Materials Science and Engineering A 527 (2010) 19381945

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Materials Science and Engineering A

journal homepage: www.elsevier.com/locate/msea

Thermal fatigue testing of Inconel 617 and Stellite 6 alloys as potential tooling
materials for thixoforming of steels
Yucel Birol
Materials Institute, Marmara Research Center, TUBITAK, Gebze, 41470 Kocaeli, Turkey

a r t i c l e

i n f o

Article history:
Received 8 September 2009
Received in revised form 9 November 2009
Accepted 9 November 2009

Keywords:
Steels
Thixoforming
Tooling
Thermal fatigue

a b s t r a c t
The principle failure mechanism in thixoforming dies is thermal fatigue as the mechanical loading on the
tooling is modest owing to a mushy feedstock. Samples of X32CrMoV33 steel, Inconel 617 and Stellite
6 alloys were submitted to thermal cycling under conditions which approximate thixoforming of steels.
The thermal fatigue test of the X32CrMoV33 hot work tool steel was terminated after 1500 cycles due
to severe surface degradation and temper softening, both leading to a relatively poor thermal fatigue
resistance, in spite of favorable thermo-physical properties. The response to thermal cycling of the Niand Co-based superalloys, Inconel 617 and Stellite 6, under steel thixoforming conditions, on the other
hand, was encouraging. The Inconel 617 and Stellite 6 samples are much more resistant to oxidation and
temper softening than the hot work tool steel, providing a superior resistance to thermal fatigue cracking
with few and relatively shallow cracks after as many as 5000 thermal cycles.
2009 Elsevier B.V. All rights reserved.

1. Introduction
Semisolid processing of aluminium and magnesium alloys is
already a well established manufacturing route for the production of intricate, thin-walled parts with mechanical properties as
good as forged grades [1]. In spite of its potential to upgrade the
market and provide lightweighting for forged steel parts, this nearnet shape forming process has not enjoyed commercialization for
high melting point alloys due to a lack of suitable high temperature
die materials [2,3]. Cyclic thermal loading on tools is substantial
when thixoforming steels and confers very specic requirements
on tool materials [47]. Thixoforming tools ought to last thousands
of forming cycles for industrial application to be attractive.
The principle failure mechanism in thixoforming dies is claimed
to be thermal fatigue as the mechanical loading on the tooling
is modest owing to a mushy feedstock [8]. The thermal fatigue
behaviour of hot work tool steels has been investigated extensively
[918] in an attempt to improve their performance in a number of
high temperature applications such as aluminium die casting. With
process temperatures above 1250 C [46], the surface-to-interior
temperature differentials in steel thixoforming dies are much larger
than with Al [19]. While very affordable, the conventional hot
work tool steels proved to be entirely inadequate [2,7,2022]. Suitable replacements for hot work tool steels, able to withstand the
steel thixoforming environment for an economically acceptable life

Tel.: +90 262 6773084; fax: +90 262 6412309.

E-mail address: yucel.birol@mam.gov.tr.
0921-5093/$ see front matter 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2009.11.021

have been investigated in recent years [8,21,2334]. Superalloys

which are generally employed for high temperature applications
are among potential candidates. Among wear-resistant alloys, a Cobased alloy, Stellite 6, retains its hardness and resists oxidation and
offers an excellent resistance to thermal shock, wear and corrosion
over a wide temperature range [35]. Inconel 617, a Ni-based superalloy, was reported to exhibit superior thermal fatigue resistance in
demanding tooling applications [36]. The present work was undertaken to explore the potential of Inconel 617 and Stellite 6 alloys
and to compare its performance with that of X32CrMoV33 steel
widely used in the manufacture of conventional forging dies [37].
2. Experimental
The tool steel was supplied as-cast by a major steel company while the Inconel 617 and Stellite 6 alloys were cast
in the laboratory. Their chemical compositions are given in
Table 1. X32CrMoV33 samples were machined from the as-received
block and were subsequently austenitized at 1025 C for 30 min,
quenched in circulating air and nally tempered twice at 625 C
for 2 h yielding a hardness of 45 HRC. The Inconel 617 samples
were solution annealed at 1175 C while Stellite 6 alloy samples
were stress relieved at 900 C for 4 h and slowly cooled to room
temperature.
The thermal fatigue test involved cyclic heating and cooling
of prismatic samples (25 mm 25 mm 20 mm) machined from
X32CrMoV33 hot work tool steel, Inconel 617 and Stellite 6 alloys
between the peak die cavity surface temperature and the temperature the die was pre-heated to before the forming operation.

Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

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Table 1
Chemical composition of the X32CrMoV33 hot work tool steel and Ni- and Co-based high temperature alloys used in the present work.
Alloy

Si

Mn

Cr

Mo

Ni

Al

Co

Cu

Nb

X32CrMoV33
Inconel 617
Stellite 6

0.281
0.080
1.089

0.190
0.945
1.099

0.200
0.513
1.154

3.005
21.88
28.272

2.788
8.177
0.004

0.221
53.861
2.802

0.025
0.167
0.094

<0.010
10.872
58.241

0.1651 0.0015
0.304 0.010

0.033

Ti

<0.001 0.413
0.211

0.009

Fe

0.020

4.512

92.63
2.850
2.660

Fig. 1. (a) Experimental set up for die cavity surface temperature measurements. (b) Thermocouple locations in the thixoforming die.

Fig. 2. (a and b) Photos and (c and d) sketches of the experimental set up for the thermal fatigue test; (a and c) heating and (b and d) cooling cycles.

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Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

Table 2
Thermo-physical properties and Youngs modulus values of the tested materials as a function of temperature.
T ( C) Conductivity (W/m K)

25
50
100
200
300
400
500
600
700
800
a

Cp (J/g K)

(m/m K)

Youngs modulus (GPa)

X32CrMoV33 Inconel 617 Stellite 6 X32CrMoV33 Inconel 617 Stellite 6 X32CrMoV33 Inconel 617 Stellite 6

X32CrMoV33 Inconel 617

Stellite 6

16.282
18.068
21.463
21.582
22.238
21.768
21.227
22.727
29.239
46.998a

7.18927

10.36247
11.91377
12.40772
12.81201
13.25921
13.53733
13.58018
13.95789

9.11893

11.50619
12.87849
13.48845
13.98874
14.51137
14.98786
15.46937
16.44683

9.246
9.901
11.579
13.269
14.872
16.555
18.706
24.155
27.18
22.646

11.403
12.525
14.039
15.775
17.197
18.694
19.684
22.692
27.666
29.803

0.3083
0.3814
0.3906
0.4194
0.4382
0.4741
0.5702
0.9289
1.8805a

0.4023
0.47767
0.49697
0.51288
0.53265
0.56354
0.68715
0.70851
0.75081

0.40935
0.46406
0.47435
0.4797
0.49211
0.496
0.54291
0.63111
0.68442

214.952

209.8534
202.4068
194.2192
185.2906
175.6209
165.2102
154.0585
142.1657

209.6828

206.5015
201.4563
195.493
188.6115
180.812
172.0943
162.4584
151.9045

207.7282

204.5025
199.4289
193.4723
186.6327
178.9099
170.3042
160.8154
150.4435

8.66638

11.14522
12.48774
13.0512
13.56039
14.14658
14.70218
15.23533
16.22454

Measured at 750 C.

These two temperatures are potentially the highest and the lowest temperatures encountered during the thixoforming operation,
respectively, and thus give the steepest temperature gradient
across the die. While the die was pre-heated to 450 C, considering
the usual industrial practice, the maximum temperature attained
at the surface of the die cavity was measured during thixoforming
experiments (Fig. 1). Slugs, sectioned from a commercial hot rolled
X210CrW12 bar, were held isothermally at 1290 C and the slurry
thus obtained was pressed into dies manufactured from a conventional hot work tool steel and Inconel 617 alloy pre-heated to 450 C
before the forming operation [33]. The temperatures across the section of the die were measured during thixoforming with K-type
thermocouples xed into 3 mm diameter holes (Fig. 1b).
The controlled parameter during thermal cycling was the temperature of the front face of the sample, heated by an oxyasetilen
ame to the maximum die cavity surface temperature within about
30 s (Fig. 2). Cooling was performed by forced air, adjusted so as to
bring the surface temperature to around 450 C, during the next
30 s. The temperatures at the front and at the rear faces of the samples (will be referred to as surfaces A and B, respectively in the
rest of the paper) were measured during thermal cycling with Ktype thermocouples xed into 3 mm diameter holes 0.1 mm from
respective surfaces. Thermal fatigue damage was assessed qualitatively using stereo and optical microscopy.
The hardness of the samples were measured in Vickers units
with a load of 1 kg (HV1) before and during thermal cycling. The
thermal expansion coefcients of the potential die materials were
determined with a Netzsch 402 PC unit in air at a scanning rate
of 10 C/min. Netzsch 409 PC Lux instrument was used for the
measurement of the specic heat capacities, Cp, under a nitrogen
gas ow at 40 ml/min at a heating rate of 10 C/min. A Netzsch
LFA457 instrument was used for thermal conductivity measurements under nitrogen gas owing at 100 ml/min at a heating rate
of 5 C/min.

forming experiments (Fig. 4). The maximum die cavity surface

temperatures were in the neighbourhood of 750 C for both hot
work tool steel and Inconel 617 dies. This is believed to be due
to the fact that the thermo-physical properties of the three materials tested in the present work are not much different below
700 C, i.e. at temperatures which dominate much of the forming
cycle.
The change in temperatures of surfaces A and B with time during thermal cycling is illustrated in Fig. 5a. The temperature vs time
proles for the three materials show typically similar features. Surface A continuously warms up to the maximum temperature during
the heating step and starts to cool as soon as the sample is elevated
to the cooling position, while surface B is still warming up as it
has to accommodate the incoming heat. After about 1520 s, the
temperatures of the two surfaces are equalized when surface A is
cooling in contrast to surface B which is still warming up. The latter also starts to cool soon after. Both surfaces keep cooling during
the rest of the cycle, with surface B temperature running higher
this time than surface A. It takes only a few seconds for surface A

3. Results and discussion

Thermo-physical properties of die materials have a big impact
on the temperature gradients across the die, which in turn, dictate the magnitude of thermal stresses. High heat capacity and
heat conductivity help to extract heat from the work piece, avoid
high surface temperatures and thereby reduce thermal gradients and extend the service life of the tooling [23]. Of the three
materials tested in the present work, hot work tool steel offers
higher heat capacity and thermal conductivity near the thixoforming temperature range and thus appears to be the material of
choice based on thermo-physical properties alone (Fig. 3, Table 2).
However, the favorable specic heat capacity and thermal conductivity values of the hot work tool steel are hardly reected
by the die cavity surface temperatures measured during thixo-

Fig. 3. Change in (a) heat conductivity and (b) specic heat capacity of X32CrMoV33
steel, Inconel 617 and Stellite 6 alloys with temperature.

Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

1941

Fig. 4. Change in die cavity surface temperatures with time during thixoforming
cycle of (a) X32CrMoV33 steel and (b) Inconel 617 alloy.

Fig. 6. Change in (a) Youngs modulus and (b) thermal expansion coefcients of
X32CrMoV33 steel, Inconel 617 and Stellite 6 alloys with temperature.

to become warmer than surface B once the next heating cycle is

underway.
It is indeed the temperature gradient across the section of the
sample which is responsible for thermal strains. The largest temperature gap occurs between surfaces A and B in the present test
conguration. The change in the temperature gap during a single
thermal cycle is shown in Fig. 5b. Surface A is colder than surface
B for the initial several seconds of the thermal cycle but becomes
warmer than surface B during the next approximately 30 s. The surface wants to expand but is kept from doing so by the more massive
bulk and is inevitably put under compression when it is warmer

Fig. 5. (a) Change in temperature at surface A and B and (b) change in temperature
difference between surface A and B of X32CrMoV33 steel, Inconel 617 and Stellite 6
alloy samples during thermal cycling.

Fig. 7. Change in thermal stresses generated at surface A with time during thermal
cycling of X32CrMoV33 steel, Inconel 617 and Stellite 6 alloy samples.

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Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

Fig. 8. Features of the front face, surface A, of (a) X32CrMoV33 steel, (b) Inconel 617 and (c) Stellite 6 alloy samples in the course of thermal cycling.

Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

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Since the mechanical loading on the tooling is modest owing to

a mushy feedstock [8], we can write for thixoforming,

Fig. 9. (a) Oxide scale at surface A of X32CrMoV33 steel and thermal fatigue cracks
after 1500 cycles on sections: (b) at 0.5 mm and (c) at 1 mm from surface A.

than the rest of the sample, i.e. during much of the heating step.
The state of compression at surface A prevails during cooling until
surface A and B temperatures equalize. The strain distribution is
reversed once again during the rest of the cycle when surface A is
colder than surface B. The increasingly colder surface wants to contract in this range but is restricted by the more massive, warmer
bulk and is put under tension.
The magnitude of stresses generated at the die cavity surface,
surface A, during thixoforming can be estimated from,
surface = mechanical + thermal

(1)

thermal  mechanical

(2)

surface
= thermal = (T ) E(T ) (T )

(3)

where and E are the thermal expansion coefcient and Youngs

modulus, respectively, both expressed as a function of temperature
[38]. It is evident from Eq. (3) that thermal expansion coefcient
is a key property of potential die materials. The change in and E
with temperature for the three alloys tested in the present work are
shown in Fig. 6 and are listed in Table 2. The X32CrMoV33 tool steel
appears to be at an advantage with a lower expansion coefcient in
the entire temperature range. This is essentially why the maximum
compressive and tensile stresses that develop at the surface during
thermal cycling are smaller for the hot work tool steel than for the
Inconel 617 and Stellite 6 alloys (Fig. 7).
Evidently, compressive stresses dominate at the surface for
much of the thermal cycle. These compressive stresses are as high
as 550 MPa for the Inconel 617 alloy near the end of the heating step
when surface A is much warmer than the bulk. High compressive
stresses are thus to be expected when the thixotropic feedstock
is forged into the die. The maximum compressive stresses generated at the die cavity surface, surface A, of Stellite 6 alloy and the
X32CrMoV33 tool steel are relatively lower, estimated to be 479
and 424 MPa, respectively. Tensile stresses dominate, on the other
hand, near the end of the cooling step, once the surface cools below
the bulk and during the start of the next heating step before the
temperatures of surface A and B equalize. This is when the forming operation is over and the thixoformed part is ejected from the
die. The tensile stresses thus generated are 109, 165 and 258 MPa
for the X32CrMoV33 tool steel, Inconel 617 and Stellite 6 alloys,
respectively. These stresses are much smaller than the compressive stresses that develop at surface A and fall well below the yield
strength of the respective alloys.
The front face, surface A, of the samples submitted to thermal cycling are shown in Fig. 8. The thermal fatigue test of the
X32CrMoV33 hot work tool steel was terminated after 1500 cycles
due to severe surface degradation (Fig. 8a). Thermal cycling under
the present conditions has produced rather thick oxide scales at
the surface of the X32CrMoV33 hot work tool steel (Fig. 9a) which
eventually started to spall off with continued thermal cycling, due
to a thermal expansion mismatch (Fig. 8a). Deep, branched thermal
fatigue cracks were noted once the oxide scales were removed from
the surface of the sample (Fig. 9b and c). These cracks were almost
always decorated with thick oxide layers even after substantial surface stock was removed by grinding and survived at sections 1 mm
from surface A. The thick oxides on crack surfaces are believed to
have exerted a wedging effect which helped to open the cracks
wide and thus encouraged their growth. The relatively poor fatigue
crack resistance of the X32CrMoV33 hot work tool steel could thus
be accounted for, at least in part, by its inferior oxidation resistance.
The poor resistance of the X32CrMoV33 hot work tool steel to
oxidation at high temperatures is believed to impact its response
to thermal fatigue in the temperature range of interest from steel
thixoforming point of view. Samples submitted to oxidation tests
performed at 750 C were coated with a thick Fe3 O4 scale [39].
Fe3 O4 has failed to sustain the thermal stresses generated at the
surface and started to spall from the surface after only 500 cycles.
The damage thus generated at the surface (Fig. 8) is believed to be
instrumental in crack initiation. Unlike the high temperature alloys
which rely on a minimum Cr content of 20 wt% to develop a continuous protective Cr2 O3 lm [40,41], the hot work tool steel cannot
take advantage of such protection with a Cr content only as much
as 3 wt%.

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Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

Fig. 11. Weight gain as a function of temperature of the three alloys used in the
present work.

protection was reported to be good at high temperatures [43,44].

The Cr content of the two alloys, above 20 wt%, facilitated the formation of a continuous Cr2 O3 lm during thermal fatigue providing
adequate protection, much like it does in high temperature alloys
[40,41]. Oxides of aluminium and silicon are also well established
to be highly protective for alloys intended for high temperature
applications [41]. Further evidence for the above account is available in the TGA tests (Fig. 11). The resistance to oxidation of the

Fig. 10. (a) Change in hardness of X32CrMoV33 hot work tool steel, Inconel 617
and Stellite 6 samples with increasing number of thermal fatigue cycles and (b)
with depth from surface A of X32CrMoV33 steel samples before and after thermal
cycling.

However, the underlying issue with the conventional hot work

tool steel was the substantial drop in hardness upon thermal cycling
(Fig. 10a). Hardness of surface A, which was 442 HV before the thermal fatigue test, dropped to approximately 275 HV after only 400
cycles. It is inferred from the hardness prole across the section
of the thermal fatigue sample that a surface layer 10 mm deep has
been adversely affected by thermal exposure (Fig. 10b). This is not
at all surprising considering the temper resistance of the present
hot work tool steel, reported to deteriorate above 650 C [42] and
the temperatures surface A must withstand during thermal cycling
getting as high as 750 C. The temper resistance of the X32CrMoV33
hot work tool steel is apparently not sufcient to sustain the temperatures thixoforming dies experience during forming operations.
This nding of the present work is in full agreement with earlier
results on various hot work tool steels [2022]. It is fair to conclude
from the foregoing that temper softening and severe oxidation both
hurt the thermal fatigue resistance of the conventional hot work
tool steels.
The response to thermal cycling of the Ni- and Co-based superalloys, Inconel 617 and Stellite 6, under steel thixoforming conditions,
on the other hand, was an encouraging one. Aside from a slight
colouring, there was hardly any oxidation on the front face of
the Inconel 617 and Stellite 6 samples (Fig. 8b and c) suggesting
that they are much more resistant to oxidation than the hot work
tool steel. The oxides formed on Inconel 617 and Stellite 6 alloy
samples submitted to oxidation tests performed at 750 C were
identied to be predominantly chromium oxide, with Al2 O3 and
SiO2 [39]. These slowly growing adhesive oxides are believed to
have sustained the thermal stresses generated at the surface without spalling. The plasticity of the chromium oxide, essential for

Fig. 12. (a) Thermal fatigue cracks on sections parallel to surface A of Inconel 617
and (b) Stellite 6 after 5000 cycles. The section seen is at 0.2 mm from surface A and
is obtained by sand paper grinding.

Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

X32CrMoV33 tool steel is clearly inferior with respect to the Inconel

617 and Stellite 6 alloys which behave very similarly over this temperature range. The adhesive oxides are claimed to contribute to
the superior thermal fatigue performance of these alloys.
Softening upon thermal cycling was noted also in these alloys
(Fig. 10). The average hardness of surface A, 306 HV before the test,
dropped to 268 HV after 1500 cycles and remained more or less constant for the rest of thermal cycling in Inconel 617. Likewise, the
hardness of the Stellite 6 sample, measured to be 430 HV before
thermal cycling, more or less equal to that in the X32CrMoV33
hot work tool steel, dropped to 337 HV after the rst 1500 cycles.
The extent of temper softening is apparently much less in the
superalloys even after over three times as many thermal fatigue
cycles. Besides, the heat-affected surface zones are relatively thinner. However, the most notewhorty feature of the Inconel 617
and Stellite 6 alloys is their superior resistance to thermal fatigue
cracking. The Inconel 617 sample has suffered very few, relatively
shallow cracks after as many as 5000 thermal cycles (Fig. 12a).
While the thermal fatigue cracks were more frequent in the Stellite 6 sample, they were smaller and more shallow with respect to
those in the Inconel 617 sample (Fig. 12b). These cracks were readily removed after light grinding of the surface. One would expect
the Stellite 6 alloy to perform considerably better than the Inconel
617 alloy owing to a higher hardness during thermal cycling and an
oxidation resistance just as good. Higher tensile stresses generated
at the front face of the Stellite 6 sample during thermal cycling could
be responsible for the frequent thermal fatigue cracks observed in
this sample.
4. Conclusions
Samples of X32CrMoV33 steel, Inconel 617 and Stellite 6 alloys
were submitted to thermal cycling under conditions which approximate thixoforming of steels, i.e. between 750 10 and 450 10 C,
every 60 2 s for a total of 5000 cycles. The thermal fatigue test of
the X32CrMoV33 steel had to be terminated, however, after 1500
cycles due to severe surface degradation and temper softening,
both leading to a relatively poor thermal fatigue resistance, in spite
of favorable thermo-physical properties. The response to thermal
cycling of Inconel 617 and Stellite 6 alloys, under steel thixoforming conditions, on the other hand, was encouraging. The Inconel
617 and Stellite 6 samples were found to be much more resistant
to oxidation and temper softening than the hot work tool steel, providing a superior resistance to thermal fatigue cracking with few
and relatively shallow cracks after as many as 5000 thermal cycles.
It is concluded that the Inconel 617 and Stellite 6 alloys are potential
tooling materials for thixoforming of steels with a superior resistance to high temperature oxidation as well as to thermal fatigue
cracking.
Acknowledgements
F. Alageyik and O. Cakr are thanked for their help in the experiments. This work was funded by TUBITAK and the facilites used in
thixoforming experiments were procured via a grant by the State
Planing Organization of Turkey.
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