistance. This could suggest the
presence of some big precipitates that would be inappropriate to
increase the abrasion resistance for the high strains developed
during the wear tests. Besides, in the QCT 200 C the martensite would have less carbon content and therefore the amount of
carbon that with alloying elements could segregate during the
cryogenic treatment will be less than in the QCT 170 C.
In relation with the wear resistance, the retained austenite was
a relevant fact due to the possible transformation into straininduced martensite during abrasion. This would be important
in gear applications, where this transformation could introduce
compression stresses which improve the behaviour of the gears
against contact fatigue. Anyway this contribution should be the
same for the samples of Steel 1, as they have approximately the
same amount of retained austenite, and the same for the samples
of Steel 2, so therefore could not be used for comparison of the
wear results.
However, the influence of the tempering temperature and
cryogenic treatment on the toughness must be studied as it is
a crucial point in engineering applications. A specific investigation based on different treatments prior and following the
cryogenic treatment is ongoing.
4. Conclusions
The deep cryogenic treatment (190 C) of quenched and
tempered carburized steels improved the wear resistance, being

this tempering in the low temperature range. This improvement was probably due to the segregation of carbon atoms and
alloying elements during the cryogenic cycle and the transformation of the retained austenite into strain-induced martensite. The best treatment for wear resistance corresponded to
a tempering at 160 C following by the cryogenic treatment.
The increase in hardness was only produced when the tempering prior to the cryogenic treatment was at about 200 C.
It is suggested that the carbides produced during this tempering could act as nuclei sites for posterior segregations during
the cryogenic treatment. This would produce a bigger size of
these carbides, making them effectives for the increase of hardness but not for the improvement of the wear resistance, as
this one depends on the strengthening mechanisms at higher
strains.
Acknowledgements
The authors wish to thank L.E. Garca Cambronero for its
help with the wear tests and the Escuela Superior de Minas from
Madrid for letting the realization of those tests.
References
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