Wear
journal homepage: www.elsevier.com/locate/wear
State Key Laboratory for Mechanical Behavior of Materials, Xian Jiaotong University, Xian 710049, China
State Key Laboratory for Mechanical Structure Strength and Vibration, Xian Jiaotong University, Xian 710049, China
art ic l e i nf o
a b s t r a c t
Article history:
Received 25 October 2012
Received in revised form
8 March 2013
Accepted 14 March 2013
Available online 2 April 2013
The friction and wear behavior of mesocarbon microbeads-based reaction-formed SiC ceramic was
investigated. The SiC, C and Si phase contents varied in the SiC ceramics. The results indicated that when
the hard SiC phase content increased, the local contact area increased and the contact pressure
decreased, resulted in lower friction coefcient and wear rate. SiC ceramics mainly had abrasive,
adhesive and plowing wear during dry sliding. There was Fe-rich not graphite-rich MML formation on
the worn surfaces, which contributed to the reduction of the contact pressure and friction force.
Lubricant effect of C phase and adhesive wear generated by Si phase were not clearly seen. Besides, the
friction and wear behavior were also related to mechanical properties, thermal conductivity, grain size
and humidity-driven tribo-reactions.
& 2013 Elsevier B.V. All rights reserved.
Keywords:
Sliding wear
Engineering ceramics
Bearings
Wear testing
1. Introduction
SiC ceramic has a variety of benecial properties such as high
hardness and strength, excellent thermal stability corrosion resistance, high thermal conductivity and low thermal expansion
coefcient, and has been widely used for tribological applications
like bearings, cylinder liners and mechanical seals. Many investigations have assessed the effects of operating parameters (load,
sliding velocity, humidity, temperature, etc.) and/or material
microstructure and properties (grain size, volume fraction, distribution, hardness, fracture toughness, etc.) on the friction and
wear properties [16]. Based on the results, many different wear
and friction mechanisms were presented. It is generally considered
that the formation of Si(OH)4 or SiOx-rich lm was an important
factor for lowering the friction coefcient of SiC ceramic, resulted
from tribochemical reactions, which was found to be sensitive to
microstructural features (grain size, chemistry, phases, etc.), atmospheric conditions (humidity, temperature) and local contact
stresses. Dong et al. [7] pointed out that at room temperature,
under high loads and high environmental humidity, the tribological behavior was controlled by tribochemical reactions between
the SiC surface and water vapor in the environment. Guha and
Basu [8] considered that tribochemical layer had a limited contribution to the wear in liquid nitrogen. Besides, it is noticed that
mechanically mixed layer (MML) or lm, mainly decided by the
0043-1648/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.wear.2013.03.038
277
reciprocating friction and wear behavior of MCMBs-derived reaction-formed SiC submitted to dry sliding tests against bearing steel
ball under different loads, in order to determine the effects that
the microstructural features and properties can have on friction
and wear behavior, as well as to clarify the wear mechanisms.
linear speed of 0.083 m/s. The sliding time for each test was
normally 20 min. Friction coefcient was measured by an analogto-digital converter and recorded in a computer. The wear rate was
calculated by
where b, h, and l were the width, depth and length of the wear scar
respectively, in which b and h were the mean value of ve different
sites on the wear scar measured by a non-contact 3D surface
proler (VK-9700, keyence, Osaka, Japan); l is the stroke amplitude, 5 mm; L is the total sliding distance.
For each sample, a minimum of two trials were conducted to
ensure repeatability of test data. Because of a sharp deection of
friction coefcient during the running-in stage, the change tendency and values of friction coefcient given in this paper were
that after 20 min running-in stage. After the wear test, the worn
surface, longitudinal section, wear debris of samples and worn
surface of counterfaces were characterized using a scanning
electron microscope (SEM, VEGAII XMU, Tescan, Czech) coupled
with an energy dispersive spectroscopy detector (EDX, INCA,
Oxford Instrument).
2.1. Materials
Reaction-formed SiC ceramics (10RFSC, 20RFSC, 30RFSC and
40RFSC) were fabricated by inltrating molten Si into the carbon
preform derived from a mixture of MCMBs and SiC powders,
whose content ranged from10 to 40 wt%. Here SiC powder limited
the volume shrinkage of MCMBs during sintering and the porosity
of the preform can be adjusted by altering SiC powder content.
With increasing SiC powder content, the morphology of reactionformed SiC changed where the SiC and Si phase contents increased
and C phase content decreased (the estimated values were in
Table 1, the OM images can be seen in [15], SEM images after
etching can be seen in Fig. 1). Meanwhile the reaction-formed SiC
ceramics have wide range of mechanical properties, as seen in
Table 1.
bhl
L
3. Results
Dry sliding wear tests were conducted on a reciprocating ballon-at contact tribometer (LFT-1, Zhongke Kaihua, Lanzhou,
China), which moved the specimen stage back and forth under a
xed ball. The ball, bearing steel GCr15 with a diameter of 5 mm,
was positioned on top of horizontal at specimen and loaded with
normal force FN. SiC specimen was xed on the base of the
tribometer that can be actuated to vibrations with a constant
stroke and a frequency of . Prior to wear test, all the contact
surfaces were polished, cleaned in acetone in an ultrasonic cleaner
and nally dried by blowing warm air. All the tests were carried
out at room temperature with a relative humidity of 60%. The
normal loads FN were 20 N, 40 N and 60 N and a constant stroke
was 5 mm at a frequency of 500 rpm, which was equal to the
Table 1
Microstructural parameters and properties of SiC ceramic.
Sample
10RFSC
20RFSC
30RFSC
40RFSC
a
b
Density, g cm3
2.59
2.63
2.69
2.81
SiC
0
3
6
15
49
60
65
73
51
37
29
12
Open porosity, %
Hardnessb, GPa
4.18
5.28
5.14
3.90
247
311
330
359
2.6
4.4
3.8
3.4
18
20
22
30
247
239
288
319
Estimated by OM in [15].
Obtained by nanoindentation test using a TI950 Tribo indenter under maximum load 4000 N, other values were obtained from [15].
Fig. 1. SEM morphologies of polished cross-sections of (a) 20RFSC, (b) 40RFSC and (c) high magnication images of SiC phase after etching.
278
Fig. 2. Representative friction coefcient curves versus time of the SiC ceramics at different loads: (a) 10RFSC, (b) 20RFSC, (c) 30RFSC, and (d) 40RFSC.
Fig. 3. Wear rates of (a) the four SiC ceramics at 40 N and (b) 20RFSC and 40RFSC at different loads.
0.089 103 mm3/m respectively. The change tendency was similar to ceramic-based W2B5C and Si3N4C composites, which had
increasing tendency of wear rate when C content increased [17,10].
Fig. 3(b) shows the wear rates of 20RFSC and 40RFSC at different
loads. Totally, the wear rates increased with increasing applied load
for the samples. Meanwhile, it is clearly noted that the wear rate of
20RFSC was much sensitive to load than 40RFSC. When applied
load increased from 20 to 60 N, the wear rates of 20RFSC sharply
increased from 0.13 to 0.30 103 mm3/m. For 40RFSC ceramic, the
value only increased from 0.076 to 0.096 103 mm3/m. On the
basis of severity indexes and morphological observations, specic
wear rate k1 1015 m2 N1 or k3 1015 m2 N1 have been
reported as acceptable limits between mild and severe wear
regimes for ceramic materials [18], so the SiC ceramic in our work
279
(the lowest specic wear rate k was 3.8 1015 m2 N1) underwent
serious wear process during sliding.
3.2. Worn surfaces
After wear test, the samples had shiny worn surfaces except
10RFSC, seen by naked eyes. With increasing applied load, worn
tracks became wider, but limited in 11.5 mm. Further investigation on worn surface morphologies of the samples are conducted
by SEM and shown in Fig. 4. For 10RFSC, large amount of debris
covered on the surface, coupled with indentation aw, which
would result in abrasive adhesive wears. For 20RFSC, some narrow
and deep furrows can be seen on the surface. According to the
high magnication SEM micrographs, the soft phase of carbon was
Fig. 4. Micrographs of wear scars of SiC ceramics loaded at 20 N: (a) and (b) 10RFSC, (c) and (d) 20RFSC, (e) and (f) 30RFSC, (g) and (h) 40RFSC.
280
peeled off from the SiC matrix and the connecting neck of network
SiC matrix was destroyed, where large amount of debris scattered.
These morphologies indicated that serious micro-cutting happened on the contact surfaces under dry sliding procedure, which
could result in high friction coefcient and wear rate. Besides, the
light gray regions (denoted as A) and dark gray regions (denoted
as B) were investigated by EDX and the results revealed that light
gray regions mainly included C, O, Si, Cr and Fe elements, which
had contents of 8.69, 7.79, 2.34, 1.17 and 80.00 at%, respectively,
and dark gray regions mainly included C and Si elements, which
had contents of 37.83 and 62.17 at%, respectively (Fig. 5). So the
dark gray regions should be the SiC matrix. The light gray regions
should be the MML, which were the debris mainly peeled from
counterpart steel ball and subsequently transferred onto the
sample, underwent complex formation process of fragmentation,
mixing, accumulation, oxidation, and compaction, etc.
Compared to 20RFSC, the worn surface of 30RFSC became
neater and smoother, accompanying with some narrow and
shallow furrows. As seen from high magnication SEM micrograph, network SiC was remained relatively intact, having no great
damage. Besides, it is worthy noted that there had network light
gray regions of MML covered on the network SiC matrix. For
40RFSC, seldom furrows and debris were seen on the worn
surface. However, some cavities left by carbon grains pulled out
from the worn surface were seen on the wear scar. The elemental
distribution map of worn surface of 40RFSC was tested. The results
showed that the content of Fe element was very small; the main
elements were Si and C. The contents of Fe, Si and C were 0.5, 47.3
and 52.2 at%, indicating that the load of 20 N hardly had effect on
serious damage for 40RFSC. Furthermore, the worn surface morphology of 40RFSC loaded at 60 N was conducted by SEM, as
shown in Fig. 6. Besides a large amount of scattered debris,
cavities, and high density of furrows, some thin lms, which
mainly came from counterpart steel ball, were covered on the
worn surface. As seen from the wear scar morphologies, the four
SiC ceramics mainly had abrasive, adhesive and plowing wear
Fig. 5. EDX results of (a) light gray regions (denoted as A) and (b) dark gray regions (denoted as B).
281
Fig. 7. SEM of the longitudinal sections below the worn surfaces of (a) 20RFSC and (b) 40RFSC.
during dry sliding. For 40RFSC, the wear mainly were plowing and
polishing under 20 N and abrasive, adhesive and plowing at 60 N,
this was in agreement with the report to a certain extent [7].
Observation on the longitudinal sections of the two specimens
(20RFSC and 40RFSC) displayed the microstructure features of the
subsurface below the worn surface, as shown in Fig. 7. It can be
seen that partial regions had MML, having a thickness of about
75 m and consisting of ne particles, located on the top of
substrates of 20RFSC. Meanwhile some microcracks in the MML
and downward-sloping microcracks below the MML can be seen
clearly. As known, ceramic materials are generally subjected not
only to brittle fracture under high or impact loads, but also to
fatigue cracking induced mainly at grain boundaries by the high
surface temperatures and cyclic stresses generally attained under
dry sliding conditions. Under the reciprocating sliding process, the
grains beneath the MML were fractured, thereby resulting in the
formation of microcracks beneath the MML. When the microcracks propagated, connected and deected to the worn surface,
the plate-like MML was peeled out from worn surface and serious
wear happened. Under high load, the fracture and removal of the
MML increased; thereby the wear rate increased and was sensitive
to applied load. The above results were in good agreement with
the results of wear rate values.
Different from 20RFSC, the MML on the top of substrate of
40RFSC was very thin, about 1 m, and no cracks appeared. The
line EDX result revealed that the MML of 20RFSC and 40RFSC both
mainly consisted of Fe element, indicating that wear of steel
bearing ball plowed by SiC ceramic at was the main wear
evidence. Meanwhile for 40RFSC the MML with thin thickness
and no cracks formation indicated that the cyclic contact pressure
should be lower than those of 20RFSC.
3.3. Wear debris
Four different types of morphologies were observed in the
debris of samples: mixed particles with large and small size for
10RFSC, plate-like akes coupled with ne accumulated particles
282
Fig. 8. Typical SEM morphologies of the wear debris of (a) 10RFSC, (b) 20RFSC, (c) 30RFSC and (d) 40RFSC.
4. Discussion
4.1. MML formation based on microstructural observations
On the basis of the careful examination and analysis of the
worn surface, longitudinal section of the worn surface and wear
debris, it can be seen that initial surface morphology played an
important role on the friction behavior and wear resistance. In the
initial stage of sliding wear, supercial carbon grains were preferentially peeled by the asperities of the counterface and released
on the worn surface as debris due to its softness and low strength.
However, because of high hardness, the SiC particles cannot be
peeled from the surface at that moment, thus to the direct
mechanical interactions between the convex of hard SiC and
counterpart steel ball, resulting in the friction force increase.
Subsequently, under high friction force, the counterpart steel ball
was plowed and transferred onto the surface of samples. As sliding
wear continued, microcracks would be produced in the samples
and gradually propagated. Meanwhile a drop of SiC debris was
generated due to its fracture under repeated shearing stress. The
debris of C, Si, Fe and SiC were subjected to a complicated process
of fragmentation, mixing, oxidation and compacting under normal
load and frictional force to form MML.
For 10RFSC, the contents of C and SiC grains were the largest
and smallest respectively among the four samples, meanwhile the
homogeneity of phase distribution was the worst [15], which
remarkably increased the local friction and micro-cutting effect,
playing very bad effect on the formation of stable MML. Khurshudov et al. reported [19] that grain detachment from the
ceramic slider surface was the most important mechanism
controlling the life of MML. The SiC grains with relative low
content in 10RFSC were much easier to be detached out from
the body and MML was hardly built up. The detached particles
scattered as debris and the main wear was abrasive wear, resulted
in the largest wear rate. But due to the large C content, the friction
coefcient was relatively low. As the content of C grains decreased
and the homogeneity of phase distribution increased, although
some Fe-rich MML was seen covered on the surface for 20RFSC,
the main contact was still the contact between the convex of hard
SiC and the counterpart steel ball. The friction force was high and
the connecting neck of the network SiC was destroyed. Correspondingly the roughness considerably increased, resulted in high
friction coefcient and wear rate. For 30RFSC, network Fe-rich
MML was covered on the SiC grains. As for 40RFSC, the network
microstructure basically vanished, SiC was the main phase where
small contents of C and Si separately and discontinuously dispersed. At this moment the contact area increased and the contact
pressure (the load divided by the contact area) decreased, the
plowing wear was the main wear mechanism. After a few minutes
of sliding, Fe-rich thin lm formed. As seen above, there were no
graphite-rich lms or MML formation on the surfaces of the four
samples. It was considered that Fe-rich lms or MML formation on
the contact surface contributed to the increase of local contact
area, further reducing the contact pressure and friction force. As a
result, the effect of local high friction force on the friction
coefcient and wear rate became smaller when increasing SiC
powder in raw materials in SiC ceramics.
283
Fig. 9. EDX results of the wear debris of (a) 20RFSC and (b) 40RFSC.
where P was the load; KC, E and H were the fracture toughness,
elastic modulus and hardness, respectively, of the material; l1 was
the stroke length; and 3 was a material-independent constant. So
the difference in wear volume among four samples can be
explained in consideration of the differences in fracture toughness,
elastic modulus, hardness, and load. Based on the mechanical
properties of SiC ceramics (Table 1), the wear volumes were
calculated and the results are shown in Fig. 11. It is clearly seen
that the change tendency in wear volumes of the theoretical
expectation was basically the same as the experimental wear rate
(the wear volume divided by the total sliding distance, which was
constant for the four samples) in Fig. 3. The wear volume increased
linearly versus applied load and the increase was less intensive to
load with increasing SiC powder in raw materials. So the
4:33
KC3
R2
1 103 C 0 3=2 E2
284
Fig. 10. Micrographs of wear scars of steel balls loaded at 60 N against: (a) 10RFSC, (b) 20RFSC, (c) 30RFSC and (d) 40RFSC.
PV
4a1 2
Acknowledgments
The authors are grateful to the National Natural Science Foundation of China (51202181), the China Postdoctoral Science Foundation
(2012M511997), the Program for New Century Excellent Talents in
285
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