18. - 20. 5.

2011, Brno, Czech Republic, EU

STRUCTURE AND PROPESTIES OF SUB-ZERO PROCESSED VANADIS 6

P/M LEDEBURITIC TOOL STEEL
Jana SOBOTOV a, Peter JURI a, Ji CEJP a, Petra SALABOV b, Otakar PRIKNER b
a Czech Technical University in Prague, Faculty of Mechanical Engineering,
Karlovo nm. 13, 121 35 Prague 2, Czech Republic, Jana.Sobotova@fs.cvut.cz
b Prikner - tepeln zpracovn kov, Martnkovice 279, 550 01, Czech Republic

Abstract
The P/M Vanadis 6 cold work steel was austenitized, quenched and tempered at various combinations of
processing parameters. For selected sets of specimens, also sub-zero period, made at different
temperatures and processing dwell times was inserted between quenching and tempering. The
microstructure and mechanical properties have been investigated as a function of austenitizing temperature,
parameters of sub-zero processing and tempering. As-quenched structure is composed of martensite,
retained austenite and carbides. Sub-zero processing led to the decrease of the retained austenite amount
and increase of tetragonality of the martensitic lattice. Therefore, the as-quenched hardness of sub-zero
processed samples was than that of no sub-zero processed steel. On the other side, the use of sub-zero
period results in a slight hardness decrease after tempering. Furthermore it was found that the three point
bending strength, decreased markedly with increased austenitizing temperature. The lowering of bending
strength with increasing austenitizing temperature can be considered as natural because of the austenitic
grain growth. The situation for sub-zero treated steel seems to be more complex. Bending strength for the
material processed at -90C was lower while the sub -zero processing at -196C led generally to increas e of
the bending strength.
Key words: P/M cold work steel, heat-treatment, sub-zero treatment, bend strength, microstructure
1.

INTRODUCTION

Vanadis 6 is a powder metallurgical cold work tool steel offering a combination of very high wear resistance
and good toughness. High compressive strength and very good dimensional stability during heat treatment
are also typical properties of this material. Based on these characteristics, Vanadis 6 is suitable for long
tooling of cold work materials (blanking, forming operations, knives). Demanded tool life is given by means of
heat treatment. Suitable heat treatment depends on application. For optimum wear resistance [1],
recommended regime is a hardening from a temperature of 1150C and 3x tempering at 560C, resulting in
hardness from the range 63-65 HRC. For optimum ductility is directed heat treatment with lower
temperatures (1000C, 2x 250C, resulting hardness is stated 60-62 HRC).
During the austenitizing, eutectoid and a part of secondary carbides are dissolved in the austenite and
results in high hardness of the material after heat treatment. Other part of carbides, which does not undergo
the dissolution, hinders the austenite grains coarsening and makes the steels wear resistant. Blek et al. [2]
reported that there are two types of carbides in Vanadis after austenitizing. The M7C3 carbides underwent
intensive dissolution in the austenite and they were not detected above the temperature of 1100C. On the
other side, MC carbides remained almost completely unaffected and symptoms of dissolution were found
only at the temperature of 1200C. The saturation o f the austenite with carbon, chromium and partly also
vanadium results to an increased hardness of the as-quenched material, with the maximum at the
austenitizing temperature of 1025C. Preceding publ ication [3] states that higher austenitizing temperature

18. - 20. 5. 2011, Brno, Czech Republic, EU

results in hardness increase of Vanadis 6 and lowering of three point bending strength, since increased
austenitizing temperature results in the grain coarsening.
After the quenching, Cr-V ledeburitic steels contain martensite, retained austenite and undissolved carbides.
For a more complete martensitic transformation, sub-zero treatment can be inserted between quenching and
tempering. There are not doubtless opinions on the effect of sub-zero processing on properties of ledeburitic
steels. In [1] it is reported a hardness increase of 1HRC after sub-zero treatment (-70 and -80C/1-3 ho urs).
Juri in [3] reported increasing hardness for Vanadis 6 after sub-zero treatment (-90C/4 hours) compared to
not sub-zero, but it is valid only before tempering. As-tempered hardness of sub-zero material is by 2,5 - 3,5
HRC lower than that of non-sub-zero processed. This opinion is in good agreement with [4]. Berns [5], on the
other hand, reported a significant hardness increase for the sub-zero processed X290Cr12 ledeburitic steel.
Authors [3,4] reported a decrease of three point bending with the application of sub-zero processing of
Vanadis 6. The nature of this effect is not clear yet and should by subjected to further investigations. It is well
known that the microstructure is one of the most important parameters, which determines the wear
resistance of steel. Particularly for tool steels, the content and the distance between primary and secondary
carbides are the key microstructural variables, controlling the tribological response [6]. Stratton [7] reported
for tool steels dramatically improved wear resistance by deep cold treatment (-196C for minimum of 24 h).
2.

EXPERIMENTAL

The experimental material was the PM ledeburitic steel Vanadis 6 with nominally 2,1 %C, 1,0 %Si, 0,4 %Mn,
6,8 %Cr, 1,5 %Mo, 5,4 %V and Fe as balance. The hardness of as-received material was 284 HV 10. There
were made two types of specimens. Three samples of structural investigation and hardness measurement
( 17x10 mm) and 5 samples for the three point bend testing (10x10x100 mm) which were fine ground to
surface roughness of 0,2 0,3 m were heat treatment in each set. Heat treatment was the following:
vacuum austenitizing at the temperatures from the range 1000 1075C for 30 min, nitrogen gas quenchi ng
at 5 bars pressure, sub-zero treatment at a temperature -196C/4 or 10 hours and 2x tempering at 530C per
two hours. Three point bending tests have been carried out at following parameters: the distance between
supports was 80 mm, loading in the central region and loading rate of 1 mm/min, up to the moment of the
fracture. Microstructure of the material was analysed by the light microscopy.
3.

RESULTS

It was stated recently [3] that three point bending strength stated decreased with the increasing austenitizing
temperature. This reality is connected with grain coarsening with increasing of austenitizing temperature.
The effect of sub-zero processing on three point strength depends on conditions. Figure 1 presents that the
three point strength after sub-zero treatment (-90C/4 hours) and tempering 2x530C is lower and, afte r subzero treatment (-196C/4 hours) is generally higher . Although there is a difference in the bending strength for
the given sub-zero treatment regimes, the resulting hardness for the material processed by these two
regimes is practically the same, Fig. 2. In addition, the hardness of sub-zero processed material is of about
2,5 HRC lower than that of no sub-zero processed steel. Figure 3 brings a comparison of the obtained three
point bending strength results of the material without sub-zero processing and sub-zero processed steel at
-196C for 4 and 10 hours, respectively. The hardn ess plot for the material as a function of the austenitizing
temperature and sub-zero processing done at -196C is in Fig.4. Although there is a slight difference in
bending strength for monitored times of sub-zero processing at -196C (lowering with longer soaking ti me),
the hardness practically does not depend on the time of the sub-zero processing. These results are rather
surprising, since one can expect higher hardness after sub-zero processing compared to that after no subzero treatment.

18. - 20. 5. 2011, Brno, Czech Republic, EU

Fig.1. The effect of sub-zero treatment on bending strength (tempering 2x 530C)

Fig.2. The effect of sub-zero treatment on hardness (tempering 2x 530C)

Also, the three point bending strength can be expected to be lower due to sub-zero treatment. But, the
situation can be considered to be more complex since various effects should be taken into account in the
assessment of the heat treatment response of the examined material. There are at least three phenomena
happened during the tempering. Firstly, the tempering of the martensite proceeds, which is always
connected with the hardness decrease. The transformation of the retained austenite during the cooling down
from the tempering temperature, corresponding to the temperature of the secondary hardness peak, induces

18. - 20. 5. 2011, Brno, Czech Republic, EU

the increase of hardness. The last process is the precipitation of carbides during the hold at the tempering
temperature, which also results in an increase of hardness.

Fig.3. The effect of the time of sub-zero processing on bending strength (tempering 2x 530C)

Fig.4. The effect of the time of sub-zero processing on hardness (tempering 2x 530C)
The amount of retained austenite was found to be three times lower for the sub-zero processed steel than
that of on sub-zero processed [8]. In the same literature, there was an increased tetragonality of the
martensite in sub-zero processed material established. These facts confirm that the microstructure of subzero processed Vanadis 6 steel differ from that of no sub-zero processed in many factors. In addition,
Stratton et al. assumed that a precipitation of nano-sized particles can happen during the hold at a
temperature of deep-cooling [7]. However, this effect can only hardly be verified since the diffusion at such a

18. - 20. 5. 2011, Brno, Czech Republic, EU

low temperature is practically impossible. Thus, the size of these carbides can be expected well below the
resolution of common TEMs. But, based on the results presented here [8] and the Strattons consideration, it
should be noted that the contribution of the retained austenite transformation to the final as-tempered
hardness can be expected to be much lower when the material was sub-zero processed. Regarding to the
martensite state after quenching and/or sub-zero processing, there is no doubtless interpretation of the effect
of higher martensite supersaturation (due to sub-zero period) on the as-tempered hardness. However, it is
known that the as-tempered hardness of plain carbon steels with a near eutectoid carbon content (but
slightly different) does not differ significantly. Therefore, one can also assume that the as-tempered hardness
of the Vanadis 6 steels martensite developed by the sub-zero process (with higher tetragonality) would also
not differ significantly from that generated by simple quenching. This consideration seems to be a logical
interpretation of lower as-tempered hardness of sub-zero processed Vanadis 6 steel at the current state of
knowledge.

-196C/4 hours

-196C/10 hours

Fig.5. The effect of the time of sub-zero processing -196C on microstructure Vanadis steel
(austenitizing 1000C, tempering 2x 530C).

-196C/4 hours

-196C/10 hours

Fig.6. The effect of the time of sub-zero processing -196C on microstructure Vanadis steel
(austenitizing 1075C, tempering 2x 530C).

18. - 20. 5. 2011, Brno, Czech Republic, EU

The microstructures of the material quenched from 1000C and 1075C, sub-zero processing
196C/4 or 10 hours and tempering 2x 530C are show n in Fig.5.and 6. The material consists of the matrix
and carbides. The matrix contains mainly the tempered martensite, the second phase is the retained
austenite. Some portion of the lower bainite could be also expected [3]. Carbides are very fine and uniformly
distributed in the structure. The material quenched from 1000C contains more carbides than that quenc hed
from 1075C, since the carbides, mainly the M 7C3, are dissolved in the austenite in a larger extent. This fact
is in accordance with [2]. Nevertheless, possibility of magnification of light metallography, are not enough for
investigation changes of structure after sub-zero processed Vanadis 6.
4.

CONCLUSIONS
a) Three point bending strength of the Vanadis 6 steel is generally higher for sub-zero processed
samples at -196C for 4 h than these of the materia l processed at -90C for 4 h or no sub-zero
processed. This becomes an importance with increasing austenitizing temperature.
b) Prolonging of the sub-zero period to 10 h (at -196C) does not bring any benefits with respect to t he
three point bending strength.
c) The hardness of sub-zero processed (-196C/4 and 10 hours) is of about 2,5 HRC lower than that of
o
no sub-zero processed Vanadis 6, and practically the same as that after deep cooling to -90 C/4h,
and does not depend on the sub-zero processing time.

d) The microstructure of sub-zero processed Vanadis 6 steel probably differ from that of no sub-zero
processed in many factors. Nevertheless, they can not be evaluated with the light microscopy and
more detailed checking with TEM seems to be necessary.
ACKNOWLEDGEMENTS
Authors wish to thank the Ministry of Industry and Trade of the Czech Republic for the financial support for
the solution of the Project TIP FR-TI1/003
REFERENCES
[1.]

http://www.bucorp.com/vanadis_6_c.htm

[2.]

BLEK. P., SOBOTOV, J., JURI, P. Evaulation of Structural changes in Cr-V Ledeburitic Tool Steels
Depending on Temperature Austenitization, Materials and Technology, paper accepted for publication.

[3.]

JURI, P. aj. Efect of Sub-zero Treatment on Mechanical Properties of Vanadis 6 PM Ledeburitic Tool Steel . In
Metal 2010: 19.mezinrodn konference metalurgie a materil: 18. - 20. 5. 2010. Ronov pod Radhotm , Hotel
Relax, esk republika [CD-ROM]. Ostrava: TANGER: Kvten, 2010, s.518-523. ISBN 978-80-87294-15-4.

[4.]

JURI, P., USTARI, B., LESKOVEK, V. Fracture Charakteristic of the Cr-V Ledeburitic Steel Vanadis 6,
Materials and Technology , 2010, 44, 1, pp.79 86.

[5.]

BERNS, H. Restaustenit in ledeburitischen Chromsthlen und seine Umwandlung durch Kaltumformen,

Tiefkhlen und Anlassen, HTM, 1974, 29, 4, pp.236 247.

[6.]

FONTALVO, G.A. et al. Microstructural Aspect Determining the Adhesive Wear of Tool Steels, WEAR, 2006, 260,
pp.1028 1034.

[7.]

STRATTON, P.F. Process Optimatization for Deep Cold Treatment of Tool Steels. In proceedings 1 International
Conference on Heat Treatment and Surface Engineering of Tools and Dies, Zagreb, IFHTSE, 2005, pp.11 19.

[8.]

JURI, P. Cr-V Ledeburitic Cold Work Tool Steels, Materials and Technology, paper accepted for publication.

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