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Tribology International 43 (2010) 22222230

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

High-temperature abrasive wear testing of potential tool materials for


thixoforming of steels
Yucel Birol n
Materials Institute, Marmara Research Center, TUBITAK, Kocaeli, Turkey

a r t i c l e in f o

a b s t r a c t

Article history:
Received 19 April 2010
Accepted 15 July 2010
Available online 23 July 2010

High temperature abrasive wear performance of Inconel 617, Stellite 6 alloys and X32CrMoV33 hot
work tool steel was investigated. The wear resistance of the latter is degraded at 750 1C due to its
inferior oxidation resistance. Extensive oxidation co-occuring with abrasive wear at 750 1C leads to
substantial material loss due to the lack of a protective oxide scale, sufciently ductile to sustain the
abrasion without extensive spalling. The wear resistance of the Inconel 617 and Stellite 6 alloys, on the
other hand, improves at 750 1C owing to protective oxides that sustain the abrasion without spalling.
& 2010 Elsevier Ltd. All rights reserved.

Keywords:
Three-body abrasion
Sliding
High temperature
Wear

1. Introduction
Steel parts for drive units and chassis components are often
manufactured by forging owing to their superior mechanical
properties since the castings fail to provide the required mechanical and fatigue properties. The rather high tooling, material and
energy costs of the conventional forging process, however, have
prompted the part manufacturers to seek alternative forming
technologies. Semi-solid forming, which combines the advantages
of casting and forging at much lower forming forces and at
competitive cost, is indeed an attractive option. Having already
matured into an industrial practice for Al and Mg alloys [1], this
innovative near-net shape forming technology could upgrade the
market and provide lightweighting for forged steel parts.
Thixoforming of steel is very demanding on tool materials with
process temperatures often exceeding 1300 1C [2,3]. The surfaceto-interior temperature gradients and the thermal stresses thus
generated across the die are much larger than with Al and Mg
[46]. The principle die failure mechanism is thus claimed to be
thermal fatigue as the mechanical loading on the tooling is
modest owing to a mushy feedstock [7]. The wear caused by the
impact of the a-Fe globular particles in the slurry and high
temperature oxidation not only impair the quality of the die
surface, but also introduce potential sites for crack nucleation
under thermal cycling. The conventional hot work tool steels were
shown to rapidly deteriorate under such severe conditions [810].
Suitable die materials with extended service life are required to
set up an appropriate process for the production of steel parts on
an industrial scale [8].

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


E-mail address: yucel.birol@mam.gov.tr

0301-679X/$ - see front matter & 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.triboint.2010.07.011

Several high temperature alloys were tested recently for their


potential to withstand the steel thixoforming environment for an
economically acceptable life [7,1114]. Shown to possess a
superior thermal fatigue performance than conventional hot
work tool steels [7,1115] these alloys are claimed to be attractive
candidates owing to their outstanding resistance also to high
temperature oxidation, erosion and wear [16]. The present work
was undertaken to investigate the high temperature abrasive
wear resistance of these materials and rate their performance
with that of the conventional hot work tool steel employed in hot
forging of steel components [17].

2. Experimental
The wear test was designed to mimic the conditions encountered in steel thixoforming where a-Fe particles of the semi-solid
feedstock move over the die cavity surface once forced into the
die. The die materials were represented by 6 mm thick square
samples (25 mm  25 mm) machined from X32CrMoV33, Inconel
617 and Stellite 6 alloys (Table 1) and ground to a surface nish of
500 grit sand paper. The wear test rig comprised of a steel pot,
150 mm  120 mm|, placed inside a resistance heating unit
(Fig. 1a and b). The steel pot was lled with zirconia sand with
an average particle size of 163 mm (Fig. 1c). The zirconia sand was
heated to the desired test temperature before the test sample was
immersed into the sand. The wear test samples were tted to a
mild steel rod attached to an electric motor assembly capable of
rotating the specimens in hot sand at 220 rpm for 6 h. Measures
were taken to maintain a trouble-free sand ow around
the samples. The present wear test is thus a three-body abrasive
wear test.

Y. Birol / Tribology International 43 (2010) 22222230

2223

Table 1
Chemical composition of the X32CrMoV33 hot work tool steel and Inconel 617 and Stellite 6 alloys used in the present work.
Alloy

Si

Mn

Cr

Mo

Ni

Al

Co

Cu

Nb

Ti

Fe

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

o 0.010
10.872
58.241

0.1651
0.304

0.0015
0.010
0.033

o0.001
0.211

0.413

0.009

0.020

4.512

92.63
2.850
2.660

motor

zirconia
sand

K-type
thermocouple
stainless
steel pot

sample
heating
elements

Fig. 1. (a) Photo and (b) sketch of the abrasive wear test set-up used in the present work. (c) Scanning electron micrograph of the zirconia sand used in abrasive wear tests.

600
before testing
after testing at 625C
after testing at 750C

hardness (HV1)

500
400
300
200
100
0
X32CrMoV33

Inconel 617

100

Stellite 6

after testing at 625C


after testing at 750C

90
80
weight loss (mg)

An assessment of the wear resistance has to take into account


the hardness of the material [18]. Hot work tool steels are known
to resist tempering and retain their hardness up to approximately
650 1C [19]. Hence, the wear tests were performed below and
above this temperature, at 625 and 750 1C, respectively, in order
to fairly describe the impact of temper resistance of the hot work
tool steel on its wear resistance. The latter is the maximum
temperature attained at the surface of the die during thixoforming of steels [20]. The temperature of the sand was maintained at
625 710 and 750710 1C throughout the wear tests. Hardness of
the samples was measured with a Vickers hardness tester with
1000 g load and a dwell time of 15 s.
Weight loss was used as the measure of wear. Electronic
balance of 0.1 mg accuracy was used to measure the weight of
specimens before and after each test. The worn surfaces were
characterized with a JEOL 6335F model eld emission gun
scanning electron microscope (FEG-SEM) tted with an Oxford
Instruments INCA model energy dispersive X-ray analyzer (EDS).
Thermo-gravimetric analysis (TGA) were performed with a
SETARAM TG/DTA unit to determine the oxidation behaviour of
the materials tested in the present work. Powder samples
pulverized via mechanical means, with an average grain size of
45 mm, placed in deep platinum pans were heated in owing
oxygen at 10 1C min 1 until 850 1C. A Shimadzu XRD-6000 model
X-ray diffractometer with Cu Ka radiation was employed for the
identication of oxides on the surfaces of the samples submitted
to high temperature wear tests.

70
60
50
40
30
20

3. Results and discussion

10
0

The hardness and weight loss of the samples submitted to high


temperature wear tests are illustrated in Fig. 2. The hardness drop
of the hot work tool steel upon a 6-h long thermal exposure at

X32CrMoV33

Inconel 617

Stellite 6

Fig. 2. (a) Hardness and (b) weight loss values of the three alloys tested at 625 and
750 1C.

2224

Y. Birol / Tribology International 43 (2010) 22222230

625 1C is negligible suggesting that 625 1C is near, yet below the


temper softening temperature of this material. Likewise, the
weight loss of the X32CrMoV33 tool steel due to abrasive wear is
the smallest at this temperature. The hardness drop of Inconel
617 alloy, on the other hand, is the largest. This substantial
softening may be responsible for the weight loss it has suffered,
measured to be the highest at this temperature. With an
intermediate hardness at 625 1C, the abrasive wear performance

of the Stellite 6 alloy falls in between. The weight loss and


hardness values are inversely proportional at 625 1C suggesting
that the wear resistance of the three alloys tested in the present
work is closely linked with their hardness.
The response to abrasive wear testing of the candidate
materials is markedly different at 750 1C. X32CrMoV33 tool steel
which has largely retained its hardness and resisted softening at
625 1C, responded to thermal exposure at 750 1C with a sharp

Fig. 3. Photos of (a) the X32CrMoV33 hot work tool steel and (b) Stellite 6 samples after abrasive wear tests at 750 1C.

10m
Element
CK
OK
Al K
Si K
VK
Cr K
Fe K
Mo L

Wt%
17.49
28.05
0.22
0.21
0.11
0.64
52.86
0.41

10m
Element
CK
OK
Al K
Si K
VK
Cr K
Fe K
Mo L

Wt%
6.47
16.81
0.29
0.42
0.37
2.50
70.42
2.33

Fig. 4. Scanning electron micrograph, EDS spectrum and EDS analysis of the corners of (a) the surface and (b) the corner of X32CrMoV33 hot work tool steel sample after
abrasive wear test at 625 1C.

Y. Birol / Tribology International 43 (2010) 22222230

hardness drop (Fig. 2a). This is not surprising since the temper
resistance of hot work tool steels is claimed to be around 650 1C
[19]. Inconel 617 alloy, on the other hand, has experienced only
slight softening with a further increase in the test temperature to
750 1C, suggesting that it has already almost fully softened at
625 1C. The Stellite 6 alloy appears to soften gradually over this
temperature range (Fig. 2a).

1mm
1mm
Element Wt%
32.84
CK
31.03
OK
0.34
Al K
0.54
Si K
0.36
VK
2.27
Cr K
28.53
Fe K
0.96
Ni K
3.12
Mo L
Fig. 5. Scanning electron micrograph, EDS spectrum and EDS analysis of a heavily
worn location at the corner of X32CrMoV33 hot work tool steel sample after
abrasive wear test at 750 1C.

10m
Element
CK
OK
Al K
Si K
VK
Cr K
Mn K
Fe K
Mo L

Wt%
2.51
19.01
0.20
0.35
0.62
4.54
0.17
67.05
4.62

2225

The weight loss of the X32CrMoV33 sample after the wear test
at 750 1C was measured to be 91 mg evidencing a marked
reduction in its wear resistance. The oxide scales, which spalled
from the surface soon after the sample cooled to room
temperature, is responsible for much of this weight loss
(Fig. 3a). The wear resistance of the Inconel 617 and Stellite 6
alloys, on the other hand, appears to have improved at 750 1C. The
weight loss of these two alloys due to abrasive wear at 750 1C is
considerably less than at 625 1C (Fig. 2b). It is also interesting to
note that the differences between the Inconel 617 and Stellite 6
alloys in terms of hardness and weight loss are almost completely
erased after the wear tests at 750 1C. The two alloys seem to have
attained similar hardness and have suffered nearly equal weight
loss after testing at 750 1C.
The abrasive wear was most prominent along the leading
edges, particularly around the bottom corners, of the samples
where the pressure head and thus the abrasion capacity of the
sand was the highest (Fig. 3b). These locations were thus rounded
off evidencing that the wear at the corners and edges is
responsible for much of the material loss incurred on the samples.
The surfaces of the samples on the other hand, hardly revealed
any wear damage as the sand particles tended to slide over the
at surfaces under the present circumstances. The specimen
geometry and the features of the wear test employed in the
present work facilitated the assessment of the relative impact of
oxidation and abrasive wear in generating material loss during
elevated temperature wear testing.
The X32CrMoV33 hot work tool steel submitted to wear test at
625 1C shows markedly different features at the surface and at the
corner. The surface is in an oxidised state while the features of the
corner are typical of three-body abrasion with multiple indentations (Fig. 4). The wear features such as craters, extrusion lips are
much ner with respect to the erodent size and instead scale with
the microstructure. The EDS analysis of the respective regions has
shown stronger oxygen peaks at the surface than at the corner,
implying that oxide at the corner has been thinned by abrasion.
The marked difference between the C levels at the surface and at
the worn corner seems to underline the impact of carbides in the
oxidation process. The EDS analysis always revealed high C levels
for those sites where O levels were also high. This is true also
for the sample corner locations where the wear damage was

10m
Element
CK
OK
Al K
Si K
VK
Cr K
Mn K
Fe K
Mo L

Wt%
7.57
37.23
0.37
0.60
0.59
5.59
0.38
43.09
4.59

Fig. 6. Scanning electron micrograph, EDS spectrum and EDS analysis of the corners of (a) the surface and (b) the corner of X32CrMoV33 hot work tool steel sample after
abrasive wear test at 750 1C.

2226

Y. Birol / Tribology International 43 (2010) 22222230

intensity (a.u)

10

20

30

40

50
60
2
(degrees)

70

80

90

100

Fig. 7. XRD pattern of X32CrMoV33 hot work tool steel sample submitted to
abrasive wear test at 750 1C: ~, a-Fe; , Fe3O4.

10m
Element
CK
OK
Al K
Si K
Cr K
Mn K
Fe K
Co K
Ni K
Mo L

Wt%
10.25
14.53
0.26
1.28
17.56
0.85
1.90
8.33
35.32
9.74

substantial (Fig. 5). Carbides appear to be involved in the


oxidation process more than the matrix phase and are thus
claimed to be more prone to oxidation at high temperatures. It is
thus inferred that the carbides oxidise more readily and are thus
removed from the surface more rapidly under abrasion.
Both the surface and the corners of the X32CrMoV33 hot work
tool steel sample submitted to wear test at 750 1C were heavily
oxidised as evidenced by the SEM micrographs (Fig. 6). The wear
features, readily identied around the corners of the X32CrMoV33
sample tested at 625 1C, were entirely concealed by oxidation
when tested at 750 1C. The oxide scale was shown by XRD analysis
to be Fe3O4 (Fig. 7) and, by much higher oxygen levels in the EDS
analysis, to be relatively thicker. This contrasts the case of wear at
625 1C where the oxide scales at the corners were thinner. This

10m
Element
CK
OK
Al K
Si K
Cr K
Mn K
Fe K
Co K
Ni K
Mo L

Wt%
13.59
8.35
0.34
0.56
16.52
0.52
2.27
10.30
41.49
6.07

Fig. 8. Scanning electron micrograph, EDS spectrum and EDS analysis of the corners of (a) the surface and (b) the corner of Inconel 617 sample after abrasive wear test
at 625 1C.

10 m
Element
CK
OK
Al K
Si K
Cr K
Mn K
Fe K
Co K
Ni K
Mo L

Wt%
10.20
24.51
0.29
1.18
19.70
0.84
1.84
7.00
28.44
6.01

10 m
Element
CK
OK
Al K
Si K
Cr K
Mn K
Fe K
Co K
Ni K
Mo L

Wt%
21.73
11.43
0.22
0.46
15.47
0.54
1.90
8.00
36.03
4.22

Fig. 9. Scanning electron micrograph, EDS spectrum and EDS analysis of the corners of (a) the surface and (b) the corner of Inconel 617 sample after abrasive wear test
at 750 1C.

Y. Birol / Tribology International 43 (2010) 22222230

2227

10 m

10 m
Element
CK
OK
Si K
Cr K
Mn K
Fe K
Co K
WM

Element
CK
OK
Si K
Cr K
Mn K
Fe K
Co K
WM

Wt%
4.83
20.39
0.86
28.23
2.22
2.53
37.57
3.38

Wt%
8.71
12.52
0.49
19.67
1.00
2.11
51.40
4.09

Fig. 10. Scanning electron micrograph, EDS spectrum and EDS analysis of the corners of (a) the surface and (b) the corner of Stellite 6 sample after abrasive wear test
at 750 1C.

1
1
2
5 m

Element
OK
Al K
Si K
Cr K
Mn K
Fe K
Co K
Ni K
Mo L

Element
OK
Al K
Si K
Cr K
Mn K
Fe K
Co K
Ni K
Mo L

Wt%
13.48
0.30
0.72
17.47
0.59
2.54
10.80
45.32
8.79
Wt%
16.73
0.47
0.91
17.34
0.23
3.06
9.96
43.39
7.91

5 m
1

Element
CK
OK
Si K
Cr K
Mn K
Fe K
Co K
Mo L
WM

Wt%
5.70
10.75
0.57
21.24
0.89
2.07
54.05
0.13
4.60

Element
CK
OK
Si K
Cr K
Mn K
Fe K
Co K
Mo L

Wt%
6.02
9.89
0.52
20.76
0.87
2.59
55.02
0.10

WM

4.24

Fig. 11. Scanning electron micrographs, EDS spectrums and EDS analysis of indicated locations corners at the corner of (a) Inconel 617 and (b) Stellite 6 sample after
abrasive wear test at 750 1C.

Y. Birol / Tribology International 43 (2010) 22222230

intensity (a.u)

2228

10

20

30

40

50
60
2
(degrees)

70

80

90

100

Fig. 12. XRD patterns of (a) Inconel 617 and (b) Stellite 6 samples submitted to
abrasive wear tests at 750 1C: &, g; D, Cr2O3.

observation conrms the synergy between wear and oxidation at


elevated temperatures. Wear, dominant at the corners, generates
fresh surfaces and promotes oxidation which in turn leads to
increased material loss under the present wear test conditions.
Once again high C levels are linked with high oxygen levels
conrming the higher tendency of carbides for oxidation.
The Inconel 617 sample which has suffered the highest
material loss at 625 1C shows at the corners features quite similar
to those observed in the hot work tool steel. Multiple indentations
over the corners imply a three-body type abrasive wear (Fig. 8).
However, there is hardly any evidence of wear damage on the at
surfaces of the sample as evidenced by the survival of the grit
paper marks introduced before the wear test. The slight
colouration of the surfaces implies oxidation as conrmed by
the EDS analysis. The oxides are too thin, however, to be identied
on cross-sections at optical microscope resolutions and to
generate Bragg reections in the XRD analysis. The EDS analysis
shows the oxides to be relatively thicker at the surface suggesting
that oxides have been abraded at the corners. Surface and corner
features of the Inconel 617 sample after the abrasive wear test at

O, wt%

20

10

Si, wt%

0
15
10
5

1 m
0
40
Cr, wt%

30
20
10

Fe, wt%

0
10
5
0

Co, wt%

15
10
5

Ni, wt%

0
40
30
20
10
0
0

Fig. 13. (a) Transverse section micrograph of the surface region of the Inconel 617 sample submitted to abrasive wear test at 750 1C and (b) line scan EDS spectrums across
the surface oxide.

Y. Birol / Tribology International 43 (2010) 22222230

2229

leading to further material loss. The two mechanisms co-occuring


at 750 1C has led to material loss possibly more than would be
produced if either process acted independently as suggested by
other researchers [25,26]. An adhesive and protective oxide scale,
sufciently ductile at 750 1C to sustain the abrasion without
extensive cracking or spalling, is clearly missing in X32CrMoV33
[27,28]. The morphology of the X32CrMoV33 wear sample is
typical of eroded oxides at 625 1C but reects the severity of the
oxidation process at 750 1C. The loss of mechanical strength with
increase in test temperature is also believed to be instrumental in
the substantial material loss suffered by the hot work tool steel.
The adhesive and protective oxides growing slowly on Inconel
617 and Stellite 6 alloys, on the other hand, has sustained the
abrasion without spalling and is claimed to be responsible for the
improved wear resistance of these alloys with increase in test
temperatures [27,28]. High-temperature alloys rely on a minimum of 20 wt% Cr to form protective Cr2O3 scales [29,30]. The
XRD analysis has shown Cr2O3 to be the predominant oxide on the
surface of both Inconel 617 and Stellite 6 samples (Fig. 12a and b).
The plasticity of the oxides, essential to sustain abrasive wear, has
been reported to be adequate for Cr2O3 at high temperatures
[23,27,28,31]. The surface oxides found by the EDS were relatively
richer with Si and with Si and Al in the case of Inconel 617 and
Stellite 6 samples, respectively, implying that Si and Al are also
involved in the development of surface oxides (Figs. 13 and 14).

750 1C are quite similar. Oxidised surfaces and indented corners


are the dominant features (Fig. 9). It is worth noting, however,
that oxidation has progressed at this higher test temperature as
inferred from the higher oxygen levels in the EDS analysis. The
oxide at the surface is, once again, thicker than at the corner,
suggesting that the oxide at the corner has been partially removed
by abrasion.
The features of the Stellite 6 samples submitted to abrasive
wear tests are very similar. The SEM micrographs and the EDS
analysis of the surface and the corners of the sample tested at
750 1C are shown in Fig. 10. The chemistry is quite uniform across
the abraded corners and is thus claimed to be independent of the
morphological features for both alloys (Fig. 11). Reduced material
loss at a higher wear test temperature, in spite of further
oxidation, is taken to imply that the oxides of the Inconel 617
and Stellite 6 alloys are protective and work against material loss,
possibly by the reducing friction coefcients [21]. This contrasts
the response to high temperature wear of the hot work tool steel
that deteriorates with increase in temperatures.
The X32CrMoV33 steel responds to abrasive wear at 625 1C via
abrasion of the oxidised surfaces. Oxidation becomes the
predominant failure mechanism in the abrasive wear test
performed at 750 1C [2224]. Synergy is generated between the
oxidation process and wear at elevated temperatures with
abrasion leading to enhanced oxidation and oxidation, in turn,

10

Si, wt%

O, wt%

10

Mn, wt%

Cr, wt%

8
20
10

6
4

Ni, wt%

1 m

Al, wt%

6
Fe, wt%

Co, wt%

30
20
10

4
2
10

5
4
W, wt%

Mo, wt%

3
2
1
0

0
0

3
m

3
m

Fig. 14. (a) Transverse section micrograph of the surface region of the Stellite 6 sample submitted to abrasive wear test at 750 1C and (b) line scan EDS spectrums across the
surface oxide.

2230

Y. Birol / Tribology International 43 (2010) 22222230

References

107
X32CrMoV33
Inconel 617
Stellite 6

weight gain (%)

106
105
104
103
102
101
100
0

100

200

300
400
500
temperature (C)

600

700

800

Fig. 15. Weight gain as a function of temperature of the three alloys used in the
present work.

Oxides of aluminium and silicon are also well established to be


highly protective for alloys intended for high temperature
applications [30]. With a Cr content only as much as 3 wt% and
with hardly any Si and Al, the hot work tool steel, on the other
hand, lacks a continuous protective oxide and cannot enjoy such
protection. The resistance to oxidation of the X32CrMoV33 tool
steel is clearly inferior with respect to the Inconel 617 and Stellite
6 alloys that behave very similarly over this temperature range
(Fig. 15).

4. Conclusions
The abrasive wear performance of the X32CrMoV33 hot work
tool steel, better than those of Inconel 617 and Stellite 6 alloys at
625 1C, is degraded at 750 1C due to its inferior oxidation
resistance. While the response of the X32CrMoV33 steel to wear
at 625 1C is abrasion dominated at 625 1C, oxidation becomes
the predominant mechanism at 750 1C. Extensive oxidation
co-occuring with abrasive wear at 750 1C leads to substantial
material loss. The wear resistance of the Inconel 617 and Stellite 6
alloys, on the other hand, improves at 750 1C.
The tribological behaviour is strongly affected by the nature,
the thickness, the adherence and the morphology of the oxide
scales [32,33]. The poor adherence and limited ductility of Fe3O4
promote the failure of the thick oxide scale on the tool steel
sample impairing its resistance to wear at elevated temperatures
[27,34]. The adhesive and highly plastic Cr2O3 lm, identied to
be the predominant oxide on the surface of both Inconel 617 and
Stellite 6 samples, on the other hand, sustains the abrasion and is
responsible for the improved wear resistance of these alloys at
750 1C as suggested in [25,29,33]. The reduced oxidation rate in
these two alloys suppresses the synergy between oxidation and
wear, thus improving the resistance to wear at 750 1C.

Acknowledgements
F. Alageyik and O. Cakr are thanked for their help in the
experiments and C. Berk for his help in SEM-EDS investigations.
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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