Journal of Materials Processing Technology 118 (2001) 350±355

Effect of deep cryogenic treatment on the mechanical

properties of tool steels
A. Molinaria,*, M. Pellizzaria, S. Gialanellaa, G. Straffelinia, K.H. Stiasnyb
a
University of Trento (I), Trento, Italy
b
GKN Bir®eld AG, Brunico (BZ), Brunico, Italy

Abstract

The effect of deep cryogenic treatment ( 1968C) on the properties of some tool steels was studied by means of both ®eld tests on real
tools and laboratory tests. The execution of the deep cryogenic treatment on quenched and tempered high speed steel tools increases
hardness, reduces tool consumption and down time for the equipment set up, thus leading to cost reductions of about 50%. A laboratory
investigation on an AISI M2 and an AISI H13 steel con®rms the possibility of increasing the wear resistance and toughness by carrying out
the treatment after the usual heat treatment. # 2001 Elsevier Science B.V. All rights reserved.

Keywords: Deep cryogenic; Tool steels

1. Introduction data from the industrial production. At the same time, a

Cold treating is widely used for high precision parts and
components, since it enhances the transformation of auste-
nite to martensite. The common practice identi®es 60 to
808C as the optimum temperature, according to material
and the quenching parameters. Many companies use this
kind of treatment to improve surface hardness and thermal
stability.
Deep cryogenic treatment in the range 125 to 1968C
improves certain properties beyond the improvement
obtained by normal cold treatment [1±4]. The main reason
for this is the complete transformation from austenite into
martensite plus the formation of very small carbides dis-
persed in the tempered martensitic structure [5]. The greatest
improvement in properties is obtained by carrying out the
deep cryogenic treatment between quenching and temper-
ing. However, a signi®cant improvement can be obtained
even by treating the tools at the end of the usual heat
treatment cycle, i.e. the ®nished tools. This last solution
is more ¯exible than the other one and can extend the use of
the treatment to many practical applications.
In order to check the potential of the deep cryogenic
treatment on the performances of the ®nished products, ®eld
tests were carried out on some high speed steel tools, and the
results were recorded for a long time, in order to get reliable
*
Corresponding author. Tel.: ‡10-39-461-881919;
fax: ‡10-39-461-881999.
speci®c laboratory investigation was carried out on two
steels: the AISI M2 high speed steel and the AISI H13
hot work tool steel. These experiments were aimed at the
study of the effect of the treatment on some mechanical
properties and on the wear resistance of the two steels. In the
laboratory tests, the deep cryogenic treatment was carried
out at different stages of the usual heat treatment route, i.e.
both after quenching and after tempering. The results of the
tests are presented and discussed here.
2. Field tests on HSS
Fig. 1 is a schematic representation of the cryogenic
equipment. It comprises an insulated box (cryo box), one
motor with a circulating fan, one thermocouple to measure
the cryogenic temperature inside the box connected to a
temperature controller and programmer, a liquid nitrogen
tank and a solenoid valve for the gas inlet. The actual
temperature of the mass loaded in the box is recorded by
a thermocouple inserted in a 30 kg steel block.
Fig. 2 shows the cryogenic cycle: the thin and the bold
lines represent the set up temperature and the test probe
temperature, respectively. One of the most critical para-
meters is the cooling rate which must not exceed 20±308C/h
in order to prevent the rupture of the components because of
the cooling stresses. The soaking time at the minimum
temperature is about 35 h; a more prolonged period does

0924-0136/01/$ ± see front matter # 2001 Elsevier Science B.V. All rights reserved.
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 A. Molinari et al. / Journal of Materials Processing Technology 118 (2001) 350±355 351

Fig. 1. Block diagram of the cryogenic equipment.

not have any signi®cant effect. The total duration of the material. For instance, the microhardness of an ASP 60
treatment is about 100 h. spline forming tool was increased from 953  20 HV0:05 to
The deep cryogenic treatment has a noticeable effect on 1234  23 HV0:05 (‡29.5%). In another case, an AISI M2
the hardness of the tools. However, the effect depends on the drill, the microhardness did not change after the deep

Fig. 2. Cryogenic cycle.

352 A. Molinari et al. / Journal of Materials Processing Technology 118 (2001) 350±355

Table 1
Comparison of normal and cryogenic treated centring drills

Number of parts produced per drill Average of parts produced

with one drill

Normal condition drills 175 190 326 64 297 210

Cryogenic treated drills 385 490 161 962 821 335 116 970 530

cryogenic treatment (890 HV0.1), but its distribution on the

cross-section improved, the standard deviation being
decreased from 64 to 22.
Field tests were carried out on different tools. As an
example, Table 1 compares the number of parts produced
by centring a 21NiCrMo2 annealed steel, in the usual
production conditions.
The data reported shows a noticeable increase in the
number of parts produced per drill due to the deep cryogenic
treatment. Moreover, the data dispersion indicates the need
to carry out a signi®cant number of tests in order to get
reliable information on the effect of the cryo treatment.
The treatment was even experimented on the tools for
spline cold forming a C50 steel, heat treated to 200±250 HB.
In this case, the tools were made of AISI M2 HSS. The tests
were carried out by using two tools: one treated in the usual
conditions, the other in cryogenic treated conditions, work-
ing together, in order to make the comparison as reliable as
possible. In fact, in this way the two tools are working the
same material, with the same machine and set up and with
the same operator. Already after 20,000 parts machined,
evidently more wear appeared on the non-cryogenic treated
tool, which failed after 48.700 parts machined due to
excessive wear. Fig. 3 compares the surface morphology
of the two tools after 48.700 parts produced.

3. Laboratory tests on HSS

Tests were carried out on an AISI M2 steel. The base

treatment was the usual one, comprising vacuum quenching
from 12208C and two tempering cycles at 5508C for 2 h each
(A). The deep cryogenic treatment was carried out both after
the two temperings (B) and after quenching; in this case one
(C) and two (D) tempering cycles were carried out. Table 2
summarises the specimens investigated (Q is the quenching,
T the tempering, and C the deep cryogenic).
Wear tests were carried out on an Amsler trybotester (disk
on disk geometry). Dry sliding tests were carried out by
using a 100Cr6 steel hardened to 64 HRc as a counterface
material. After some preliminary tests, the following test
Fig. 3. Surface morphology of normal treated (a) and cryogenic treated (b)
conditions were set up: load, 150 N and sliding speed, 0.8 m/ spline rolling tools.
s for a total sliding distance of 5000 m. For example, Fig. 4
shows the wear curve of specimen B. Since the experimental
points can be interpolated by a straight line in all the Table 3 shows that the deep cryogenic treatment increases
experiments, the slope of the line was calculated to measure both the dry wear resistance and the hardness of AISI M2
the wear rate. Table 3 shows the wear rate and the hardness and that the two effects are correlated, i.e. the higher the
measured on the different specimens. hardness, the lower the wear rate. The analysis of the wear
 A. Molinari et al. / Journal of Materials Processing Technology 118 (2001) 350±355 353

Table 2 debris allows the wear mechanism to be identi®ed: oxidative

Investigated specimens wear with the contribution of abrasive wear caused by the
Code Treatment hard carbides dispersed in the microstructure of the two
counterfacing materials. Since both mechanisms are in¯u-
A Q‡T‡T
B Q‡T‡T‡C enced by hardness, the correlation between hardness and
C Q‡C‡T wear rate can be explained: an increase in hardness increases
D Q‡C‡T‡T the abrasion resistance and the load bearing capacity of the
material, i.e. the ability to support the surface layers where
frictional heating causes oxidation. Therefore, it may be
concluded that the deep cryogenic treatment increases the
hardness of AISI M2 steel and, in turn, dry sliding wear
resistance. Moreover, the results in Table 3 shows that the
effect of the deep cryogenic treatment is highest when the
treatment is carried out on the quenched and tempered steel.
The execution of the treatment before tempering leads to a
lower improvement of the properties of the steel.
Impact tests on V-notched Charpy specimens were carried
out on materials A and B only, because they represent the
extreme behaviour. Impact energy was the same for the two
materials (2 J). Contrarily, three points bending tests
revealed a signi®cant increase in both strength (as computed
by the Navier equation, since the bending behaviour was
purely brittle, as shown in Fig. 5 relating to the specimen A)
and absorbed energy after the deep cryogenic treatment:
Fig. 4. Wear curve obtained for specimen B. 3230 MPa and 0.56 J for material B, 2680 MPa and 0.38 J
for material A. Given the purely brittle behaviour, the
increase in the bending properties can be attributed to the
increased hardness of material B. Impact tests are not
Table 3
Results of wear tests
sensitive to the increase in hardness likely because of the
higher strain rate than bending tests.
Specimen Wear rate …g=m  10 6 † HV30 In order to interpret the above results, materials A and B
A 3.7 826 were characterised at optical microscope and scanning
B 1.8 894 electron microscope, without revealing any differences
C 2.2 888 caused by the deep cryogenic treatment. In addition, the
D 2.4 874
residual austenite was lower than the detection limit of the
X-ray diffractometry (2%) in both cases. Therefore, the

Fig. 5. Bending test curve of material A.

354 A. Molinari et al. / Journal of Materials Processing Technology 118 (2001) 350±355
Fig. 6. Microstructure of tempered martensite in material A.
effect of the deep cryogenic treatment must be sought in the
submicroscopic microstructure of the steel. Some authors
attribute the effect of the deep cryogenic treatment, when
carried out after quenching and prior to tempering, to the
activation of the tempering transformations of the virgin
martensite, because of its high oversaturation attained at
1968C [5]. Because of this, the carbide precipitation
occurs with a higher activation energy, thus leading to a
higher nucleation rate and, in turn, to ®ner dimensions and a
more homogeneous distribution. However, in our experi-
ments, the deep cryogenic treatment was carried out after
two tempering cycles, and therefore on a less oversaturated
martensite, so that the effect on the carbides is lower.
Preliminary TEM analyses did not reveal signi®cant differ-
ences in the carbides dispersed in the tempered martensite.
Instead, Figs. 6 and 7 show the submicrostructure of the
tempered martensite in materials A and B, respectively.
While the tempered martensite shows a twinned submicros-
tructure, that cryogenically treated does not show any twins.
This result was con®rmed by several observations. No
evidence was found in the literature of this phenomenon
(tempered martensite detwinning). Further experiments are
Fig. 7. Microstructure of tempered martensite in material B.
ongoing in order to con®rm and study the phenomenon in
more detail.
The reason why the deep cryogenic treatment has a lower
effect when carried out after quenching and followed by the
usual tempering is not yet clear. The results here presented
contrast with those of Yun et al. [5]. However, in that case the
steel has been quenched from a higher temperature
(12808C), which leads to a greater oversaturation of the
virgin martensite and to a higher retained austenite content.
This could in¯uence the transformation during tempering
and modify the effect of the deep cryogenic. Further experi-
ments are in course.
4. Laboratory tests on hot work tool steels
Tests were carried out on an AISI H13 hot work tool steel.
The base treatment comprises vacuum quenching from
10208C and two tempering cycles at 5708C for 3 h each
(A). Also in this case, the deep cryogenic treatment was
carried out both after the two temperings (B) and after
quenching; again one (C) and two (D) tempering cycles
were carried out on the quenched and deep cryogenic treated
steel. Therefore, Table 3 summarises the AISI H13 speci-
mens investigated, as well.
First of all, hardness, impact energy (E) and toughness
(KIC) were measured on the different specimens, obtaining
the results reported in Table 4. Both impact and fracture
mechanics tests were carried out on V-notched Charpy
specimens, with a 0.25 mm notch radius.
The results show that the cryogenic treatment, when
carried out after the usual heat treatment, increases tough-
ness and does not in¯uence hardness and impact energy; in
other words, the increase in toughness is attained without
reducing hardness. A toughness increase can be obtained,
even if lower, by carrying out cryogenic treatment just after
quenching. In this case, as for the usual heat treatment
procedure, the number of tempering cycles cannot be
reduced to one, because of the excessive brittleness of the
single-tempered material. The same wear tests as above were
carried out on specimens A and B. Given the lower hardness
of AISI H13 than AISI M2, the predominant mechanisms are
oxidative wear, abrasion and delamination, as detected by
the debris analysis (Fig. 8).
Even in this case the experimental points of the wear
curves can be interpolated by a straight line over the whole
sliding distance, and the wear rate can be determined by the
Table 4
Results of mechanical tests on the AISI H13
Specimen HRc E (J) KIC (N/mm3/2)
A 46.5 17.9 42.8
B 46.7 18.1 49.1
C 49.7 13.6 45.4
D 47.9 16.9 45.0
 A. Molinari et al. / Journal of Materials Processing Technology 118 (2001) 350±355
Fig. 8. Diffraction pattern of the collected wear debris.
slope of the wear diagram. Wear rates are one order greater
than in AISI M2, and a signi®cant difference between the
two specimens was determined: 2:1  10 5 for specimen A,
1:5  10 5 for specimen B. The deep cryogenic treatment is
therefore able to strongly reduce the wear rate of the hot
work tool steel. This result can be interpreted on the basis of
increased toughness, because in the presence of delamina-
tion the ability of the material to oppose crack propagation
can really increase the mechanical stability of the wear
surface and the load bearing capacity. Therefore, even if
the deep cryogenic treatment does not in¯uence the hardness
of the AISI H13 steel, it increases both toughness and wear
resistance. This effect can have an important effect on the
performances of the tools, in particular those used for Al
extrusion and for the hot forming of steels, where wear
resistance and toughness are frequently the key properties.
Also, in this case the metallurgical interpretation of the
results must be found in the submicroscopic microstructure
of the steel. A speci®c investigation based on TEM analyses
is ongoing.
5. Conclusions
The deep cryogenic treatment ( 1968C) of quenched and
tempered high speed steel tools improves their properties; in
particular, it increases the hardness and improves the hard-
ness homogeneity, reduces the tool consumption and the
355
down time for the equipments set up, thus leading to about
50% cost reduction. In addition to the ®eld tests, laboratory
tests were carried out on two different steels in order to study
the effect of the deep cryogenic treatment on some mechan-
ical properties and on the wear resistance. While in the AISI
M2 steel the increase in wear resistance can be attributed to
the increased hardness, in the case of the AISI H13 steel the
increased wear resistance can be correlated to the increased
toughness. When the cryogenic treatment is carried out after
quenching and followed by the usual tempering cycle, its
in¯uence on the properties of steel is negligible.
The results presented here are not exhaustive; TEM
analyses are being carried out in order to investigate the
submicrostructure of the treated materials in the different
treatment conditions.
References
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tool steel, Heat Treatment Met. 3 (1997) 71.
[4] P.L. Yen, Formation of fine eta carbides in special cryogenic and
tempering process key to improved properties of alloy steels, Ind.
Heating 1 (1997) 40.
[5] D. Yun, L. Xiaoping, X. Hongshen, Deep cryogenic treatment of high-
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