Academic Journal of Science and Technology 
ISSN: 2771-3032 | Vol. 9, No. 2, 2024 

 

276 

Effect	of	Cryogenic	Time	on	Wear	Resistance	of	M2	High	
Speed	Steel	
Qiang Li, Xiaoyang Huo* 

School of Materials Science and Engineering Henan Polytechnic University, Jiaozuo city 454003, China 
* Corresponding author 

 

Abstract: The wear resistance, residual austenite volume and carbon content in martensite of M2 steel were studied by means 
of universal vertical friction and wear testing machine, X-ray diffractometer (XRD), scanning electron microscope (SEM) and 
digital Rockwell hardness tester. The results show that a large number of fine carbide particles in M2 steel martensite are 
precipitated by cryogenic treatment and distributed uniformly and diffusely in the structure. With the increase of cryogenic time, 
the residual Austenite volume of M2 steel gradually decreases, while the Martensite volume increases, resulting in the wear 
resistance and Rockwell hardness increasing first and then decreasing. After 24 hours of cryogenic treatment of M2 steel, its 
wear resistance increased by 310%, hardness increased by 3.6%. Therefore, 24 hours is confirmed as the best cryogenic treatment 
time for the wear resistance and hardness of M2 steel. 

Keywords: Cryogenic treatment, Friction and wear properties, M2 high speed steel, Carbide, Rockwell hardness. 
 

1. Introduction 
High speed tool steel M2 is widely used and is a kind of 

cold working die steel. The steel has the characteristics of 
high hardness, wear resistance, high temperature stability and 
high strength [1], and is often used in hard cutting materials 
tools, cold extrusion convex die, concave die, cold heading 
die, plastic die and mechanical parts [2]. M2 steel, that is, the 
national standard steel number is W6Mo5Cr4V2, the steel 
number in the American ASTM standard is M2, and the 
Japanese JIS standard is called SKH10. Tool steels are often 
tempered after quenching by Conventional Heat Treatment 
(CHT). This treatment method helps to transform austenite 
into martensite, release internal stress, and improve the 
hardness and toughness of steel. However, a large amount of 
austenite and thick slab martensite are often left in the steel 
after conventional treatment, which is not ideal for improving 
wear resistance. The instability of austenite makes it prone to 
martensitic transformation under heat and mechanical stress, 
resulting in the deformation of workpieces (such as molds, 
tools, etc.), which further affects its accuracy and use effect, 
and may even lead to the failure of mechanical parts and even 
cause safety accidents [3-4]. In the industry, the economic 
loss caused by parts failure is considerable, so it is very 
important to improve the wear resistance of die steel to extend 
its service life and save production costs [5-7]. In order to 
reduce losses and increase efficiency, the wear resistance 
must be improved. 

Cryogenic treatment is a method that can significantly 
improve the wear resistance of materials, thereby extending 
the life of tools and drills. Compared with heat treatment, cold 
treatment has the advantages of simple operation, no damage 
to the workpiece, no pollution, low cost. The effect of cold 
treatment on the material organization is permanent and acts 
on the entire part. Depending on the treatment temperature, 
cold treatment can be divided into Sub-zero Treating (ST) and 
Cryogenic Treating (CT). Shallow cooling treatment is 
generally carried out above -100 ° C, and dry ice with a 
temperature of about -72 ° C is usually used as the treatment 

medium. The cryogenic treatment is carried out in the range 
of -100℃ to -190℃, and liquid nitrogen with a temperature 
of about -198℃ is often used as the cooling medium [8-9]. 

Studies in recent years have shown that the introduction of 
cryogenic treatment can significantly improve the wear 
resistance of tool steel, improve the hardness and dimensional 
stability of steel, and reduce the internal stress [10-20]. 
Therefore, it is widely used in aerospace, automobile, 
electronics and other industries in developed countries, as 
well as in medicine, oil and gas, Musical Instruments and 
other fields. For example, some Swiss watch manufacturers 
place key parts under snow mountains for cryogenic treatment 
to improve the wear resistance and dimensional stability of 
watch parts. However, the effect of cryogenic treatment time 
on the wear resistance of tool steel has not been fully 
discussed in the current literature. It is important to determine 
the optimal cryogenic treatment time, which can not only 
ensure the improvement of material properties, but also 
reduce the cost of cryogenic treatment and improve 
production efficiency. The study of the effect of cryogenic 
treatment time on the wear resistance of M2 steel is helpful to 
promote the development and application of cryogenic 
treatment technology in the industrial field and save energy at 
the same time. Therefore, this study conducted 0-36 hours of 
cryogenic treatment on M2 steel through experiments, aiming 
to explore the influence of cryogenic treatment on the 
properties of M2 steel under different time lengths, and then 
determine the best cryogenic treatment time to improve the 
properties of M2 die steel. 

2. Experimental Materials and 
Methods 

2.1. Material and cryogenic treatment 
The steel used in the experiment is M2 steel rolled, 

softened and annealed by the manufacturer. Table 1 shows its 
main chemical composition (mass fraction, wt %). 5 cuboid 
samples of the same size (10mm× 10mm×55m) were 
processed using EDM wire cutting. 

 



 

277 

Table 1. Chemical composition of M2 steel (mass fraction, %) 
C W Mo Cr Si Mn S P Fe 

0.85 6.38 5.37 4.34 0.228 0.28 0.02 0.067 remain 
 

The sample heat treatment process curve is shown in Fig.1 : 
①Austenitizing and quenching: The sample is heated in the 
furnace to 800℃ for 10min, and then heated to 1200℃ for 
10min before oil quenching. ② Cryogenic treatment: The 
sample is placed in liquid nitrogen (-196℃) for soaking, 
holding time is 1, 12, 24 and 36 h, respectively. After the 

cryogenic treatment, the sample is taken out and placed in the 
air to restore its temperature to room temperature. ③ 
Tempering: Heat the heat treatment furnace at 600℃, and 
then put the sample into the vacuum furnace, hold the heat for 
1 h, air cool to room temperature and remove the surface 
oxide, and grind off the decarbonized layer with sandpaper. 

 

 
Figure 1. Heat treatment process diagram 

 
Table 2 shows the number and grouping of heat treatment 

samples. The number represents the holding time at -196℃. 
CT0 indicates no cryogenic treatment. As the control group of 
the experiment, CT1, CT12, CT24 and CT36 indicate 
cryogenic treatment for 1, 12, 24 and 36h respectively. 

 
Table 2. Numbers of heat treatment samples 

Sample number Heat treatment procedure 
 (1) Quenching (2) cryogenic treatment (3) tempering 

CT0 

1200℃，10min 

0h 

600℃，1h 
CT1 1h 

CT12 12h 
CT24 24h 
CT36 36h 

 

2.2. Characterization experiment 
After grinding and polishing the sample, the phase 

composition was analyzed using the SmartLab 9kw X-ray 
diffractometer, and the phase retrieval function in MDI Jade 
6.5 analysis software was used to determine the residual 
austenite content. The X-ray diffraction test 2θ has a range of 
30° to 90° and a scanning speed of 10° per minute. The test 
was performed under CuKα radiation (wavelength λ=0.15406 
nm) with a current set at 250 mA and a voltage of 40 kV. The 
surface morphology of the fracture was observed using 
Merlin Compact scanning electron microscope. The hardness 
of the sample is tested by an electric Rockwell hardness tester 
(model SHBRV-187.5). Each sample is tested 5 times and the 
hardness value is averaged. 

2.3. Wear test 
The wear test was carried out by using MMW-1 vertical 

universal friction and wear testing machine using pin-disk 
method. In the test, a cylindrical specimen with 
Φ4.8mmx12.7mm was selected as a rotating pin with a 
rotating radius of 24cm. 45# quenched steel is used as the 
material for rotating grinding surface, and the ring size is 

Φ54mm×Φ38mm×10mm, its hardness is 52~55HRC, and the 
surface roughness Ra is less than 0.5m. The sliding speed of 
the rotating pin is 2m/s (corresponding speed is 800rpm), and 
the wear test is carried out under the condition of normal load 
(FN) of 30N (3kgf). Each set of experiments was repeated 
three times at room temperature, the weight of the sample (m1, 
m2) before and after wear was recorded, and the mass loss 
was calculated using an electronic scale with an accuracy of 
0.1mg. The formulas of wear rate (WR) and wear resistance 
(WR) are shown in (1) and (2): 

 

             (1) 

 

              (2) 

 
Where: WR is the wear rate of composite material, unit 

mg/m; m1 represents the mass of the sample before wear, in 
milligrams (mg); m2 represents the mass of the sample after 
wear, also in milligrams (mg); L is the sliding distance of the 
sample in the experiment, in m. WR is wear resistance, FN is 



 

278 

positive load, unit N; VS is the sliding speed in m/s; It is the 
pin wear rate in mg/L, and Hr is Rockwell hardness [6]. 

3. Result and Analysis 

3.1. Residual Austenite volume 
The X-ray diffraction (XRD) patterns of the samples after 

different heat treatments are shown in Fig.2. It can be 
observed from the figure that the (220), (200), (111) crystal 
faces and (110), (200), (221) crystal faces of the residual 
austenite and martensite of the sample show sharp peaks in 
the annealed state, indicating that the grain sizes of austenite 
and martensite are large. After cryogenic treatment, the half-
height width of these peaks decreased, suggesting that the 
grain size became finer. In Fig. 2, the diffraction peak 
intensity of residual austenite (111) and (221) of the 
cryogenically treated sample is reduced, indicating that the 
content of residual austenite is reduced, and cryogenically 
treated sample is helpful to promote the phase transition of 
austenite. 

 

30 40 50 60 70 80 90 100





(3
11

)

 


 Martensite

Austensite

(1
10

)

(2
00

)

(2
21

)

(2
00

)

(2
20

)

 

 

 

In
te

ns
it

y

Annealed sample

CT0

CT1

CT12

CT24

CT36

2

(1
11

)

 
Figure 2. XRD patterns at different cryogenic times 

 
According to industry standard YB/T5338-2019, the 

formula for the volume fraction of residual austenite in steel 
is shown in formula 3: 

 

               (3) 

 
Where: is the total integral number of carbide phase in the 

sample, is the cumulative diffraction line intensity of 
martensite crystal face, is the cumulative diffraction line 
intensity of austenite crystal face, G is the ratio of martensite 
to austenite strength factor. The cumulative diffraction 
intensity of austenite (200) (220) (311) crystal face and 
martensite (200) (211) crystal face is selected as the 
calculated value.  

The residual austenite volume fraction calculated 
according to formula (3) is shown in Fig. 3. The figure clearly 
shows that with the increase of cryogenic time, the content of 
residual austenite in tissues gradually decreases. This is 
consistent with previous research results [21-23], indicating 
that cryogenic time has a significant impact on organizational 
transformation. The content of residual austenite is the 
highest in the initial annealing state, which can be attributed 
to the fact that M2 steel is a high alloy steel, which is rich in 

alloying elements to help the stable existence of austenite at 
room temperature. In contrast, CT0 showed a slight decrease 
in residual austenite content compared to annealed samples. 
This is due to the relatively low martensitic transition 
temperatures Ms and Mf of high alloy steels, which retain a 
large amount of residual austenite even after quenching and 
tempering treatment. It can be observed from the figure that 
the austenite content of CT1 sample decreased sharply, while 
the austenite content of CT12, CT24 and CT36 samples 
decreased slowly. This is because as the amount of austenite 
transformed into martensite increases, the stress existing in 
the organization also increases, and the compressive stress 
state is expected to stabilize austenite, thus making it difficult 
for the residual austenite to further transform [5]. The increase 
of cryogenic time gradually promoted the organizational 
transformation, but the transformation efficiency gradually 
decreased. For the samples with more than 24 hours of 
cryogenic treatment, the austenite content was significantly 
reduced to less than 5%. Cryogenic treatment helps to 
promote the transformation of austenite, and the longer the 
cryogenic soaking time, the number of transformations also 
increases. 

 

4

8

12

16

20

24
21.988

19.773

8.892

7.271

5.857
4.919

Annealed 
  sample

CT36CT24CT12CT1

 

 

R
es

id
ua

l a
us

te
ni

te
 v

ol
um

e 
fr

ac
ti

on
 / 

%

Sample coding

CT0

 
Figure 3. Residual Austenite volume (volume 

fraction, %) 
 

The amplified XRD pattern of the sample M (110) side is 
shown in Fig. 4. Relative to the annealed steel, the peak Angle 
of the other samples shifted to the left between 0.26˚ and 0.72˚. 
After cryogenic treatment, the peak Angle of M (110) surface 
of the sample is obviously shifted to the left, which indicates 
that the spacing d of the crystal surface increases, which 
causes the change of martensite crystal structure. It may be 
that the precipitation of susaturated carbon atoms in 
martensite causes the shift of the peak angular position of 
martensite M (110). 

 

 
Figure 4. Local XRD patterns of different samples 



 

279 

3.2. Microstructure analysis 
The electron microscope scanning images of CT0 and 

CT24 samples are shown in Fig.5. Comparing the two images, 
it is found that the number of carbide particles in CT0 is small, 
and the distribution is not uniform, and most of them are 
distributed in the grain boundary. However, the carbide 
particles in CT24 are smaller and more numerous, and the fine 
carbide is dispersed at the grain boundaries and inside the 
grain. The results show that the cryogenic treatment promotes 
the precipitation of carbides in M2 steel and makes them 
uniformly dispersed in the structure. This is conducive to 
improving the mechanical properties of the material. In 
addition, the grain boundaries of CT0 are clear, while those 
of CT24 are blurred. This may be because cryogenic 
treatment promotes the transformation of austenite to 
martensite, resulting in martensite appearing inside the grain, 
thus blurring the grain boundaries. 

 

 
(a) CT0 

 
                                                              

(b) CT24 
Figure 5. Electron microscope scanning of CT0 and 

CT24 samples 

3.3. Carbon content in martensite 
The carbon content formula (6) of martensite is derived by 

the formula (4)(5)(6) of the lattice parameter relation of 
martensite, and the carbon atom content of M2 steel 
martensite after cryogenic treatment is calculated. 

 

            (4) 

 

             (5) 

 

              (6) 

 

                 (7) 

 
Where, a0 is the lattice constant of a-Fe; p is the percentage 

of carbon content in martensite; a and c are the lengths of the 
martensite axis. d（hkl） is the distance between the crystal faces. 

The carbon content of martensite samples with different 
cryogenic time is shown in Fig.6. With the increase of 
cryogenic treatment time, the content of carbon atoms in 
martensite decreases gradually, which indicates that 
cryogenic treatment can promote the precipitation of carbon 
atoms in martensite matrix. CT0 treatment results in a sharp 
decrease in the carbon content of annealed samples, which 
indicates that tempering can effectively promote the diffusion 
and precipitation of carbon atoms. The carbon atomic weight 
of CT1, CT12, CT24 and CT36 decreased slowly and tended 
to be stable. As can be seen from the figure, susaturated 
carbon atoms are basically precipitated from martensite 
before and after 12 hours of cryogenic treatment, while longer 
cryogenic treatment has little effect on the precipitation of 
carbon atoms. 

 

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4
1.39

0.38 0.35

0.095 0.07 0.062

Annealed sample CT24 CT36CT12CT1CT0

 

 

T
he

 m
as

s 
fr

ac
ti

on
 o

f 
ca

rb
on

 / 
%

Sample coding

 
Figure 6. Carbon content in martensite samples with 

different cryogenic time 
 

Although in the extremely low temperature liquid nitrogen 
immersion environment, the activity of carbon atoms in 
martensite matrix is reduced, and it is not easy to diffuse and 
move. However, plastic deformation occurs during the 
martensitic phase transition, which causes a sliding 
dislocation to trap the immobile carbon atom and carry it to a 
defect, such as a grain boundary or dislocation. This process 
reduces the number of carbon atoms in martensite and 
promotes the aggregation of carbon atoms [24]. With the 
extension of cryogenic time, the degree of phase transition 
and plastic deformation increase, so the number of carbon 
atoms driven by dislocation increases, and the content of 
carbon atoms is further reduced. 

3.4. Hardness 
The hardness values under different cryogenic times are 

shown in Fig.7. With the extension of cryocooling time, 
Rockwell hardness of M2 steel first increased and then 
decreased, and the hardness of CT24 was the highest, 
reaching 67.5HRC. Hardness is affected by a number of 
factors, including: (1) the number, nature and size of 



 

280 

martensite; (2) The amount of austenite; (3) The type, quantity, 
distribution and size of carbides. According to the previous 
analysis, cryogenic treatment promotes the transformation of 
austenite to martensite in M2 steel, thereby increasing the 
amount of martensite in the tissue and the dislocation density 
in martensite. At the same time, the amount of soft austenite 
is reduced, and the distribution of carbides is more uniform 
and the number is increased. With the increase of cryogenic 
time, the influence of these factors gradually increases, 
resulting in a gradual increase in the hardness value. However, 
the hardness of CT36 is reduced, which may be affected by 
the following factors. 

 

65.0

65.5

66.0

66.5

67.0

67.5

65.1

66.3

66.9

67.5

67

CT36CT36CT24CT12CT1

H
ar

dn
es

s 
va

lu
e 

 /H
R

C

Sample coding
CT0

 
Figure 7. Hardness values at different cryogenic times 
 

Cryotreatment causes the secondary hardening peak to 
move to the lower tempering temperature [25-26], forming a 
state of "over-tempering" [27], resulting in the hardness first 
rising and then decreasing. The excessively long 
cryogenically cooling time of the CT36 sample is equivalent 
to being in the state of "over-tempering", which makes the 
carbide in the tissue gradually accumulate and increase, and 
cannot effectively nail the dislocation, resulting in a decrease 
in hardness. In addition, long-term cryogenic treatment will 
also cause M3C carbides to become coarser, further reducing 
hardness. Cryogenic treatment promotes the precipitation of 
carbides in large quantities and intensifies the decomposition 
of martensite, so the hardness also decreases slightly [28-30]. 
In the structure of CT36, the alloy carbide increases and 
martensitic decomposition increases, resulting in a slight 
decrease in hardness compared with CT24. In addition to the 
above influencing factors, the content of austenite also affects 
the hardness. Although the austenite content of CT36 
decreased by 1% compared to CT24, the hardness decreased 
when it should have increased, indicating that the hardness 
was more significantly influenced by martensite and carbide. 
The final hardness curve is the result of the competition of the 
above three factors. 

3.5. Wear rate and wear resistance 
According to formula (1) and (2), the calculated wear 

resistance and wear rate of the sample are shown in Fig.8. 
Compared with the samples of conventional treatment, the 
wear of the samples of cryogenic treatment first decreased 
and then increased with the extension of holding time. When 
the cryogenic treatment time reached 24 h, the wear rate of 
the sample was the lowest. There is a critical value of 24h for 
the effect of the deep cooling time on the wear rate of M2 
steel. The wear rate of CT36 samples increased significantly, 

indicating that the improvement of wear resistance by 
cryogenic cooling time is limited, and too long treatment is 
not conducive to the improvement of wear resistance. The 
wear resistance of D2 tool steel decreases after 36 hours of 
cryogenic cooling[31], which is similar to the results obtained 
in this paper. It can be seen from the wear resistance diagram 
that the wear resistance of M2 steel first increases and then 
decreases, which is exactly the opposite of the change 
diagram of wear rate. 

 

12.64

10.28

9.03

3.89

15.97

0

3

6

9

12

15

18

CT36CT24CT12CT1CT0

 

W
ea

r 
ra

te
/（

m
g/

m
）

Sample number

0.5

1.0

1.5

2.0

2.5

3.0

3.5

1

1.22
1.37

3.18

0.77

 
Im

pr
ov

em
en

t o
f 

w
ea

r 
re

si
st

an
ce

Sample number

CT0 CT1 CT12 CT24 CT36

 
Figure 8. Wear rate and wear resistance of samples 

 
During the wear process, a contact layer is formed between 

sliding surfaces, and the structure and properties of the 
contact layer determine its wear behavior [32-33]. The 
cryogenic treatment increases the hardness of M2 steel, 
increases the carbide and decreases the residual austenite 
volume, thus reducing the degree of friction thermal softening, 
improving the resistance to thermoplastic deformation and 
improving the wear resistance. 

The amount of austenite in the tissue of CT36 sample is 
small (only 4%), indicating that there is more martensitic 
transformation, and theoretically the wear resistance should 
be further improved. However, contrary to the experimental 
results, the wear resistance of CT36 was significantly reduced. 
There may be several reasons for this phenomenon: First, the 
austenite volume in CT36 sample is too low, which may not 
be enough to effectively inhibit crack growth, but lead to 
reduced wear resistance. Secondly, long-term cryogenic 
treatment leads to the most significant refinement 
decomposition of tempered martensite twins, which is 
unfavorable to the improvement of wear resistance. In 
addition, the large-sized secondary carbides precipitated in 
the CT36 sample are easy to be peeled to form pits in the wear 
process, resulting in abrasive wear, which further intensifies 
the wear amount and reduces the wear resistance. Finally, too 



 

281 

long cryogenic cooling time may cause microscopic internal 
stress in the martensitic structure, making the material more 
vulnerable to damage during friction, resulting in reduced 
wear resistance [35]. 

4. Conclusions 
1) The residual austenitic transition of M2 steel is 

positively correlated with the cryogenic time. In the initial 
stage of cryogenic treatment, the volume of Austenite 
decreased significantly, and the transformation rate gradually 
slowed down in the later stage. Cryogenic treatment 
significantly reduces the residual austenite volume in M2 
steel to less than 5%. 

2) With the extension of cryogenic time, the Rockwell 
hardness of M2 steel does not continue to increase, but first 
gradually rises, and then slightly decreases. After 24 hours of 
cryogenic treatment, the hardness of the steel reached the 
maximum value (67.5HRC), which was 3.6% higher than that 
of conventional treatment. 

3) Cryogenic treatment promotes a large number of carbide 
particles in M2 steel to precipitate, resulting in a uniform 
distribution of fine carbide particles in the organization. With 
the extension of cryogenic time, the carbon content in M2 
steel martensite decreased significantly, almost making the 
martensite without carbon atoms. 

4) Cryogenic treatment improves the wear resistance of M2 
steel, and the wear resistance gradually increases with the 
increase of cryogenic time. When the cryogenic time reaches 
24 hours, the wear resistance of M2 steel reaches the highest 
point, which is 3.1 times that of the sample without cryogenic 
treatment. Therefore, the experimental results show that 24 
hours of cryogenic treatment in liquid nitrogen environment 
is the best cold treatment process. 

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