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Wear
journal homepage: www.elsevier.com/locate/wear
Faculty of Engineering, University of Wollongong, Northelds Avenue, Wollongong, NSW 2522, Australia
Electron Microscope Unit, The University of New South Wales, Sydney, NSW 2052, Australia
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 1 September 2012
Received in revised form
13 November 2012
Accepted 17 November 2012
Available online 29 November 2012
In this paper, a high temperature pin-on-disc conguration was used to simulate the contact
established between a high-speed steel (HSS) work roll and a hot strip material in hot rolling, in
which the pin represented the HSS roll and the disc represented a strip steel. The pin surfaces were
oxidised due to the heat transfer from the disc while they were in contact. This work focused on the
contact behaviour of the oxide scale in the roll bite during hot rolling while the testing temperature was
close to the rolling temperature, the Hertzian pressure was similar to the contact pressure and the
sliding speed was close to those in the roll bite. The coefcient of friction during the tests was
monitored and recorded in-situ. It was found that the evolution of the coefcient of friction could be
divided into three stages. Associated with the evolution of the coefcient of friction, the morphologies
and micro-structures on the surface of pin were characterised by means of SEM, FIB and TEM
techniques to study the tribological behaviour of oxide scale in contacts. The results indicated that
the wear mechanism of pin surface varies in different stages. At the stages I and II, the oxide scale on
the pin surface is signicantly deformed. At the stage III, which the coefcient of friction is stable, the
wear mechanism is a mixture of adhesion, abrasion and oxidation. The oxide transfer from the mild
carbon steel disc to HSS pin signicantly contributed to the scale formed on the HSS pin surface.
& 2012 Elsevier B.V. All rights reserved.
Keywords:
Oxide scale
Tribology
High-speed steel
Pin-on-disc
1. Introduction
High-speed steels (HSS) have become the most favourable material choice of manufacturing hot rolls for their excellent mechanical
performance, i.e. hardness and wear resistance, at elevated temperatures. During hot rolling process, a supercial oxide scale forms on
the work rolls due to thermal cyclic working conditions. This oxide
scale plays a major role in hot rolling because it allows the starting
and driving of metal sheet between the rolls [1,2]. Under thermomechanical working conditions this scale grows to a critical thickness
and then deteriorates and causes damage by inlaying and breaking
down on the surfaces of rolled product and tools. The wear mechanisms of the work rolls in hot rolling are well known, i.e. thermal
fatigue, abrasion, adhesion and oxidation. However, little attention
has been given to the oxidation of rolling-mill roll surface and its
effects on the tribological behaviour [3]. The tribological behaviour of
oxides is very complex. It could be abrasive and therefore detrimental,
or lubricated and form a protection against wear, either way it is
inuenced by the nature and physical properties of the oxide scales
into which it makes contact [47].
0043-1648/$ - see front matter & 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.wear.2012.11.032
pin-on-disc test rig was used to identify the role of oxide scale on
the tribological behaviour, in which the pin represented the HSS
roll and the disc represented a steel strip. This work is an attempt
to study the wear of the high-speed steel, especially concerning
the oxide evolution during contact in the roll bite of hot strip
rolling. Although the continuously sliding contact in pin-on-disc
tests is different from cyclic sliding/rolling contact of work roll on
hot strip, it can help us to gain a fundamental understanding of
the role of the oxide scale in high speed work roll wear in hot
rolling. The testing temperature was chosen close to the rolling
temperature, the Hertzian pressure was similar to the contact
pressure and the sliding speeds were close to those in the rolling
bite of hot rolled strip. The coefcient of friction was monitored
and recorded in-situ during the tribological tests. Scanning
electron microscope (SEM), focused ion beam (FIB) and transmission electron microscope (TEM) techniques were used to characterise the morphologies and micro structures of the contact
zones on the surface of the pin. The evolution of oxide on HSS pin
during the test, especially scale spallation and oxide transfer from
hot disc, and its inuence on wear mechanism at the different
stages have been investigated.
2. Experimental procedure
The pin-on-disc tests were carried out on the CETR tribometer.
This device is not a hot rolling simulator, but this laboratory
apparatus can reveal the oxidational wear mechanism involved in
hot rolling [21]. In a pin-on-disc conguration, the pin represented the HSS grade material and the disc represented a strip
steel (Fig. 1). The chemical compositions of these two materials
are listed in Tables 1 and 2, respectively. The pin is manufactured
Table 1
Chemical composition of the HSS pin material (wt%), analysed by X-ray uorescence spectroscopy.
Fe
Ni
Mn
Cr
Mo
Si
Balanced
1.96
0.78
1.26
4.85
4.47
4.00
3.40
0.99
0.028
0.034
1311
3. Results
Fig. 2 shows the evolution of temperatures of disc and pin
surface during the test. It can be seen that the temperature of the
disc remained stable at 900 1C throughout the whole test while
the pin quickly reached approximately 660 1C (less than 5 min)
after making contact with the heated disc. The pin was kept
contacting with the heated disc for 20 min for pre-oxidation
before the test started. It should be noted that this monitored
pin temperature refers to the location 2 mm vertically away from
the sliding contact zone.
Fig. 3a shows a friction coefcient curve of a typical tribological test under a normal load of 5 N and a sliding speed 0.05 m/s.
It can be seen that the friction stabilised in a very short time (less
than 300 s) from the start of the test and the friction coefcient
remained at approximately 0.260.28 for the most of the test
period. According to the friction coefcient curve, the pin-on-disc
test can be divided into three stages, as shown in Fig. 3b; (i) the
rst stage, noted Stage I, the friction coefcient decreased
Table 3
Operating conditions of the pin-on-disc test.
Normal
load
Hertzian
pressure
Sliding
speed
Disc
temperature
Testing duration
5N
650 MPa
0.05 m/s
900 1C
90 s, 150 s, and
1h
Table 2
Chemical composition of the disc material (wt%), analysed by atomic emission spectroscopy.
Fe
Mn
Si
Ni
Cr
Mo
Cu
Al
Balanced
0.215
0.015
0.79
0.34
0.029
0.006
0.020
o 0.002
0.014
o 0.003
1312
Fig. 2. Temperatures of disc and pin surface during a typical tribological test.
Fig. 4. (a) Secondary electron (SE) image of the pin wear track after the
tribological test at normal load 5 N and sliding speed 0.05 m/s for 90 s (in Stage
I), (b) TEM bright eld image of the cross section of the pin wear track, FIB was
used to prepare the cross section.
Fig. 3. (a) Evolution of friction coefcient during the pin-on-disc test with
conditions of normal load 5 N, and sliding speed 0.05 m/s; (b) three tribological
stages and two interrupted points considered in a typical pin-on-disc test.
immediately after the start of the wear test; (ii) the second stage,
noted Stage II, corresponds to an increase in the friction coefcient after the minimum value; (iii) the last stage, noted Stage III,
is the stabilisation step of the friction. To better understand the
tribological behaviour, two interrupted pin-on-disc tests, which
have been labelled in Fig. 3b, were performed to investigate the
evolution of tribological contact mechanisms during the test. The
rst interrupted test corresponds to the end of Stage I (around
90 s from the start of the test), the second interrupted test refers
to the middle of Stage II (around 150 s from the start of the test).
Fig. 4a shows the wear track of the pin surface after an
interrupted pin-on-disc test which terminated at 90 s since the
1313
Fig. 5. (a) Secondary electron (SE) image of the pin wear track after the pin-on-disc test at normal load 5 N and sliding speed 0.05 m/s for 150 s (in Stage II), (b) higher
magnied SE image of the pin wear track, the sample is titled 531, and (c) TEM bright eld image of the cross section of the pin wear track, FIB was used to prepare the
cross section.
scale spalling in some areas of the sliding contact zone on the pin
surface (Fig. 5b). In this spallation area the sub-surface of the pin
was re-oxidised because it had no protection from original oxide
scale. Fig. 5c shows the TEM bright eld image of the crosssection of the contact zone (non-spallation area) of the pin
showing a compact oxide scale of approximately 800 nm covering
the pin surface. The bonding of the oxide scale and HSS substrate
was still very good because there are no visible cracks and micropores at the interface.
Fig. 6a shows the wear track of the pin after 1 hs pin-on-disc
test (Stage III). It can be seen that the morphology of the wear
track at Stage III is different to Stage II. The contact zone of the pin
surface is covered by a discontinuous glaze oxide scale; however, the adherent non-spallation glaze oxide scale is much
thicker compared with that at Stage II. As shown in Fig. 6d, the
oxide spallation is prevalent and serious in the sliding contact
zone. The ne oxide debris can be clearly observed left inside the
contact region; and the crack propagation occurs in the contacted
oxide. As shown in Fig. 6b and c, there are clear interfaces
between the sliding contact zone and non-contact area either at
the front and tail of wear track.
Fig. 7a shows the SE and TEM bright eld images of the cross
section of wear track after 1 hs pin-on-disc test (end of Stage III).
It can be seen that the pin wear track is covered by an oxide scale
of non-uniform thickness and at the centre of the wear track, a
small piece of material has been rubbed off and cracks underneath propagated into the substrate. It is possible that this
material rubbed off is vanadium MC carbide. Fig. 7b shows the
detailed microstructure of the cross-section of the pin wear track
where glaze oxide scale is adhering to the substrate and after
the pin-on-disc test, a thick oxide has developed in the contact
1314
Fig. 6. (a) Secondary electron (SE) image of the pin wear track after the pin-on-disc test at normal load 5 N and sliding speed 0.05 m/s for 1 h (end of Stage III),
(b) morphology of the wear track front, (c) morphology of the wear track tail, and (d) spallation and wear debris at the wear track.
Fig. 7. (a) Secondary electron (SE) image of the cross-section of the pin wear track after the pin-on-disc test at normal load 5 N and sliding speed 0.05 m/s for 1 h (end of
Stage III), (b) TEM bright eld image of cross-section of the wear track, (c) higher magnied TEM bright eld image of the oxide scale at the contact frontier, and (d) higher
magnied TEM bright eld image of the oxide scale near the interface of oxide scale and the HSS matrix.
1315
Fig. 8. TEM/X-ray mapping of the cross-section pin wear track after tribological test at normal load 5 N and sliding speed 0.05 m/s for 1 h (inner part of the oxide scale and
the HSS matrix).
900 1C. The oxide scale was around 70 mm thick after the test. The
oxide scale consists of three sub-layers; the outer layer is
haematite (Fe2O3) approximately 4.7 mm, the columnar crystalline middle layer is magnetite (Fe3O4) approximately 19 mm thick,
4. Discussion
The temperature of the pin and disc were well controlled
during the pin-on-disc tests (Fig. 2). The surface temperature of
the disc was kept at 900 1C with uctuations less than 2 1C. The
surface temperature of the pin reached 660 1C in a very short time
1316
Fig. 9. (a) Secondary electron (SE) image of non-contact pin surface after the pinon-disc test at normal load 5 N and sliding speed 0.05 m/s for 150 s in Stage II,
(b) TEM bright eld image of the cross section of the non-contact zone, FIB was
used to prepare the cross section.
(less than 300 s) after being into contact with the disc due to
thermal conduction and radiation. Although the temperature of
the pin was monitored from a position located 2 mm above the
contact zone, by comparing the morphologies of pin close to the
contact zone (Figs. 9 and 10) with our previous study [2224], the
temperature of the pin in the contact zone was probably around
700 1C. During hot rolling, the temperature of strip ranges from
800 to 1200 1C, and the ash temperature of the surface of the
work rolls can reach up to 650 1C, or even up to 700 1C due to heat
generated by plastic deformation and friction [2531]. Therefore,
the pin-on-disc tests reproduced the temperatures of hot rolling
very well. The temperature of disc was well kept at 900 1C during
the tests which led a thick oxide scale forming on the surface
(around 70 mm thick after 1 h). The pin was pre-oxidised for
nearly 20 min after being in contact with the disc before the pinon-disc test began, the contact mechanism between the pin and
disc is oxide-to-oxide, which reproduces the real contact condition in the hot strip rolling.
The testing condition of the pin-on-disc test with a normal
load 5 N and sliding speed 0.05 m/s is close to the tribological
conditions in the roll bite during hot rolling. Three stages were
identied after analysing friction coefcient curve: Stage I where
the friction coefcient decreased dramatically from around 0.4
(static contact) to 0.23 (dynamic contact) in a very short time
(less than 100 s). Stage II where the friction coefcient increased
from the minimum value (0.23) to approximately 0.29 in a short
time (about 150 s); and Stage III where the friction coefcient
remained at about 0.27 for the rest of the test. Vernge et al. [4]
reported the similar phenomenon. But, Vernge dened the period
before the friction stabilised as a running-in period. In the current
work the running-in period consists of Stages I and II, and Stage III
corresponds to the friction stabilisation period.
SEM and TEM investigations (Figs. 4 and 5) showed that a thin,
compact, and smooth glaze oxide scale around 800850 nm
formed on contact zone of the pin during the running-in period of
Stages I and II. Compared to the thickness of the oxide scale
formed at the non-contact zone (approximate 1 mm) in the period
(Fig. 9), the thickness of the oxide scale remained almost
unchanged. However, the TEM cross-section observation
(Fig. 5c) shows that the glaze oxide scale in the contact zone
has been heavily compressed and deformed, resulting a very
dense microstructure. Therefore, the phenomenon of oxides
transferring from the disc to the pin surface is supposed to occur
in this stage. The glaze oxide scale consists of iron oxides (Fe2O3
and Fe3O4), (Fe, Cr)-rich oxides and some vanadium oxides (V2O5).
It has a good adhesion to the HSS matrix, as seen in Figs. 4b and
5b, and the interface between the oxide scale and HSS matrix was
very compact and free from pores and cracks. The formation of
the glaze oxide scale protects the pin from surface wear, which
can be reected from the coefcient of friction whose value in the
running-in period was lower than the rest of the pin-on-disc test.
From the beginning of Stage I, the pin began to slide from static to
dynamic, with an oxide to oxide contact conguration. The oxide
on an HSS pin was deformed and a continuous and complete
glaze oxide scale (Fig. 4a) covered the whole contact area to act
as a solid lubricant and leading to the minimum friction. However, this protection did not last long, at the Stage II running in
period the oxide scale was spalled off due to shear stress
generated by friction, oxide scale thickening, thermal impact,
and stress growth inside the oxide scale (seen in Fig. 5c). The
contact surface became rougher due to the oxide spallation, hence
the coefcient of friction quickly increased from its minimum
value. However, there was no debris or cracks on the contact
surface of the pin at this stage.
As the test proceeded, friction between the pin and the disc
stabilised (Stage III), while the wear mechanisms became complicated. Local spallation of the oxide scale kept occurring during
the rest of the test and oxide debris generated on the wear track.
On one hand, spallation of the oxide scale may cause supercial
damage and increase the rate of oxidation on the HSS pin. On the
other hand, oxide debris on the wear track may act as free third
bodies abrading the antagonistic surfaces [32]. Vanadium MC
carbides have been rubbed off the surface due to the relative
weak binding energy between them (Fig. 7a). The adhesive nonspallation oxide scale in the contact region was around 9.5 mm
thick after 1 h pin-on-disc test, whereas the oxide scale at the
non-contact zone was only 2.8 mm thick. A much thicker nonspallation oxide in the contact region is not possible only from
oxidation by the HSS pin itself. It can be deduced that oxides
transferring from the mild carbon steel disc to the pin
1317
Fig. 10. (a) Secondary electron (SE) image of pin surface morphology at the non-contact area after 1 h pin-on-disc test in Stage III, (b) TEM bright eld image of the cross
section of the non-contact area, (c) TEM/X-ray mapping of the cross section of the non-contact area.
5. Conclusions
Fig. 11. Secondary electron (SE) image of the cross-section of oxide scale formed
on the disc surface after 1 h pin-on-disc test (outside the contact zone).
1318
Acknowledgement
The authors acknowledge the nancial support from The
Australian Research Council (ARC), Australia.
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