Materials Science and Engineering A 527 (2010) 60916097

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Materials Science and Engineering A

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

Thermal fatigue testing of Stellite 6-coated hot work tool steel

Yucel Birol
Materials Institute, Marmara Research Center, TUBITAK, Kocaeli, Turkey

a r t i c l e

i n f o

Article history:
Received 19 April 2010
Accepted 8 June 2010

Keywords:
Ferrous alloy
Semisolid processing
Fatigue

a b s t r a c t
The performance of Stellite 6 coating deposited on X32CrMoV33 hot work tool steel via Plasma Transfer
Arc (PTA) process was investigated under steel thixoforming conditions. The Stellite 6 coating made a
very favorable impact on the thermal fatigue performance of the hot work tool steel. The coated hot work
tool steel survived much longer, for nearly 5000 cycles before the rst thermal fatigue crack was detected
on the coating. This marked improvement is attributed to the higher oxidation resistance of Stellite 6 alloy
and its ability to retain its mechanical strength at elevated temperatures. The Cr content of the Stellite
6 alloy facilitated the formation of stable Cr-rich oxides which sustained the thermal stresses generated
at the surface without spalling and thereby retarded crack initiation. The peak compressive and tensile
stresses acting on the coating were estimated to be 500 MPa and 170 MPa, respectively, and eventually
led to thermal fatigue cracking. Once the crack initiated, the impact of microstructural features was only
minor.
2010 Elsevier B.V. All rights reserved.

1. Introduction
Hardfacing is one of the most attractive surface engineering
methods employed to enhance the wear and corrosionoxidation
resistance of surfaces [1]. Much effort has been devoted to developing alloys for hard facing applications. A variety of Co-based
alloys are commercially available at present in powder and wire
form for hardfacing to extend the service life of industrial components in wear related applications [210]. Co-based alloys retain
their hardness and offer excellent thermal fatigue, wear and oxidation resistance at elevated temperatures [1116]. Stellite 6 is
one of the most common wear-resistant alloys for a wide range
of hardfacing applications. The wear resistance of Stellite 6 alloy
is attributed to the high hardness provided by Cr-rich M7 C3 and
M23 C6 carbides [12,17]. Cr also provides oxidation and corrosion
resistance by forming an adherent oxide lm at high temperatures
while refractory metals such as Mo and W contribute to the strength
via precipitation hardening by forming MC and M6 C carbides and
intermetallic phases such as Co3 (Mo,W).
Stellite 6 could be the very sought after solution for tooling
applications in steel thixoforming where thermal fatigue, abrasive
wear and high temperature oxidation render the conventional hot
work tool steels entirely inadequate [1822]. Stellite 6 has recently
been tested among other materials [21,2335] as monolithic die
under steel thixoforming conditions and showed encouraging
results. However, cost considerations favor coating hot work tool

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

E-mail address: yucel.birol@mam.gov.tr.
0921-5093/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2010.06.015

steels over employing high temperature alloys for tooling applications. It is thus very attractive to use Stellite 6 as hardfacing on
conventional hot work tool steels.
Among several advanced deposition techniques employed
in cladding wear resistant layers on tool materials, PlasmaTransferred Arc (PTA) process stands out owing to a higher
deposition rate and lower heat input and thus very low dilution
and distortion [16,36]. It has thus been applied extensively in the
deposition of coatings for wear and high temperature applications
[13,3739]. The present work was undertaken to investigate the
performance of Stellite 6 coating deposited on X32CrMoV33 hot
work tool steel via Plasma Transfer Arc (PTA) process under steel
thixoforming conditions.
2. Experimental procedure
Stellite 6 alloy powders from Deloro Stellite Inc. with an average
diameter of 163 m were deposited on 30 mm-thick X32CrMoV33
hot work tool steel plates by the PTA overlaying process using a
Castolin Eutronic GAP400 P.T.A. unit. The metal powders injected
from a powder feeder are melted inside the plasma arc ame and
the melted metal powders thus obtained are deposited on the
substrate. The chemical compositions of the 3 mm-thick coating
thus obtained and the tool steel substrate are listed in Table 1.
The coated X32CrMoV33 samples were subsequently austenized
at 1025 C for 30 min, quenched in circulating air and nally tempered twice at 625 C for 2 h yielding a substrate hardness of 45
HRC. The clad layer was ground to a nal thickness of 2 mm to
remove the surface imperfections. Non-destructive testing (NDT)
via radiography and eddy current testing was employed to check

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Y. Birol / Materials Science and Engineering A 527 (2010) 60916097

Table 1
Chemical composition of the X32CrMoV33 hot work tool steel and the PTA Stellite 6 coating.
Alloy

Si

Mn

Cr

Mo

Ni

Al

Co

Cu

Nb

Fe

X32CrMoV33
Stellite 6

0.281
1.089

0.190
2.682

0.200
0.634

3.005
28.803

2.788
0.608

0.221
2.259

0.025
0.066

<0.010
49.962

0.165
0.168

0.002
0.023

0.413
0.054

0.020
4.425

92.63
10.12

Fig. 1. Sketch of the experimental setup for the thermal fatigue test: (a) heating and
(b) cooling cycles.

the quality of the clad layer and its interface with the substrate. The
coated plates were nally sectioned into thermal fatigue samples,
25 mm 25 mm 20 mm in size, with the Stellite 6 coating on only
one face.
The thermal fatigue test involved cyclic heating and cooling of
the coated samples between 450 C and 750 C (Fig. 1). The former
is the temperature the dies are pre-heated to before thixoforming while the latter is the peak temperature attained at the die
cavity surface shortly after the steel slurry is forced into the die
[34]. Details of the thermal fatigue test are given elsewhere [40].
The temperatures of the samples were measured during thermal
cycling with K-type thermocouples xed at the interface between
the coating and the substrate and near the rear face. Contactless
temperature measurements right at the front face of the thermal
fatigue samples have shown that the surface temperature is in the
neighbourhood of 770 C when the thermocouple near the interface
indicates 750 C. It is thus concluded that the surface temperatures
are not much different with respect to the thermal fatigue tests
performed with monolithic Stellite 6 samples.
Coating surface was examined at a multitude of magnications using stereo, optical and a JEOL 6333 F model eld emission
scanning electron microscope (FEGSEM) tted with an Oxford
Instruments INCA model energy dispersive X-ray analyzer (EDS)
before and after the thermal fatigue tests. The hardness of the samples were measured across the section of the samples in Vickers
units with a load of 1 kg (HV1) before and during thermal cycling.
An X-ray diffractometer with Cu K radiation was employed for the
identication of phases of the Stellite 6 coatings.

Fig. 2. (a) General view of the Stellite 6 coating and (b) optical micrograph of the
micro-structure across the interface between the Stellite 6 coating and hot work
tool steel substrate.

3. Results and discussion

A general view across the section of the as-deposited coating
is shown in Fig. 2. Metallographic analysis and NDT testing of the
coated samples provided no evidence for asperities, porosities and
cracks across the Stellite 6 coating, and along the interface between
the coating and the tool steel substrate (Fig. 2a). It is thus concluded
that the PTA process employed in the present work produced sound
metallurgical bonds between the Stellite 6 coating and the tool steel
substrate. EDS analysis across the interface showed some enrichment of the Stellite 6 coating with Fe, while the Cr, Co and W
levels were slightly reduced, as typically encountered in cladding
operations (Fig. 3). Dilution results from the heating conned to
deposition area, which leads to local melting and thus allows interdiffusion of the hardfacing and substrate elements. The dilution

Fig. 3. Elemental proles across the interface between the Stellite 6 coating and hot
work tool steel substrate.

Y. Birol / Materials Science and Engineering A 527 (2010) 60916097

6093

Fig. 5. (a) SEM micrograph of the interdendritic carbides and (b) the EDS analysis
of the coarse and ne carbides marked in (a).

Fig. 4. SEM micrograph of (a) the interface between the Stellite 6 coating and hot
work tool steel substrate and (b) of the coating at 500 m from the interface.

level in the present work is judged to be acceptable considering

the dilution levels previously reported for the PTA process [41].
While a uniform ne scale solidication structure is recognized at overview magnications (Fig. 2a), several distinct zones
are identied at still higher resolutions (Figs. 2b and 4a). The tool
steel substrate, which typically consists of ne carbides dispersed
in a tempered martensitic matrix, revealed a lamellar, pearlitictype structure in the immediate vicinity of the fusion line. The
fusion line is marked by a continuous planar zone, measured to be
approximately 25 m thick. This zone appears featureless at optical
microscope resolutions (Fig. 2b). This is taken to imply that solidication at the fusion line occurs very rapidly as the heat input is
dissipated by the underlying substrate almost immediately. This
planar zone is followed by a cellular region. The Fe content in the
cellular region was found to be as high as 40 wt% suggesting substantial intermixing. The cellular region is replaced almost entirely
by a columnar dendritic structure at approximately 50 m from
the fusion line (Fig. 4b). Dendritic features are predominant in the
rest of the coating. The secondary dendrite arm spacing (SDAS) was
measured to be in the neighbourhood of 7 m. The ne structure
across the coating conrms the rapid solidication process involved
in the deposition process [42,43]. The average as-deposited hardness was measured to be 460 13 HV. Both the hardness and the
SDAS values are in good agreement with those reported for PTA
coatings [37,44].
The rst phase to form in the Stellite 6 coating during cooling
from the liquid state is the primary Co-rich dendrites. The remain-

ing liquid eventually solidies by a eutectic reaction into a lamellar

mixture of Co-rich phase and Cr-rich carbides. This solidication
sequence produces a Co-rich solid solution dendritic matrix with
hard eutectic carbides at interdendritic sites [43,45,46] (Fig. 5). The
EDS analysis has shown the eutectic carbides to be rich in Cr and Co.
The majority of the coarser carbide particles were found to generally conform to the M7 C3 stoichiometry while the smaller carbide
particles inside the dendrites are likely to be of the M23 C6 variety.
Likewise, XRD analysis has shown the coating to be mainly composed of M7 C3 carbides with an orthorhombic crystal structure,
M23 C6 type carbides with an f.c.c. crystal structure (M = Co, Cr, W,
Fe, Ni, Si) and Co-rich matrix phase with an f.c.c. crystal structure
(Fig. 6). The f.c.c. structure of the Co-based matrix of the hard facing, instead of the h.c.p. crystal structure of the monolithic alloy
[47] is believed to be due to the Fe enrichment in the coating due
to dilution effect of the deposition process. Fe is known to promote
the stability of the f.c.c. structure of the Co-rich matrix [13].

Fig. 6. XRD spectrum of the Stellite 6 coating before the thermal fatigue test.

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Y. Birol / Materials Science and Engineering A 527 (2010) 60916097

Fig. 8. Change in thermal stresses generated at the front face with time during
thermal cycling of the Stellite 6-coated hot work tool steel sample.

Fig. 7. (a) Change in temperature at the front and rear faces of the Stellite 6-coated
sample during thermal cycling and (b) change in temperature difference between
the front and rear faces.

Typical thermal cycles recorded near the front and rear faces
of the coated hot work tool steel are illustrated in Fig. 7a. The
maximum and minimum temperatures at the rear face of the Stellite 6-coated hot work tool steel sample were measured to be
580 C and 486 C, respectively, while the front face went through
the set peak temperatures, 750 C and 450 C, every 30 s. This relatively smaller amplitude of the thermal cycle at the rear face,
which is displaced to the right due to an apparent delay in both
heating and cooling of the rear face, produces a temperature gap
across the section of the coated sample which becomes as large
as 205 C, 25 s into the cycle (Fig. 7b). This temperature interval
sets up thermal stresses at the front face which were shown to

be substantial for monolithic Stellite 6 under steel thixoforming

conditions [40].
The thermal stresses generated inside the Stellite 6 coating can
be estimated from,  surface
= (T)E(T)(T) [48] where and E
are the thermal expansion coefcient and the Youngs modulus of
the Stellite 6 coating, respectively and T is the temperature gap
between the front and rear faces of the sample given in Fig. 7b. Dilution of the coating with Fe is ignored and the E and values of the
Stellite 6 alloy were used in the estimation of the thermal stresses
(Fig. 8). Compressive stresses are produced in the coating when it
is warmer than the substrate and tensile stresses dominate when
the coating cools below the substrate. The peak compressive and
tensile stresses acting on the coating are estimated to be 500 MPa
and 170 MPa, respectively. While these stresses are safely below
the room temperature yield strength of the Stellite 6 alloy [49],
they could be seriously degrading, leading to coating failure when
applied in a cyclic fashion. Besides, the yield strength of the Stellite 6 coating at the thixoforming temperature range is expected
to be relatively lower in spite of the fact that Stellite 6 alloy is
known to be capable of retaining its mechanical strength at elevated
temperatures [50].
The response to thermal cycling of the Stellite 6 coating is shown
with a series of macrographs in Fig. 9. The Stellite 6 coating retained
its integrity for several thousand thermal cycles with no evidence
of heat checking or blistering often encountered in thin hard coatings [51]. Slight colouring was noted after 1000 cycles particularly
at the focal point of the ame, i.e. at the centre of the front face,
where heat accumulation is maximum. The colour and contrast
changes observed on the coating with increasing number of thermal cycles are best accounted for by the progress of oxidation
in Cr-bearing alloys [52]. The surface oxidation did not progress,
however, to a point where the oxides scales could no longer survive on the surface and thus start to spall off. This is exactly
what happened in the X32CrMoV33 steel samples, the oxides

Fig. 9. General view of the front face of Stellite 6-coated hot work tool steel samples in the course of thermal cycling.

Y. Birol / Materials Science and Engineering A 527 (2010) 60916097

6095

Fig. 10. (a, b) Oxide scale and thermal fatigue cracks at the front face of the Stellite 6-coated hot work tool steel sample after 5000 thermal cycles. Front face of the sample
after (c) metallographic polishing and (d) chemical etching.

of which were already too thick after only a thousand thermal

cycles [40].
The rst crack was detected on the coating surface after 5000
thermal cycles. Since the samples were checked thoroughly under
the microscope every 500 cycles and only visually during thermal
cycling in between, the crack might have initiated several hundred
cycles earlier. The crack was located at the very centre of the front
face where surface oxides are probably the thickest (Fig. 10a and b).
In fact, several cracks of various sizes were identied once the front
coated face of the thermal fatigue test sample was polished using
standard metallographic procedures to remove the surface oxides
(Fig. 10c). The crack opening at the surface is relatively larger than
the scale of the dendritic microstructure, i.e. SDAS (Fig. 10d) and
is thus judged to be a serious threat to the integrity of the coating.
It is inferred from Fig. 10b that oxidation has been instrumental in
crack initiation. Surface scales induce considerable damage at the
surface owing to a thermal expansion mismatch, particularly when
they spall off from the surface. The latter was shown to introduce
crack nucleation sites in hot work tool steels [40].
The crack was found to traverse almost the entire coating
(Fig. 11a). Propagation occurred perpendicular to the surface, i.e.
to the axis of maximum stress, suggesting that the impact of
microstructural features was only minor. SEM micrographs suggest
that crack propagation is not interdendritic. Nevertheless, crack
growth involved the fracture of interdendritic carbides when the
crack was traversing the dendrite boundaries (Fig. 11b). M7 C3 carbides, shown to be present in the high-Cr Stellite coatings transform
into M23 C6 carbides when exposed to high temperatures [5,5355].
This process is promoted under cyclic loading leading to a high volume fraction of M23 C6 carbides [56]. M23 C6 carbides are more voluminous than M7 C3 carbides and promote cracking at interdendritic

Fig. 11. SEM micrograph showing the crack on vertical section of the sample (a, b).

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Y. Birol / Materials Science and Engineering A 527 (2010) 60916097

its thermal fatigue performance. The coated hot work tool steel
survived steel thixoforming conditions much longer, for nearly
5000 cycles before the rst thermal fatigue crack was detected on
the coating. This marked improvement is attributed to the higher
oxidation resistance of Stellite 6 alloy and its ability to retain its
mechanical strength at elevated temperatures. The Cr content of
the Stellite 6 alloy facilitated the formation of stable Cr-rich oxides
which sustained the thermal stresses generated at the surface without spalling owing to their plasticity and thereby retarded crack
initiation. The peak compressive and tensile stresses acting on the
coating were estimated to be 500 MPa and 170 MPa, respectively,
and eventually led to thermal fatigue cracking. Once the crack initiated, the impact of microstructural features was only minor.
Acknowledgements
Fig. 12. Change in hardness across the interface between the Stellite 6 coating and
the hot work tool steel substrate with increasing number of thermal fatigue cycles.

sites [57]. The crack morphology in Fig. 11 suggests that such local
fractures indeed occurred and get connected to the growing crack.
The hardness measurements across the section of the Stellite 6coated tool steel samples at various stages of the thermal fatigue
test are shown in Fig. 12. Hardness measurements were performed
starting from the surface of the coating until the hardness level
of the substrate tool steel measured before the thermal fatigue test
was obtained. One can see that the hardness of the Stellite 6 coating
was more or less retained during the thermal fatigue test. The hardness of the tool steel substrate, on the other hand, decreased with
increasing depth from the surface after the rst 500 thermal cycles
producing a hard coating on a relatively soft substrate. The tool
steel substrate softened further opening the hardness gap across
the interface with increasing number of thermal cycles (Fig. 12). A
hard coating on a relatively soft substrate is not a desirable combination and is known to be a serious risk for the integrity of the
coating. While this is not as critical for overlay coatings as for PVD
coatings where the substrate support is essential for the integrity
of the coating, it could nevertheless present problems. The increasingly softer substrate inevitably responds to thermal stresses by
increasingly larger strains. This, in turn, would put an additional
tensile stress component on the coating due to the mismatch in
the magnitude of the respective plastic strains. This could be much
more substantial than the thermal strains produced by the thermal
expansion mismatch.
It is fair to conclude from the foregoing that the thermal fatigue
performance of the Stellite 6-coated hot work tool steel is much
better with respect to the uncoated hot work tool steel and also
compares very favourably to the monolithic Stellite 6 alloy. This
performance of the coated sample can be attributed to a number of factors. The higher oxidation resistance of Stellite 6 alloy, is
indeed very helpful [13,16,40,5860]. With a Cr content well above
20 wt%, oxide lms formed on the Stellite 6 coatings during thermal cycling are expected to be Cr-rich (Cr,Co,Fe)2 O3 type oxides
[61,62]. Oxides of this type are well established to be slowly growing, stable oxides and act as a protective layer in highly corrosive
environments [52]. They can sustain the thermal stresses generated
at the surface without spalling owing to their plasticity and thereby
retard crack initiation [63,64]. The stable hardness of the coating is
partly responsible for the superior thermal fatigue resistance of the
Stellite 6-coated hot work tool steel.
4. Conclusion
Stellite 6 coating deposited on X32CrMoV33 hot work tool steel
via Plasma Transfer Arc process made a very favorable impact on

F. Alageyik and O. Cakr are thanked for their help in the experiments and KOBATEK for coating tool steel samples. This work was
funded by TUBITAK.
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