Progress in Natural Science: Materials International 31 (2021) 255–263

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Progress in Natural Science: Materials International

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Original Research

Enhancement of tribological properties in siliconized graphite via

hierarchically hybrid SiC/C composite
Zilin Li a, Zhaowei Zhu a, Xianglong Yu a, Kai Li b, Zixi Wang a, *, Zezhao Zhang a, Yuming Wang a
a
State Key Laboratory of Tribology, Department of Mechanical Engineering, Tsinghua University, Beijing, 100084, Beijing, China
b
Institute of Chemical Defense, Academy of Military Sciences, Beijing, 102205, China

A R T I C L E I N F O A B S T R A C T

Keywords: This study aims to investigate tribological properties in a siliconized graphite (СГ-П-0.5) and hierarchically
Siliconized graphite hybrid SiC/C composites at the load ranging from 10-40 N under dry air/water lubrication conditions. A feasible
Coefficient of friction liquid silicon infiltration (LSI) was used to fabricate the SiC/C composites. Morphology and phase identification of
Surface microstructure
two materials were characterized and analyzed by scanning electron microscope (SEM) and energy dispersive
Feature extraction
spectrometer (EDS). An image feature extraction was used to post-process the data of wear test, further to gain the
wear properties of the samples. The results demonstrated that a lower coefficient of friction (COF) and wear rate
can be achieved in the LSI SiC composites than that in the sample of СГ-П-0.5. Both COF decreased under water-
lubricated conditions, compared with that under the dry air lubrication. The excellent tribological properties in
two materials can be due mainly to the microstructure of the СГ-П-0.5 sample, showing much more graphite and
Si dispersed on the matrix. The СГ-П-0.5 sample indicated the typical oxidative wear mechanism, whereas, the
sample of LSI SiC demonstrated the combined oxidative and fatigue wear. This finding can provide a promising
new siliconized graphite materials for ceramic rolling bearings.

1. Introduction
SiC/C composite materials are increasingly demanded in cutting-edge
industries, due to their high specific strength, high hardness, high ri-
gidity, wear and oxidation resistance, as well as low thermal expansion
coefficient. The hierarchically hybrid SiC/C composites can serve a
promising candidate for applications as rolling bearing materials,
particularly providing less slippage at high speeds. Therefore, tribolog-
ical properties of composites mainly determine the quality and accuracy
of the bearing unit during friction under the service conditions.
Most previous studies focused on the fabrication, microstructure and
mechanical properties of porous SiC ceramic materials [1–4]. In fabri-
cation, a molten/liquid silicon infiltration (MSI/LSI) method can be used
to prepare SiC ceramics. Specifically, taking the graphite or other carbon
materials as a substrate, the molten (liquid or gaseous) silicon can
naturally infiltrate into the surface and internal pores of substrate at high
temperature. This method exhibits a shorter manufacturing time, while
better performance than the high-pressure sintered SiC technique [5–9].
Xia et al. [7] pointed out that the pure porous graphite can serve as a
substrate, which can shrink the volume of whole microstructure at high
temperature. This result indicated that the addition of binder or SiC
powder can reduce the shrinkage of silicon graphite. Cornolti et al. [8]
proposed that the process of LSI was a exotherm reaction, and the tem-
perature can rise by 500
C. Skakov et al. [10] successfully produced the
silicon-infiltrated graphite using carbon black, graphite and quartz,
which greatly reduced manufacturing costs because these available nat-
ural materials are cost-saving.
In microstructure, Calderon et al. [9] studied the effect of porosity in
the carbon substrate on the degree of silicon penetration. When the
porosity exceeds 36%, the carbon substrate was completely infiltrated.
Favre et al. [6] found that the formation time of SiC was no more than 30
min, and the depth of the SiC layer was less than 10 μm in LSI method.
Roger et al. [11] used LSI method to explore the influence of temperature
and time on the infiltration process. In the first 60 s, the rapid diffusion
and infiltration of molten silicon were observed, while reaching at least
half of the maximum penetration depth. In the subsequent study, the
weight gain kinetics model was established by comparing the permeation
effect of cetane and molten silicon on porous graphite [12,13]. In all
samples, the curves exhibit the similar shapes with two successive filling
kinetics. In order to avoid blocking the passage caused by too fast reac-
tion, Song et al. [14] found the graphite as a slow release carbon source,
due to the ordered microstructure and large particle size. Padovano et al.

* Corresponding author.
E-mail address: zxwang@mail.tsinghua.edu.cn (Z. Wang).

https://doi.org/10.1016/j.pnsc.2020.12.014
Received 20 March 2020; Received in revised form 30 November 2020; Accepted 31 December 2020
Available online 28 January 2021
1002-0071/© 2021 Chinese Materials Research Society. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
Z. Li et al.
[15] used the microwave assisted the reactive melt infiltration to fabri-
cate the silicon graphite, and then investigated the effects of microwave
power variation on the microstructure and the mechanical properties.
In mechanical properties, Xiong et al. [16] performed the chemical
vapor infiltration on a solid SiC after additive manufacturing, and sub-
sequently the tensile strength after treatment increased from 3.3 MPa to
15.7–47.3 MPa. In tribological properties, SiC ceramic materials are
often used as brake discs and gaskets in friction systems, due mainly to
high coefficient of friction (COF) and low wear rate under dry conditions
[17,18]. Sun et al. [19] revealed that ceramic materials have stable
tribological properties at high temperatures. Under water-lubrication,
Tomizawa et al. [20] found that the SiC and Si3N4 composites pro-
duced tribochemical wear, and thereby hydrolyzed as SiO2 during
running-in process. As such, the wear surface can form a 70 nm thick
water film, further to greatly reduce COF. At a sliding velocity above 60
mm/s, the COF of SiC can be achieved less than 0.03 [21]. Therefore, the
SiC composite can also be used as a material for hydromechanical
bearings and seals, even as a bearing bush in water lubricated bearings.
The silicon-infiltrated graphite that prepared by Zhou et al. [22] has
shown a COF of 0.29 in a dry condition, and a COF of 0.13 in a water
lubricated condition. Xia et al. [7,23] conducted tribological properties
of siliconized graphite, indicating that the higher COF and the lower
wear rate than that of graphite. Fan et al. [13] reported that the main
wear mechanisms of siliconized graphite can be abrasive wear, oxidative
wear, fatigue wear, and adhesive wear.
Two aspects were mostly focused on previous studies: 1) The fabri-
cation methods of SiC composites using different material processes, 2)
The tribological properties of SiC composites. However, there were
various microstructure and physical properties of silicon graphite pre-
pared by different methods, and thereby bring different tribological
properties. A systematic evaluation is lacking on tribological properties
of SiC composites fabricated by different approaches, particularly on the
tribological mechanism of different surface morphology in SiC materials.
Therefore, this study highlighted the comparison of tribological proper-
ties of two different SiC composites, and subsequently an attempted was
also made to investigate the influence mechanism of its surface micro-
structure on tribological properties.
2. Materials and experimentals
2.1. Siliconized graphite
Two different sources of siliconized graphite were used in the tribo-
logical test. One was a material of the Russian designation, called
СГ-П-0.5, which was prepared by the vapor phase deposition of silicon at
1800
C–2200
C infiltrating into the substrate of porous graphite. It
consist of graphite, silicon carbide and free silicon, wherein the volume
of silicon carbide was 50%–55%, the free silicon was 20%, and the rest
was free graphite, accounting for about 30%. The СГ-П-0.5 samples in
this test were taken from the serviced water-lubricated bearings. The
main physical properties of sample СГ-П-0.5 and LSI SiC composites were
shown in Table 1.
2.2. Liquid silicon infiltration SiC
Another material was a silicon-infiltrated graphite prepared by a
liquid silicon infiltration method (LSI SiC). Fig. 1 shows the Si–C phase
diagram provided by Refs. [24,25], which gave the melting temperature
Table 1
Physical properties of sample СГ-П-0.5 and LSI SiC composite.
Sample Density g/cm3 Tensile strength MPa Compressive strength MPa
СГ-П-0.5 2.4–2.6 60 420–450
LSI SiC 2.65 50 412–441
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Fig. 1. Si–C phase diagram [25].
of Si. The procedure was following, the firing at a temperature of 1500


C, the melting point of silicon at 1414
C for 30 min in a vacuum at-
mosphere. The complete liquid silicon infiltration method can be found
in Ref. [26] in detail. The formation of carbon was filled in a silicon
powder bed in a graphite crucible with a lid in the high-temperature
furnace. In order to obtain an uniform pool of liquid silicon in the car-
bon sample, the sample in the furnace was heated with 100% output
power until the set temperature was reached.
After fabrication, surface residual silicon was washed away with the
hydrofluoric acid, and weak adhesion SiC was removed. Boron carbide
was used as an abrasive to fully grind before friction test to ensure that
the surfaces of two materials have the same roughness of Ra 0.05. Ul-
trasonic cleaning was performed using acetone after grinding.
It is note that the selection of reaction temperature was because the Si
phase can be completely in the liquid state above the temperature of
1404  5
C, as shown in the Si–C phase diagram in Fig. 1, where the Si
phase can fully react to produce SiC composites.
2.3. Tribolgical test
The tribological test was carried out under a pin-on-disc configuration
on a UMT-3 (Bruker) multi-specimen test system [27]. Specifically, a
controlled environment friction and wear meter was used for a
counter-grinding of same material under dry and water immersion con-
ditions. In each test, a cylinder with a diameter of 3 mm was placed on
the upper jig. The lower sample was directly fixed to the base in the
chamber. The material of cylinder pin was the same as the lower sample.
The operating conditions applied for each friction test were: The normal
force (FN) of 10 N and 40 N, the rotation speed of 100 rpm, the radius of
gyration was 15 mm, and the duration of 30 min in each test. All tests
were performed at room temperature in air. For each test condition, three
tests have been carried out in order to verify the reproducibility of the
results. The COF was measured and recorded during the sliding test. The
wear rate was calculated by the formula proposed by Archard et al. [14],
Vi
ki ¼ (1)
FN  s
Bending strength MPa Compressive modulus MPa Thermal conductivity
W/(m⋅K)
100–120 1.27  105 120–140
190 1.40  105 150–175
Z. Li et al.
where Vi is the wear volume. Vi ¼ M=ρ, which is the ratio of material
weight loss to density. FN is the normal load. s is the friction distance.
2.4. Analytical methodology
After tribological test, the samples were sectioned into round slices
with a diameter of 50 mm and a thickness of 5 mm, using wire electrical
discharge machining. Microstructural characterisation was studied using
a scanning electron microscope (SEM, Zeiss Gemini SEM 300) with a
energy dispersive spectrometer (EDS) detector, where operated at an
acceleration voltage of 10 kV, a working distance of 5–10 mm. X-ray
diffraction (XRD) and Raman analyses were also used to identify the
components contained in the materials.
An feature extraction technique was used to process the scanning
images captured by SEM. In this study, an Otsu thresholding algorithm
was used to extract features of images, since different gray level pre-
sented different elemental components under the backscattered-electron
diffraction (BSD) mode in an electornmicrope. Applications of image
feature extraction to the SEM images in materials science have been
shown in the qualitative [28] and quantitative [29] investigations.
Chowdari et al. [28] used qualitative algorithms, such as binarization,
Otsu threshold, connected feature labelling and erosion, while calcu-
lating the most characteristic pathological parameters. The work of
Raimundo et al. [29] showed the use of algorithms, such as turning off
morphological operators, dimorphism, and feature labels. A specific
block quaternization was selected, because multiple different areas in the
sample varied in different phases to identify, including SiC, Si, and
graphite, particularly compared with the general Otsu thresholding
method, such as block binarization. By calculating an interclass variance
between a specified grayscale and objectives, the three or four areas can
be separated. The introduced elimination algorithm can be used to
remove the noise elements. Finally, it is necessary to count the pixels
contained in each value of feature. More detailed and specific image
feature extraction procedures can be found in Ref. [30].
3. Results
3.1. Microstructure before tribology test
Fig. 2 shows the XRD pattern of the sample СГ-П-0.5 before tribology
test. In the sample, most component was SiC phase, less amount of Si and
graphite.
In the LSI SiC material, an oxidation test was performed after the
sample preparation. The polished sample was oxidzed in a high-
temperature furnace holding at 400
C for 2 h in an oxygen atmo-
sphere. Fig. 3 shows the Raman spectra of LSI SiC sample before and after
Fig. 2. XRD pattern of sample СГ-П-0.5.
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oxidation. Before the oxidation, free silicon and graphite existed on the
surface of sample, whereas, all silicon on the surface translated to silicon
dioxide after oxidation. It is note that the oxidation test aims to make sure
the performance of fabricated composites, due to the oxidation resistance
is the key property of LSI SiC surface. Furthermore, the oxide layers on
the surface of samples were removed before the friction test.
Fig. 4a–d shows the morphological characteristics of sample LSI SiC in
various states, including oxidized surface, interior microstructure
without completely infiltration, primitive microstructure, and the single
grain of matrix. In Fig. 4a–b, it can be seen that only a small number of
grains appeared in the interior, whereas, the rest was graphite in the
sample of LSI SiC composite. In Fig. 4c, the uniform cubic grains in the
average grain size of 3–30 μm densely distributed on the surface of
sample LSI SiC composite, particularly around a larger grain in Fig. 4d.
Fig. 4e–f shows the initial morphological characteristics of sample
СГ-П-0.5. In the unpolished surface, there were most open-cell micro-
structure formed on the sample. After processing, the flattening micro-
structure was obtained on the surface of scratches.
3.2. Microstructure after tribological test
Fig. 5 shows the SEM morphology and EDS mapping of samples LSI
SiC composite under a normal load of 40 N after friction test. The reason
is that the EDS technique can be use to identify different elements on the
surface of sample. In the elemental distribution of Si and C in Fig. 5, it
infers that the dark gray area can be graphite in scanned image, and the
light gray area can be a mixture component of SiC and Si. As such, a
distribution mapping can be obtained to evaluate various elements on the
surface. Furthermore, the morphology of LSI SiC composite under dry air
conditions exhibited many pits with a maximum diameter of 100 mm in
Fig. 5a, whereas, it was not found that under water immersion condi-
tions. These pits can be indicator of fretting wear, which can cause the
embedded graphite to fall off in dry conditions during the friction
process.
Fig. 6 shows the comparison of СГ-П-0.5 material before and after
tribological test, particularly on the distribution of oxygen element
before and after friction. Under dry friction, there were slight scratches
on the worn surface of sample, whereas, the surface scratches were not
obvious under water lubrication. In Fig. 6a, there was a clear boundary in
the mapping of oxygen element can be observed between the unworn and
worn surface of the sample. It infers that the oxidation and wear occurred
on the intersurface of friction paris during the tribological test.
Specifically, Table 2 lists the specific elemental volume proportion of
sample surface in the EDS mapping, particularly on the worn/unworn
areas after the tribological test. It can be found that the total amount of
elements was similar from the two materials. The difference can be that
the content of oxygen increased greatly after wear test. The degree of
oxidation in dry condition was significantly higher than that in water
lubricated condition.
3.3. Feature extraction
Post-processing of the acquired dataset was conducted using a newly
developed user-defined programme on the Matlab software package. A
feature extraction was performed on the obtained SEM-BSE images. All
the obtained SEM-BSE images were first cleaned by removing the wild
spikes of elements. Three grayscales were then defined in the SEM-BSE
images, to serve as the characteristic values of SiC, graphite and Si
phase. An Otsu thresholding was finally used to classify and regenerate
component of phases represented by each grayscale color. The high
resolution was maintained for the phase reconstruction during the data
post-processing.
Fig. 7 shows the BSD images and feature extraction for the sample
СГ-П-0.5 and LSI SiC composite. The BSD scanning image was divided
into three main color regions according to different gray levels, and
thereby the components in the sample were identified by EDS technique,
Z. Li et al. Progress in Natural Science: Materials International 31 (2021) 255–263

Fig. 3. Raman spectra of LSI SiC sample, (a) before, and (b) after, oxidation.

Fig. 4. SEM images of samples morphology before tribology test: (a) oxidized surface, (b) interior morphology without completely infiltration, (c) primitive structure,
(d) enlargement of single grain, in LSI SiC composite; (e) unpolished surface, (f) processed scratches, of СГ-П-0.5.

where the darkest region can be the graphite phase, the gray region as SiC
phase, and the white region as free Si phase. It can be found that there
was very close detection in the two materials under EDS mapping.
Nevertheless, the detection range of EDS mapping normally can repre-
sent a micron-scale depth. In contrast, the BSD image was used as the
detection method of surface topography to obtain a more precise meso-
scale information.
In addition, a great challenge in the EDS mappings can be to
distinguish SiC and Si phase. Normally, one way is to compare the same
area in the distribution map of Si and C element. SiC phase was set when
Si and C concurrently appeared at the same spot, whereas, Si phase was
set when only Si element but no C at the same spot. Nevertheless, this
approach can be difficult to discern, demanding high resolution mapping.
That is why the feature extraction from the BSD images demostrated an
obvious difference in the composition ratio of surface morphology.
Table 3 shows the volume proportion of each component on the

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Fig. 5. SEM images and EDS mapping of LSI SiC composites under, (a) dry air, and (b) water lubrication, after tribology test.
surface of sample, based on the counting of characteristic values related
to Si, SiC and graphite in the phase distribution of dataset after feature
extraction. These specific values differed from the data that observed by
EDS technique. The СГ-П-0.5 sample surface was mainly composed of
graphite, accounting for about 50%, with 40% SiC and 10% free Si phase.
The surface of LSI SiC sample mainly consist of SiC composite, indicating
a volume ratio of about 75%, about 20% of graphite, and 5% of free Si. In
contrast, the sample of LSI SiC composites contained much more SiC and
less Si phases on the sample surface.
Since the matrix of both materials were based on the graphite, Si
phase can be infiltrated into the inside microstructure, leading to the
graphite therein exhibited the shape of enclosed crystal. The sample of
СГ-П-0.5 was estimated to be much more than twice larger in the
diameter of the graphite particles in LSI SiC composite, as the difference
increased in the grain size of graphites. Generally, the graphite grains in
LSI SiC composites were in a diameter of several tens of micrometer, with
a maximum of about 100 μm. On the surface of sample СГ-П-0.5, the
grain size of graphite was much larger, with the diameter ranging from
100 to 250 μm, particularly the graphite grains were mostly connected to
each other in the matrix.
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3.4. COF and wear rate in tribological test
Fig. 8 shows the time-dependent variation of the COF for the various
samples under different normal loads during the tribological test. The
COF of СГ-П-0.5 sample was generally higher than that of LSI SiC com-
posite. In the dry condition, the COF of СГ-П-0.5 sample rised first and
then stabilize during the friction. In СГ-П-0.5 sample, the stability COF
value was 0.27 under the normal load of 10 N, whereas, the COF was
slightly higher reaching 0.3 under the normal load of 40 N. In water-
lubricated condition, the COF of СГ-П-0.5 sample decreased with the
sliding duration, and eventually stabilized at 0.13 at the normal load of
10 N, and 0.12 at the normal load of 40 N. The COF of LSI SiC composite
was relatively sensitive to the normal load during dry condition, where
the COF was 0.13 at the normal load of 10 N, and 0.16 at the normal load
of 40 N. Moreover, there was some sawtooth shape of the COF curves in
Fig. 8 b and d, where the COF suddenly rised, and then slowly returned to
the previous value. Under water lubrication, LSI SiC composite exhibited
a very low COF of 0.08 at the normal load of 10) and 0.09 at the normal
load of 40 N. These tribological data were similar to the previous report
of Zhou et al. [22], and the tribological mechanism that associated with
Z. Li et al. Progress in Natural Science: Materials International 31 (2021) 255–263

Fig. 6. Surface morphology of СГ-П-0.5 sample under a normal force of 40 N under, (a) dry air, and (b) water lubrication, after tribology test.

Table 2
Elemental proportion of surface before and after wear (vol%).
Elements СГ-П-0.5 LSI SiC

Dry air Water lubrication Dry air Water lubrication

Unwore surface Worn surface Unwore surface Worn surface Unwore surface Worn surface Unwore surface Worn surface

Si 13.48 13.16 13.62 16.74 20.32 16.33 14.69 15.27

C 82.53 78.36 82.85 76.93 77 71.02 81.61 80.13
O 3.64 8.12 2.88 6.14 2.35 12.23 3.43 4.32
Fe 1.36 0.36 0.65 0.19 0.33 0.42 0.27 0.28

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Fig. 7. BSD images and feature extraction for samples, (a) СГ-П-0.5, and (b) LSI SiC composite.

this COF evolution will be discussed in Section 4.1 in detail.

Table 3
Fig. 9 shows the wear rates under the normal load of 10 N and 40 N
Proportion of phase distribution on sample surface (vol%).
during the dry and water-lubricated conditions. It is worth noting that
Components СГ-П-0.5 LSI SiC the wear rate of СГ-П-0.5 sample decreased with the increasing load. On
SiC 40.66 74.28 the contrary, the wear rate of LSI SiC composite increased as the load
Graphite 49.45 21.46 increased. Both materials have an excellent wear resistance during the
Si 9.89 4.26
working conditions. In water-lubricated condition, the wear rate of
СГ-П-0.5 sample reduced. The wear rate of LSI SiC composite reduced

Fig. 8. COF of СГ-П-0.5 and LSI SiC composite under different normal loads, (a) СГ-П-0.5, 10 N, (b) LSI SiC, 10 N, (c) СГ-П-0.5, 40 N, (d) LSI SiC, 40 N.

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Fig. 9. Wear rate of СГ-П-0.5 and LSI SiC composite under different work-
ing conditions.
greatly, which was only 0.750  105 mm3/Nm at the normal load of 10
N under the water lubrication. This changes demonstrated that the LSI
SiC composite can have better wear resistance with a relatively lower
load capacity than that of СГ-П-0.5 sample.
4. Discussion
4.1. Tribological mechanism
The oxidative wear occurred on the surface of sample in dry condition
(in Fig. 6a), where the Si phase was oxidized to SiO2 during rubbing,
indicating that the noticeable scratches were found. This results is agree
with that wear mechanisms of the C/SiC brake materials in Ref. [31]. In
the water environment, there was no obvious wear scars that can be
found on the surface of two materials. It can infer from Table 2 that the
water can undergo a tribochemical reaction with the SiC surface. A
boundary film can formed on the surface layer during friction, leading to
the boundary lubrication [20]. It also revealed that water can also play a
key role in the heat dissipation, which can lower the temperature of
contact surface to prevent oxidation reactions. The reaction of SiC and
water was as follows [32].
SiC þ 2H2 O ¼ SiO2 þ CH4 (2)
It is note that the measurement for thickness of lubricating film can be
highly challenged in the experiment beyond this scope [20]. In this work,
it can infer that the lubrication form was boundary lubrication, because
there was no obvious scratch on the friction surface under water lubri-
cation (in Figs. 5-6), while the COF was significantly reduced (in Fig. 8).
Moreover, there were the sudden instability and rising COFs that
occurred during friction process in the LSI SiC composite (in Fig. 8b and
d), and concurrently, some pits were observed on the worn surface of the
sample (in Fig. 5a). It is note that the SiC particles were totally different
from graphite particles. This is because the hardness of SiC phase was
normally high (KH in 2960 kg/mm2), where the liquid phase sinter SiC
slightly lower than that in the solid state sintered SiC materials, while
showing high wear-resistant. Therefore, the SiC composite can translate
to the abrasive particles after falling off the worn surface of sample, and
consequently co-exist between the two interfaces for a period of time.
That is why the abrasive wear can result in the unstable change during
friction process (in Fig. 8d). The explanation can well elucidate the wear
rate of LSI SiC composite increased with the rising normal load, whereas
the СГ-П-0.5 sample had a opposite change, as shown in Fig. 9. It also
infers that the LSI SiC composite was more prone to shedding of SiC
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grains during the friction. In water-lubricated conditions, both materials
exhibited a very low COF, while the lubrication state behaved the type of
boundary lubrication. Particularly, there was no abrasive particles falling
off, while the surface of LSI SiC composite behaved a low wear rate.
4.2. Microstructure effect on friction and wear
In Fig. 7, the unpolished surface of LSI SiC composite was observed
using a enlarged in SEM image, and a distinct grain-like SiC micro-
structure was found. According to the previous study of Favre et al. [2], it
was formed into the β-SiC phase in LSI fabrication, which has the char-
acteristics of very high hardness and wear resistance of single grains. But
the cubic structure of grains can be easy to cause stress concentration
when these grains contact each other. When the surface of sample was
subjected to high stress under the different normal loads, some cracks can
easily occur among grains, and thereby causing the failure of fatigue
peeling [33]. The graphite morphology of two materials was very
different, based on the findings of feature extraction for the BSE images
(in Fig. 6). Compared with the СГ-П-0.5 sample, the surface of LSI SiC
composite contained much more SiC and less graphite. Therefore, the
graphite behaved the shape of closed particles on the surface of LSI SiC
composite. On the surface of СГ-П-0.5 sample, the number of graphite
was much more, while the grain size was much larger that on the LSI SiC
composite. Particularly, the grain size reached a diameter of 100–200
μm, while most of graphite particles were connected to each other. The
bonding force between them was much stronger than that in LSI SiC
composites.
In the LSI SiC composite, the peeling pits usually appeared on the
worn surface, while, the morphology was grainy inside the pits. More-
over, since the peeled β-SiC crystal grains had a high hardness, the
abrasive wear normally occurred during friction. That is the reason that a
sudden rise in COF occurred in Fig. 8. The finding demonstrated that the
LSI SiC composite had a higher wear rate under high loads. In the
СГ-П-0.5 sample, the SiC grains were surrounded by graphite phase in
the matrix of sample. The graphite can act as a support microstructure,
and thereby to reduce the stress concentration during the friction. That is
why there was no fatigue wear that can be observed. The wear was
derived mainly from the graphite in terms of the wear scar observation.
The low interlayer force of graphite led a good lubrication effect,
resulting in a low COF and wear rate of LSI SiC composite [34]. Because
the wear resistance of graphite was not as good as that of SiC phase, the
total wear rate of СГ-П-0.5 sample was slightly higher than that, but the
stabile performance was better than that during the friction test.
Due to the interaction between the crystal grains, the shedding of
graphite during friction was not obvious. However, the graphite on the
surface of LSI SiC composite does play a role of solid lubrication, and
consequently the COF was reduced. In the future, the LSI SiC composite
can be expected to serve a novel porous material for rolling bearings, and
even high-temperature air foil bearings [35]. The hybrid SiC/C com-
posite has also self-lubricating properties, particularly for non-lubricating
ceramic bearings. A further research direction can be to compare the
toughness and impact resistance of the hybrid SiC/C composite, and
further to find the optimal conditions of silicon graphite microstructure
for better performance.
5. Conclusion
(1) Tribological experiments and feature extraction have been carried
out on two siliconized graphite materials, СГ-П-0.5 and LSI SiC
composite. The СГ-П-0.5 sample had a COF of 0.26–0.3 under dry
friction, whereas the COF of LSI SiC composite was 0.13–0.16.
Under water-lubricated conditions, the SiC surface formed a
boundary film, and thereby the lubrication state was in a bound-
ary lubrication, with the COF of both materials droped to about
0.1.
Z. Li et al.
(2) The wear type of СГ-П-0.5 sample was mainly the oxidative wear,
together with the abrasive wear of graphite. The wear rate
decreased significantly, as the normal load increased during the
friction. The main wear type of LSI SiC composite also included
fatigue wear, which caused the SiC grains to fall off continuously.
That is why the COF suddenly increased, while the wear rate
increased with the rise of the normal load. The oxidative wear of
surface mostly derived from the oxidation reaction of free Si at
high temperature at the interface of friction pairs.
(3) The proportion of SiC phase was 75% on the surface of LSI SiC
sample. It’s easy to form the stress concentration among the SiC
grains during friction, which caused some cracks to expand, and
concurrently abrasive particles to fall off, therefore finally leading
to the presence of abrasive wear. The surface of СГ-П-0.5 sample
was dominated by graphite phase. The SiC phase was surrounded
by graphite, as a structural support for higher stability and fatigue
life.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This work was financially supported by the National Key R&D Pro-
gram of China (Grant No. 2018YFB2000100), the Aviation Science Fund
of China (Grant No. 20164058002), the Tsinghua University Initiative
Scientific Research Program and Beijing Municipal Science & Technol-
ogy Commission (Grant No. Z181100004518004), and the Science and
Technology Commission of the Central Military Commission (Grant No.
1916321TS00100501).
References
[1] Z. He, H. Li, X. Shi, Q. Fu, H. Wu, Prog. Nat. Sci. Mater. Int. 24 (2014) 247–252,
https://doi.org/10.1016/j.pnsc.2014.05.005.
[2] F. Wang, J. Yin, D. Yao, Y. Xia, K. Zuo, Y. Zeng, Prog. Nat. Sci. Mater. Int. 27 (2017)
380–384, https://doi.org/10.1016/j.pnsc.2017.04.006.
[3] Q. Qi, J. Zhang, C. Lu, Q. Zhang, Y. Xuan, M. Liu, Prog. Nat. Sci. Mater. Int. 28
(2018) 378–385, https://doi.org/10.1016/j.pnsc.2018.04.006.
[4] X. Lin, H. Gong, Y. Zhang, J. Bi, Y. Feng, Y. Liu, S. Wang, Prog. Nat. Sci. Mater. Int.
29 (2019) 184–189, https://doi.org/10.1016/j.pnsc.2019.03.009.
[5] F.H. Gern, R. Kochend€ orfer, Compos. Part A Appl. Sci. Manuf. 28 (1997) 355–364,
https://doi.org/10.1016/S1359-835X(96)00135-2.
[6] A. Favre, H. Fuzellier, J. Suptil, An original way to investigate the siliconizing of
carbon materials 29 (2003) 235–243.
[7] H. Xia, J. Wang, H. Jin, Z. Shi, G. Qiao, Mater. Sci. Eng. 528 (2010) 283–287,
https://doi.org/10.1016/j.msea.2010.08.088.
[8] L. Cornolti, S. Martinelli, G. Bianchi, A. Ortona, J. Am. Ceram. Soc. 102 (2019)
2304–2315, https://doi.org/10.1111/jace.16124.
263
Progress in Natural Science: Materials International 31 (2021) 255–263
[9] J. Narciso, F. Rodrı, The Combined Effect of Porosity and Reactivity of the Carbon
Preforms on the Properties of SiC Produced by Reactive Infiltration with Liquid Si,
vol. 7, 2009, https://doi.org/10.1016/j.carbon.2009.04.002.
[10] M.K. Skakov, S.R. Kurbanbekov, Y.T. Koyanbaev, V.V. Baklanov, A.Z. Miniyazov,
R.M. Mukhamedzhanova, Siliconized Graphite Production Technology, 2015,
pp. 215–218, https://doi.org/10.2991/cas-15.2015.51.
[11] J. Roger, G. Chollon, Ceram. Int. 45 (2019) 8690–8699, https://doi.org/10.1016/
j.ceramint.2019.01.191.
[12] J. Roger, M. Avenel, L. Lapuyade, J. Eur. Ceram. Soc. 40 (2020) 1869–1876,
https://doi.org/10.1016/j.jeurceramsoc.2019.12.050.
[13] J. Roger, M. Avenel, L. Lapuyade, J. Eur. Ceram. Soc. 40 (2020) 1859–1868,
https://doi.org/10.1016/j.jeurceramsoc.2019.12.049.
[14] S. Song, Z. Gao, B. Lu, C. Bao, B. Zheng, L. Wang, Ceram. Int. 46 (2020) 568–575,
https://doi.org/10.1016/j.ceramint.2019.09.004.
[15] E. Padovano, M. Giorcelli, G. Bianchi, S. Biamino, M. Rovere, A. Tagliaferro,
A. Ortona, J. Eur. Ceram. Soc. 39 (2019) 2232–2243, https://doi.org/10.1016/
j.jeurceramsoc.2019.01.057.
[16] H. Xiong, H. Chen, Z. Chen, X. Xiong, D. Zhang, K. Zhou, Ceram. Int. 46 (2020)
6234–6242, https://doi.org/10.1016/j.ceramint.2019.11.092.
[17] W. Krenkel, B. Heidenreich, R. Renz, Adv. Eng. Mater. 4 (2002) 427–436, https://
doi.org/10.1002/1527-2648(20020717)4:7<427::AID-ADEM427>3.0.CO;2-C.
[18] W. Krenkel, F. Berndt, Mater. Sci. Eng. 412 (2005) 177–181, https://doi.org/
10.1016/j.msea.2005.08.204.
[19] Q. Sun, J. Yang, B. Yin, H. Tan, Y. Liu, J. Liu, J. Cheng, Z. Qiao, W. Liu, J. Eur.
Ceram. Soc. 37 (2017) 4505–4513, https://doi.org/10.1016/
j.jeurceramsoc.2017.07.016.
[20] H. Tomizawa, T.E. Fischer, A S L E Trans. 30 (1987) 41–46, https://doi.org/
10.1080/05698198708981728.
[21] H.C. Wong, N. Umehara, K. Kato, Tribol. Lett. 5 (1998) 303–308, https://doi.org/
10.1023/A:1019174615499.
[22] H. Zhou, S. Dong, Y. Ding, Z. Wang, D. Wu, Tribol. Lett. 37 (2010) 337–341,
https://doi.org/10.1007/s11249-009-9523-6.
[23] H. Xia, J. Wang, Z. Shi, G. Qiao, J. Nucl. Mater. 433 (2013) 341–344, https://
doi.org/10.1016/j.jnucmat.2012.09.016.
[24] V. Haase, G. Kirschstein, H. List, S. Ruprecht, R. Sangster, F. Schr€ oder, W. T€
opper,
H. Vanecek, W. Heit, J. Schlichting, H. Katscher, The Si-C phase diagram, in:
H. Katscher, R. Sangster, F. Schr€ oder (Eds.), Si Silicon Syst. Si-C. SiC Nat. Occur.
Prep. Manuf. Chem. Spec. Forms. Manuf. Electrochem. Prop. Chem. React. Appl.
Ternary High. Syst. With Si C, Springer Berlin Heidelberg, Berlin, Heidelberg, 1985,
pp. 1–5, https://doi.org/10.1007/978-3-662-06994-3_1.
[25] R.W. Olesinski, G.J. Abbaschian, Bull. Alloy Phase Diagrams 5 (1984) 486–489,
https://doi.org/10.1007/BF02872902.
[26] J.C. Margiotta, D. Zhang, D.C. Nagle, C.E. Feeser, J. Mater. Res. 23 (2008)
1237–1248, https://doi.org/10.1557/jmr.2008.0167.
[27] X. Yu, Z. Jiang, D. Wei, C. Zhou, Q. Huang, D. Yang, Wear 302 (2013) 1286–1294,
https://doi.org/10.1016/j.wear.2013.01.015.
[28] K.S. Choudhari, P. Jidesh, N.K. Udayashankar, Synth. React. Inorg. Met. Nano-Metal
Chem. 42 (2012) 369–375, https://doi.org/10.1080/15533174.2011.611206.
[29] D.S. Raimundo, P.B. Calíope, D.R. Huanca, W.J. Salcedo, Microelectron. J. 40
(2009) 844–847, https://doi.org/10.1016/j.mejo.2008.11.024.
[30] D. Saladra, M. Kopernik, J. Microsc. 264 (2016) 102–124, https://doi.org/
10.1111/jmi.12431.
[31] S. Fan, L. Zhang, L. Cheng, J. Zhang, S. Yang, H. Liu, Tribol. Int. 44 (2011) 25–28,
https://doi.org/10.1016/j.triboint.2010.09.003.
[32] M. Chen, K. Kato, K. Adachi, Wear 250 (2001) 246–255, https://doi.org/10.1016/
S0043-1648(01)00648-2.
[33] S. Fan, C. Yang, L. He, J. Deng, L. Zhang, L. Cheng, Tribol. Int. 114 (2017) 337–348,
https://doi.org/10.1016/j.triboint.2017.04.035.
[34] S. Fan, L. Zhang, L. Cheng, S. Yang, Ceram. Int. 37 (2011) 2829–2835, https://
doi.org/10.1016/j.ceramint.2011.04.075.
[35] E. Uhlmann, C. Neumann, Air bearings based on porous ceramic composites, in:
D.T. Pham, E.E. Eldukhri, A.J.B.T.-I.P.M, S. Soroka (Eds.), Elsevier Science Ltd,
Oxford, 2006, pp. 211–216, https://doi.org/10.1016/B978-008045157-2/50041-
9.