Classic contributions: cryogenic treatment
Effects of cryogenic treatments on mechanical
properties and wear behaviour of high-speed
steel M2*
R. Mahmudi, H. M. Ghasemi and H. R. Faradji
In this contribution, originally published in 2000, the levels of hardness, impact toughness and
wear resistance of M2 high-speed steel after conventional heat treatment are compared with
those imparted by additional subzero and deep cryogenic processing.
Keywords: High speed steel, Cryogenic treatment, Wear resistance, Retained austenite, Toughness, Hardness
Introduction
Conventional hardening (CH) of high-speed steel M2 is
normally performed by austenitising at about 1230uC
followed by cooling to ambient temperature. This
treatment results in significant amounts of retained
austenite which may be reduced in the subsequent
tempering operations. The amount of retained austenite
is increased by increasing the austenitising temperature
and by the lowering of the cooling rate.
Retained austenite has some detrimental effects on the
hardness, wear resistance, machinability and dimen-
sional stability of high-speed steels.1,2 It is therefore
desirable to fully transform the retained austenite
present even after tempering in high-speed steels. This
can be achieved by cryogenic treatments in which steels
are cooled to below the Mf temperature where complete
transformation will occur.
Some investigators35 have drawn a distinction
between cold treatment (CT), at temperatures down
to 280uC or thereabouts, and deep cryogenic treat-
ment (DCT), at about liquid nitrogen temperature
(2196uC), as these two temperature ranges result in
different effects. It has been suggested that two different
mechanisms are operating in the cryogenic treatments of
steels, these being transformation of retained austenite
and low-temperature conditioning of martensite.
Transformation of retained austenite, which is largely
complete for most steels in the temperature range from
270 to 2110uC (CT), results in better dimensional
stability, higher hardness values, lower toughness and
very modest improvement in wear resistance. Continued
cooling of martensite, well below the Mf temperature,
e.g. to 2196uC (DCT), and holding in this temperature
range for sufficient time, results in the precipitation of
very fine carbide particles on tempering.68 The
formation of conditioned martensite results in an
*This is an edited version of a paper originally published in Heat Treatment
of Metals (2000, 27, (3), 6972). At the time of publication, the authors
were in the Department of Metallurgy and Materials Engineering, Faculty
of Engineering, University of Tehran, PO Box 11365-4563, Tehran, Iran.
162 International Heat Treatment and Surface Engineering 2008
improvement in toughness and wear resistance with
little or no increase in hardness.
In the present study, the effects of both cold (CT) and
deep cryogenic (DCT) treatments on the hardness,
toughness and wear resistance of M2 high-speed steel
are discussed and compared with those of the con-
ventionally-treated (CH) material.
Experimental details
The material used was an M2 high-speed steel of
composition 0?87C6?0W4?9Mo4?0Cr1?9V0?4Si
0?2Mn0?2Ni0?1Cu (wt-%). It was received in the
annealed condition as 6 mm-diameter bar from which
all test pieces were cut to length for different purposes.
Austenitising was carried out in a salt bath, held in the
temperature range of 10501200uC, usually for times of
a few minutes. Quenching was conducted in all cases in
another salt bath at 300550uC, with a holding time of
10 min, followed by oil quenching to ambient tempera-
ture. Cold treatment (CT) down to 270uC was
conducted in a mixture of dry ice and ethanol for
90 min. Deep cryogenic treatment (DCT) was per-
formed by immersion in liquid nitrogen (2196uC) for
a duration of 90 min. In all cases, warming to room
temperature was in still air. Tempering was conducted in
an air-circulating furnace held at 300560uC.
After completion of the whole treatment cycles,
different mechanical tests were performed at room
temperature. Hardness values were determined by
standard Vickers HV30. The impact toughness was
measured on a universal impact tester, tested samples
being unnotched specimens having nominal diameters
and lengths of 6 and 55 mm respectively. In order to
avoid any inconsistency of the results, at least four
different specimens were tested and the results were
averaged.
The volume fraction of retained austenite was
determined by X-ray phase analysis at room tempera-
ture. Peaks {211} of martensite and peaks {220} and
{311} of retained austenite were employed. Scanning
electron microscopy (SEM) was used for metallographic
examinations and observation of fracture surfaces.
2008 IHTSE Partnership
Published by Maney on behalf of the Partnership
VOL 2 NO 3/4 DOI 10.1179/174951508X446394

1 Effect of austenitising temperature and cryogenic treat-
ment on a hardness and b toughness of M2 tool steel. All
samples were quenched at 300uC and tempered at 560uC
Wear resistance was measured under dry conditions
using a pin-on-wheel configuration. The wheel was made
of sintered cemented carbide (WCCo) 40 mm in
diameter, having a nominal hardness of 90 RA. The pins
were 4?5 mm in diameter, making a line contact with the
periphery of the wheel. Before testing, the treated steels
were ground to a reference microfinish of 0?8 mm. Tests
were done by rotating the wheel at a peripheral speed of
0?5 m s21, with a normal load of 80 N over distances up
to 2000 m. Wear behaviour was studied by determining
the weight loss, using an electronic balance, after the
specimens were cleaned in acetone.
Experimental results and discussion
Hardness and toughness
The effect of austenitising temperature on hardness and
impact energy is shown in Fig. 1. It is observed that, for
2 Micrographs (SEM) of a CH, b CT and c DCT specimens. Samples were austenitised at 1200uC, quenched at 550uC
and tempered at 560uC
International Heat Treatment and Surface Engineering
Mahmudi et al. Effects of cryogenic treatments on high-speed steel M2
any of the heat treatment processes studied, an increase
in austenitising temperature is accompanied by a
substantial increase in hardness and a drastic decrease
in toughness. Increasing austenitising temperature
results in an enhanced dissolution of alloy carbides
which, in turn, increases the concentration of carbon in
the matrix, leading to higher hardness values. This
harder and more brittle matrix is responsible for the
lower toughness values obtained. It might be expected
that, after quenching from higher austenitising tempera-
tures, greater amounts of retained austenite would
enhance toughness. However, it seems that retained
austenite is eliminated substantially upon cryogenic
cooling and the subsequent tempering at 560uC, result-
ing in lower toughness values.
Lowering the cryogenic treatment temperature
increases the hardness and decreases the toughness,
mainly due to a more enhanced transformation of
austenite to martensite. This effect is much more
pronounced at around the CT temperature range
(270uC), where a large quantity of retained austenite
is transformed to martensite. Lowering the temperature
further in DCT (2196uC) results in less change in both
hardness and toughness. The elimination of retained
austenite in CT and DCT specimens is believed to be
responsible for the 3852 HV improvements in hardness
values and the 2536 J cm22 drop of impact toughness
for the austenitising temperature of 1200uC.
As reviewed in the literature, some investigators have
reported increased toughness after DCT, an effect which
is not observed in the present work. The reason should
be sought in the microstructural changes taking place
after cryogenic treatments. Figure 2 shows the scanning
electron micrographs of the material processed in CH,
CT and DCT. Because of the high austenitising
temperatures involved (1200uC), the structure consists
of fine carbides and agglomerations of large carbide
particles in the martensite matrix. Although the struc-
tures of CH and CT conditions are very similar,
significant carbide refining occurred in the DCT condi-
tion. This might be, in part, due to the low temperature
conditioning of martensite which results in the pre-
cipitation of fine carbides on tempering. However, it is
well accepted that the conditioning process is diffusion
dependent and requires a minimum time and tempera-
ture.9 It seems very likely that the 90 min holding time at
DCT temperature was not sufficient and a longer time is
required to fully condition the structure in order to
significantly improve the impact toughness.
For the various cryogenic treatments, the influence of
quenching temperature on hardness and impact tough-
ness is illustrated in Fig. 3. In contrast to the effect of
austenitising temperature, it can be seen that higher
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Mahmudi et al. Effects of cryogenic treatments on high-speed steel M2
3 Effect of quenching temperature and cryogenic treat-
ment on a hardness and b toughness of M2 tool steel.
All samples were austenitised at 1200uC and tempered
at 440uC
quenching temperatures result in lower hardness and
higher toughness. However, the inverse relation between
hardness and toughness still exists. This behaviour can
be related to the retained austenite present under
different processing conditions. Bearing in mind that
the amount of untransformed austenite is proportional
to the difference between the Ms and quenching
temperature, one may expect a higher amount of
retained austenite for higher quenching temperatures.
This results in a relatively low hardness and a reasonably
4 Effect of tempering temperature and cryogenic treatment on a hardness and b toughness of M2 tool steel. All samples
were austenitised at 1200uC and quenched at 300uC
164 International Heat Treatment and Surface Engineering
high toughness in the CH condition. The low hardness
can be improved significantly by DCT, with only a slight
decrease in toughness, especially for quenching tem-
peratures higher than 450uC.
The influence of tempering temperature on the
hardness and toughness of the material, as shown in
Fig. 4, indicates that a higher tempering temperature
results in higher hardness and lower impact toughness.
However, there are distinct differences in the behaviour
of the material under the various heat treatment
conditions. The variation of hardness with tempering
temperature is much greater for CH than for CT and
DCT. In other words, for cryogenically-treated speci-
mens, tempering at higher temperatures will result in less
hardness improvement without a significant drop in
toughness. This is believed to be due to the effective
transformation of retained austenite which takes place
after CT and DCT and before tempering, reducing the
contribution of the subsequent tempering in the
elimination of austenite. Improvement in hardness,
however, can be attributed to the precipitation of very
fine and hard carbide particles, formed as a result of the
martensite conditioning process.
Fracture surfaces
An SEM study of the fracture surfaces of the Charpy
specimens in the CH, CT and DCT conditions can be
seen in Fig. 5. A mixed-mode fracture, consisting of
quasi-cleavage within the prior austenite grains and low-
energy tear at the pre-existing grain boundaries, can be
detected under all conditions tested. The amount of
plasticity associated with the tear region appears to be
quite small, with not much evidence of dimples or
microvoid coalescence. Quasi-cleavage fracture is typical
of steels that have been quenched and then tempered to
precipitate a fine network of carbide particles.10 Under
these conditions, true cleavage facets are initiated at
carbide particles or large inclusions. This quasi-cleavage
mechanism can be seen in the SEM fractographs shown
in Fig. 5.
Although CH samples exhibited an impact energy of
260 J cm22 which is slightly higher than the 228 J cm22
shown by the DCT samples, no significant differences in
fracture surfaces appearance can be detected. However,
the measured impact energy values decreased in the
order CH, CT and DCT, which corresponds to the order
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 Mahmudi et al. Effects of cryogenic treatments on high-speed steel M2

5 Fractographs (SEM) of a CH, b CT and c DCT specimens. Samples were austenitised at 1200uC, quenched at 300uC
and tempered at 560uC

6 Weight loss as function of a sliding distance (sliding speed: 0?5 m s21) and b sliding speed (sliding distance: 400 m)
for three types of treated specimens given in Table 1. Load is 80 N

of decreasing retained austenite, as shown in Table 1.
The volume of retained austenite was 6?8, 5?1 and 4?0%
respectively for CH, CT and DCT specimens austeni-
tised at 1200uC, quenched at 300uC and tempered at
560uC.
Wear behaviour
The influence of sliding distance and speed on the wear
behaviour of CH, CT and DCT specimens is shown in
Fig. 6. Figure 6a shows the variation of weight loss with
sliding distance up to 2000 m of sliding at a constant
sliding speed of 0?5 m s21. The deep cryogenically-
treated specimens showed the smallest weight loss
followed by those subjected to cold treatment and
conventional hardening at all sliding distances. At
2000 m sliding, the wear resistance of DCT specimens
is about 20% better than CH and 15% better than CT
conditions.
The effects of sliding speed on the wear behaviour of
the specimens, at a sliding distance of 400 m, are
illustrated in Fig. 6b. At all sliding speeds, DCT
specimens are seen to have the smallest weight loss
and the CH specimens the largest, the CT condition
lying between these two limits. It seems that the
transformation of retained austenite to martensite
during sliding has improved the wear resistance of the
specimens, irrespective of heat treatment conditions.
This might be due to the fact that the increased strain
rates at higher sliding velocities can cause some
strengthening which will reduce the wear rate.
Concerning the influence of cryogenic temperature on
wear behaviour, it is observed that, although the volume
fraction of retained austenite is reduced from 6?8 to
5?1%, the improvement in wear resistance in the CT
condition is rather small. However, DCT specimens,
with levels of retained austenite similar to those of the
CT condition (4 and 5?1% respectively), have shown
significantly lower levels of weight loss. Therefore, the
transformation of retained austenite cannot adequately
describe this behaviour and, thus, carbide precipitation
must be the main cause of enhanced wear resistance in
the DCT condition.

Table 1 Processing routes and retained austenite Conclusions

contents of M2 samples used in the wear tests:
samples austenitised at 1200uC, quenched at Different processing parameters, such as austenitising,
300uC and tempered at 560uC quenching and tempering temperatures, have been
shown to affect the mechanical properties and wear
Retained
behaviour of M2 tool steel. Increased austenitising and
Cooling austenite,
Condition temperature, uC vol.-% tempering temperatures, as well as lower quenching
temperatures, increased the hardness and reduced the
Conventional hardening (CH) 25 6.8 impact toughness of the material. This was the case for
Cold treatment (CT) 270 5.1 both conventionally hardened and cryogenically-treated
Deep cryogenic 2196 4.0 conditions. Cold treatment down to 270uC transforms
treatment (DCT)
most of the retained austenite and causes significant

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Mahmudi et al. Effects of cryogenic treatments on high-speed steel M2
gains in hardness and wear resistance and some losses in
the impact toughness of the material.
In deep cryogenic treatments at 2196uC, the hardness
and wear resistance are further improved, due mainly to
a more advanced state of the transformation of retained
austenite and also some precipitation of fine carbide
particles. However, because of short soaking times of
90 min at DCT temperature, the process of carbide
precipitation, which is believed to be the key factor in
increasing toughness, seems to be incomplete and thus
the expected improvement in toughness was not
observed.
Acknowledgements
The authors wish to thank the Research Council of
Tehran University for providing financial support of
this study, under grant no. 61 5111345. This project was
supported by BOC Gases. The Editors of IHTSE are
grateful to the Wolfson Heat Treatment Centre for
permission to reproduce this article.
166 International Heat Treatment and Surface Engineering
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