Acta Materialia Transylvanica 2/2. (2019) 87–92.

https://doi.org/10.33924/amt-2019-02-04
Hungarian: https://doi.org/10.33923/amt-2019-02-04
https://eda.eme.ro/handle/10598/31509

Examination of Heat Treatment on the Microstructure

and Wear of Tool Steels
Enikő Réka Fábián,1 László Tóth,2 Csenge Huszák3
Óbuda University, Donát Bánki Faculty of Mechanical and Security Engineering, Budapest, Hungary
1 [email protected]
2 [email protected];
3 [email protected]

Abstract
The microstructure of the investigated X153CrMoV12 grade tool steel in delivered condition consisted of
spheroidal matrix and primary carbides. The primary carbides were not dissolved under austenitisation
time on either 1030°C or 1070°C. The microstructure and abrasion resistance of the steel changed due to
quenching from different austenitisation temperatures. After conventional quenching from the higher aus-
tenitising temperature, there is more residual austenite in the steel than at quenching from the lower auste-
nitisation temperature, which decreased the wear resistance. As a result of quenching from 1070°C followed
by a multiple tempering process around 500 to 540°C, the retained austenite content is reduced and finely dis-
persed carbides are precipitated in the matrix, resulting in a higher matrix hardness and an increased wear
resistance. After cryogenic treatment, the residual austenite content decreases compared to the conventional
process, which leads to an increase in hardness and wear resistance.
Keywords: tool steel, austenitisation, retained austenite, precipitation, cryogenic treatment, tempering,
wear resistance.

1. Introduction ally achieved after quenching from 930–960 °C

[1]. Using high quenching temperature (1100 °C),
The X153CrMoV12 grade steel is commonly used
secondary hardening appears in the material
by tool makers as a raw material for blanking and
the maximum hardness result after tempering
punching tools, woodworking tools, shear blades
at 520–530 °C. The standard [2] recommendation
for cutting light-gauge material, thread rolling
for austenitisation is 1020°C, and cooling in air.
tools, tools for drawing, deep drawing and cold
The standard for maximum hardness (over 62
extrusion, pressing tools for the ceramics and
HRC) recommends 970°C for austenitisation, air
pharmaceutical industries, cold rolls (working quenching followed by tempering under 200°C
rolls) for multiple-roll stands, measuring instru- Voestalpine is one of the world's leading tool
ments and gauges and small moulds for the plas- steels, high-speed steels and special steels manu-
tics industry where excellent wear resistance is facturers. The company publication does not pro-
required. This steel in delivered condition is an- vide data on secondary hardening after the hard-
nealed, the hardness is max. 250 HB. In this state ening process from 1030 °C, but secondary hard-
the steel is relatively easy to be manufactured ening is expected at 520 °C after hardening from
despite its high alloy content. The properties 1070 °C, so double tempering at this temperature
of the tool are achieved in the final heat treat- is recommended before any nitration [3]. Inter-
ment. There are differences in the recommenda- alloy recommends triple tempering at 500–550°C
tions for heat treatment, despite the fact that the [4]. Cryogenic treatment is not mentioned by
X153CrMoV12 grade steel is widely used. Small companies, nor by the standard, although when
dimension changes and high hardness is usu- cooled to room temperature with this carbon con-
88 Fábián E. R., Tóth L., Huszák Cs. – Acta Materialia Transylvanica 2/2. (2019)

tent, the martensitic transformation is not com-

pleted [5]. While company data do not suggest a
relationship between wear resistance and heat
treatment parameters, the effects of deep cooling
and tempering on mechanical and wear proper-
ties have been addressed by several researchers
for similar cold forming tool steels [6–11]. The
tool makers ask from the heat treatment shops
only the Rockwell hardness, however, tool life,
wear resistance, and toughness depend also on
the heat treatment technology.

2. Test materials and methods Figure 1. Abrasive equipment

The chemical composition of the examined
X153CrMoV12 grade steel is shown in Table 1. loading force was provided by the sample which
supported a load with 50 g.
Table 1. Chemical composition of the test material
The wear factor (K) was used as a measure of
C Cr Mo V Si Mn Fe wear resistance, calculated from the volume
1.67 11.25 0.837 1.41 0.364 0.422 rest
mass loss (Vv), the sliding distance (s) and the nor-
mal load (F):
Austenitization of the 20×40×20 mm samples
was carried out at 1030°C and 1070°C, respec- (1)
tively, in an Ipsen VFC type vacuum furnace with
300 × 370 × 200 mm chamber size after a two-hold- The volume mass lost is calculated from the di-
ing steps at 650 °C and 900 °C. Some of the sam- ameter of the calotte formed during the wear (d)
ples were quenched down to 40 °C conventionally, and the depth of the crater (h):
using nitrogen gas, and some samples were cryo-
genic treated in nitrogen to –80 °C for 3 hours. The (2)
effects of simple and multiple tempering on the
microstructure and wear resistance were studied The height of the abrasive calotte is calculated
for the conventional and cryogenic quenching. by a simple relationship between the radius R of
The experimental samples were examined after the abrasive ball and the diameter of the calotte
metallographic preparation using an Olympus formed during the wear test:
PMG3 light microscope (LOM) and a Jeol JSM 5310
scanning electron microscope (SEM). Primary ex-
(3)
amination was of the carbides size and distribu-
tion in the microstructure using nital. For the de-
termination of retained austenite the Beraha'2 re- The sliding distance (s) depends on the time of
agent (85 ml water, 15 ml HCl, 1 g K2S2O5) proved the wear (t), on the radius of the abrasive ball (R)
to be the most suitable. Beraha'2 reagent colors and its rotational speed (n) (4):
the ferrite and martensite but not austenite and
carbides. The primary carbides are clearly distin- (4)
guishable from the matrix. The carbide precipi-
tations in the matrix are spherical, and so could For comparison with literature data [11–12], the
be distinguished from the residual austenite. The speed was 570 rpm and the abrasion test time was
hardness of the carbides and of the matrix after 5 minutes.
different heat treatments was measured with
Vickers hardness testing equipment type Buhler 3. Test results
1105. The hardness of the tested X153CrMoV12 grade
For the wear resistance testing, a self-developed tool steel in delivered condition was 248 HV 1
abrasive equipment was used [12] (Figure 1.). on average and its microstructure consisted of
The used abrasive tool was a 20 mm diameter a spheroidal matrix and primary carbides. The
Al2O3 ceramic ball with polished surface. The austenitisation temperature recommended by
Fábián E. R., Tóth L., Huszák Cs. – Acta Materialia Transylvanica 2/2. (2019) 89

Voestalpine Hungary Kft. strongly influences the

microstructure and hardness of the treated ma-
terial.
3.1. Effect of the austenitisation temperatu-
re
Examining the microstructure of the samples,
it was found that the primary carbides did not
dissolve during heating at 1070°C, as can be seen
in the photos of Figures 2. a) and b). As shown
in the photos of Figures 2. c) and d), quenching
from a higher austenitization temperature result- a)
ed in more residual austenite than in the case of
quenching from 1030 °C. Hardness and wear re-
sistance test results are fully consistent with the
microstructure. When the sample was quenched
from 1030 °C, the average hardness of the matrix
was 674 HV 1, while for the sample quenched from
1070°C it was 648 HV 1. By increasing the austeni-
tising temperature, the wear coefficient increased
from 2.46 10–5 mm3/Nm to 2.94 10–5 mm3/Nm due
to the higher retained austenite content. The dis-
tribution of retained austenite is always uniform
in the matrix. The primary carbides appearance
b)
was similar after quenching from 1030°C and
1070°C. This microstructural similarity explains
the phenomenon that the Rockwell hardness-
es measured after quenching are the same (Ta-
ble 2.).

Table 2. The effect of heat treatment parameters on

hardness and wear resistance
Tempering
Hardening
(°C) K
HRC HV 1
TA (mm3/Nm)
HRC T1 T2 T3
(°C)
1030 62 – – – 62 674 2.46·10–5 c)
1030 62 200 – – 61 668 1.56·10–5
1070 62 – – – 62 648 2.94·10–5
1070 62 200 – – 61 641 1.04·10–5
1070 61 520 – – 60 663 2.22·10–5
1070 61 520 540 – 59 685 3.00·10–5
1070 61 520 540 500 59 748 2.46·10–5

3.2. Effect of tempering

The temperature and number of cycles of tem-
pering following the quenching after austenitiza-
d)
tion at 1070 °C significantly influence the micro-
structure, hardness and wear properties of the Figure 2. The effect of the hardening temperature on
X152CrMoV12 steel. The amount of fine dispersed the microstructure; LOM image. Etching agent:
Beraha-2. a) c) Taust = 1030 °C b) d) Taust = 1070 °C
carbides in the martensite is very small (photos
90 Fábián E. R., Tóth L., Huszák Cs. – Acta Materialia Transylvanica 2/2. (2019)

a) a)

b) b)

c) c)

d) d)
Figure 3. The effect of tempering temperature on Figure 4. The effect of tempering temperature on mi-
microstructure; LOM images. TAust = 1070 °C. crostructure. SEM images.Etching agent: 2% Ni-
Etching agent: 2% Nital. a) quenched, b) Ttemper = tal. a) Ttemper = 200 °C, b) Ttemper = 520 °C, c) Ttemper
200 °C, c) Ttemper = 520 °C, d) Ttemper = 520 °C + = 520 °C + 540 °C, d) Ttemper = 520 °C + 540 °C + 500
540 °C + 500 °C °C
Fábián E. R., Tóth L., Huszák Cs. – Acta Materialia Transylvanica 2/2. (2019) 91

in Figure 3. b), Figure 4. a)) when the sample is Table 3. The effect of deep cooling on matrix hard-
tempered at 200 °C after quenching. After temper- ness and wear factor
ing at high temperature (520 °C) the result is fine
Cool- Wear fac-
dispersed carbides precipitations, but retained Tempering
Austeni- ing tor
(°C)
austenite can be detected as shown in the photos tisation (°C) (mm3/N·m)
of Figure 3. c) and Figure 4. b) Multiple high-tem- (°C) HV1
perature tempering processes result in a higher T T1 T2 T3 K·
mátrix
quantity of fine, dispersed carbides in the micro- 1070 20 510 – – 663 4.29·10–5
structure while the residual austenite content de-
1070 –80 510 – – 746 2.66·10–5
creases, as shown in the photos of Figures  3. c),
d) and 4. c), d) The characteristic of the primary 1070 20 510 480 480 695 3.00·10–5
carbides does not change significantly. 1070 –80 510 480 480 738 2.24·10–5
Changes in microstructure due to tempering at
500–550 °C increase the hardness of the matrix.
Due to multiple tempering around 500–550 °C, the
hardness of the matrix increased to 750 HV 1 (Ta-
ble 2.).

3.3. The effect of cryogenic treatment

High-temperature tempering is required for
tools that would be nitrided [1, 3]. Nitrided prod-
ucts typically require dimensional accuracy, so a
large amount of residual austenite is not allowed.
In our investigations it was found that the resid-
a)
ual austenite content of the cryogenic treated
workpiece is low even after a single high-tem-
perature tempering process compared to the
conventional treated sample (Figure 5. a) , 2. c)).
The triple high-temperature tempering process
decreases the residual austenite content further
(Figure 5.).
Due to cryogenic treatment the hardness of the
matrix increase, and its positive effect on the
wear factor is clearly demonstrated (Table 3.).

4. Conclusion
Increasing the austenitisation temperature re- b)
duces the hardness of the martensitic matrix af- 5. ábra. The effect of deep cooling on texture LOM
ter quenching due to the increasing amount of images Etching: 2% nital , Tquench = –80 °C a)
residual austenite. Multiple high-temperature Ttemper = 510 °C, b) Ttemper = 510 °C + 480 °C + 480 °C
tempering increases the hardness of the sample
quenched from 1070 °C, partly due to the reduc- References
tion of residual austenite content and partly due [1] Smóling K., Czeglédi L.: Szerszámacélok kéziköny-
to the finely dispersed precipitates. Cryogenic ve. Szabvány Kiadó, Budapest, 1977. 94–95.
treatment causes a good reduction in the amount [2] MSZ EN ISO 4957: 2018. Szerszámacélok
of residual austenite and an increase in wear re- [3] Voestalpine Böhler Edelstahl GmbH & Co KG:
sistance. Szerszámacélok, nemesacélok, 45.
http://www.boehler.hu/media/productdb/down-
Acknowledgments loads/K110DE.pdf (accessed on: 2019. 01.28)
[4] Interalloy Engineering Steels and Alloys: Product
The authors would like to thank the Hungarian state datasheets, Tool steel D22011 Inter-alloy Pty Ltd
and the European Union for the financial support of (accessed on: 2019. 02.15)
our work in the framework of the project EFOP-3.6.1- http://www.interlloy.com.au/our-products/tool-
16-2016-00010. steel/d2-tool-steel-x153crmov12
92 Fábián E. R., Tóth L., Huszák Cs. – Acta Materialia Transylvanica 2/2. (2019)

[5] Capdevila C. et al.: Determination of Ms tempera- [9] Das D., Sarkar R., Dutta A. K., Ray K. K.: Influence
ture in steels: A Bayesian Neutral Network Model. of sub-zero treatments on fracture toughness of
ISIJ International, 42. (2002) 894–902. AISI D2 steel. Materials Science Engineering A,
https://doi.org/10.2355/isijinternational.42.894 528. (2010) 589–603.
[6] Gavriljuk V. G., Theisen W., Sirosh V. V.: Low-tem- https://doi.org/10.1016/j.msea.2010.09.057
perature martensitic transformation in tool steels [10] Das D., Dutta A. K, Ray K. K.: Sub-zero treatments
in relation to their deep cryogenic treatment. Acta of AISI D2 steel: part II. Wear behaviour. Materi-
Materiala, 61. (2013), 1705–1715. als Science and Engineering A, 527. (2010) 2194–
https://doi.org/10.1016/j.actamat.2012.11.045
2206.
[7] Das D., Dutta A. K., Toppo V., Ray K. K.: Effect of
https://doi.org/10.1016/j.msea.2009.10.071
deep cryogenic treatment on the carbide precipita-
[11] Kumar S., Nagaraj M., Khedkar N. K., Bongale A.:
tion and tribological behaviour of D2 steel. Mate-
rials Manufacturing. Process, 22. (2007) 474–480. Influence of deep cryogenic treatment on dry slid-
https://doi.org/10.1080/10426910701235934 ing wear behaviour of AISI D3 die steel. Materials
[8] Molinari A., Pellizzari M., Gialanella S., Straffelini Research Express, 5/11. (2018) 116525, 1–9.
G., Stiasny K. H.: Effect of deep cryogenic treat- https://doi.org/10.1088/2053-1591/aadeba
ment on the mechanical properties of tool steels. [12] Kovács T., Dévényi L.: Kopásvizsgálati eljárás fej-
Journal of Materials Processing Technology, 118. lesztése. Anyagok világa, 5/1. (2004).
(2001) 350–355. https://www.kfki.hu/~anyag/tartalom/2004/
https://doi.org/10.1016/s0924-0136(01)00973-6 dec/05_KT_DL.pdf