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Wear 264 (2008) 599605

Effect of carbon fibers surface treatment on tribological

performance of polyurethane (PU) composite coating
Zhao-Zhu Zhang a, , Hao-Jie Song a,b , Xue-Hu Men a , Zhuang-Zhu Luo a
a State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences,
Lanzhou 730000, PR China
b Graduate School, Chinese Academy of Sciences, Beijing 100039, PR China

Received 17 August 2006; received in revised form 17 March 2007; accepted 1 May 2007
Available online 11 June 2007

Abstract
The carbon fibers (CF) were pre-treated in two different ways: no pre-treatment, and activation in HNO3 plus application of toluene-2,4-
diisocyanate (TDI). Carbon fibers have been introduced into polyurethane (PU) composite coatings. The tribological behaviors of the polyurethane
composite coating filled with CF or TDI-modified CF (TDI-CF) were studied using a ring-on-block wear tester under dry sliding, and the worn
surfaces of the filled PU coatings and transfer films formed on the surface of the counterpart ring sliding against the PU coating were investigated by
SEM and optical microscope (OM), respectively. Owing to the effective improvement of the interfacial adhesion between the CF and polyurethane
matrix, compared with the cases of untreated CF, the employment of low content TDI-CF provided the PU coating with much higher tribological
performance enhancement efficiency. The investigations of the frictional surfaces showed that low content TDI-CF was able to enhance the adhesion
of the transfer films of the PU coating to the surface of counterpart ring, so they significantly reduced the wear of the PU coating.
2007 Elsevier B.V. All rights reserved.

Keywords: Polyurethane coating; Carbon fibers; TDI; Tribological performance

1. Introduction
Carbon fibers combine exceptional mechanical proper-
ties and low weight, making them ideal reinforcements for
polymer matrix composite materials [1,2]. The performance
of these composites depends largely on the quality of the
matrixreinforcement interface, which determines the way loads
can be transferred from the polymer to the fiber [3,4]. How-
ever, carbon fibers usually perform a poor bonding behavior to
polymer matrix due to their nature of smoothness and chemical
inertness. This limits their applications. Therefore, a signifi-
cant amount of scientific work has been done over the years to
improve the surface activity of carbon fibers. Li et al. [5] reported
that the impregnating performance of CF was also improved
after Co60 -ray irradiation and the interlaminar shear strength
of CF/epoxy composites was enhanced by about 37%. Park et al.
[6] reported that ozone treatment was attributed to the increase
Corresponding author. Tel.: +86 931 4968098; fax: +86 931 4968098.
E-mail address: shj6922@163.com (Z.-Z. Zhang).
of both the acidic functional groups and the degree of adhesion
at interfaces between the fibers and polymeric resin in com-
posites. Zhang and Zhang [7] studied that under an appropriate
air oxidative condition, the wear resistance of carbon fiber rein-
forced epoxy was significantly improved at low contact pressure,
whereas that was reduced at high pressures. Miyoshi et al. [8]
asserted that a friction material containing 140 wt.% of acti-
vated carbon fiber bonded by synthetic thermosetting resin had
high friction coefficient and superior heat resistance.
Polyurethane coating have excellent gloss, hardness, flexi-
bility, chemical resistance and ultraviolet durability. Because
polyurethane coatings offer so many advantages, they are the
market leader for coating various substrates in the follow-
ing end-use market: automotive refinish, aircraft and chemical
agent resistant coatings [9]. However, in general, polyurethane
materials have poor abrasive wear resistance [1011]. To fur-
ther improve the mechanical and tribological performance of
polyurethane-based friction material, one of the most efficient
methods is to add various kinds of nanofillers or fibers into
the matrix as reinforcement. In our previous works, we studied
the influence of nano-SiC and nano-ZrO2 -filled polyurethane

0043-1648/$ see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.wear.2007.05.003
600 Z.-Z. Zhang et al. / Wear 264 (2008) 599605
composite coatings on friction and wear and declared that
an optimum range for nanofillers in polyurethane matrix was
5 wt.% according to the improved specific wear rate [12]. How-
ever, there is little reported work examining the friction and wear
behaviors of the untreated and TDI-treated CF-filled PU coating.
With the aim of improving the dispersion of carbon fibers and
the interfacial adhesion between the carbon fibers and the matrix
polyurethane, we design a scheme in which carbon fibers first
react with TDI. This work is believed to be conductive to the
understanding of the effect of CF or TDI-CF on the tribological
properties of the PU composite coating.
2. Experiments
2.1. Materials
In our work, steel 45 (12.7 mm 12.7 mm 19 mm) was
used as substrate of the composite coatings. An AISI-C-52100
ring of 49.2 mm in diameter and 12 mm in thickness (Hardness
Hv850) was made of bearing steel. The chemical compositions
of steel 45 are shown in Table 1.
Single-component polyurethane (PU) was provided by Xin-
Hua resin company of Shanghai, the ash content and the
isocyanate content (NCO) were 50 and 58 wt.%, respectively.
Polyfluo wax (PFW) (density 1.17 g/cm3 ) which is copolymer of
CF2 CF2 and CH2 CH2 in a diameter of approximately 34 m
were prepared by Mircopowder Company of USA. The mixed
acetone/xylene/cyclohexanone in a volume fraction of 4:2:1 was
employed in the present work as a solvent.
2.2. Surface treatment of carbon bers
Toluene-2,4-diisocyanate (TDI) was provided by China
Medicine Shanghai Chemical Reagent Corporation. The carbon
Table 1
The chemical compositions of the steel 45 (in wt.%)
C Si Mn
Steel 45 0.420.5 0.170.37 0.500.80
Fig. 1. The FTIR spectra of CF COOH and TDI-CF.
fibers (CF) with an average primary particle size of 10 m were
purchased from Shanghai Sxcarbon Technology Co. Ltd., China.
Dibutyltin dilaurate was supplied by Tianjin No. 1 Chemical
Reagent Factory, China.
In a typical experiment, carbon fibers (4 g) were added to
60% HNO3 aqueous solution (70 ml). The mixture was treated
with an ultrasonic both for 30 min and stirred for 5 h at reflux.
Then the mixture was vacuum-filtered through 0.2-m Millipote
PVDF membrane and washed with distilled water until the pH
of the filtrate was 7.0. The filtered solid was dried under vacuum
for 24 h at 60 C, obtaining CF COOH.
The typical grafting of CF proceeded as follows. A 150 ml
round-bottomed flask was charged with 2.0 g of the CF COOH,
50 ml benzene, 20 ml TDI and 23 drops dibutyltin dilaurate.
The mixture was stirred at 80 C for 4 h under a slow stream
of N2 . The solid was separated by filtration through a 0.2-m
Millipote PVDF membrane, thoroughly washed with benzene
and dried at 60 C for 24 h under vacuum to obtain TDI-CF.
2.3. FTIR analysis of TDI-CF
Fig. 1 shows the FTIR spectra of CF COOH and TDI-CF.
The FTIR spectrum of the acid-treated CF shows the presence of
many groups on the surface of the acid-treated CF, for example,
carbonyl groups reveals at about 1730 cm1 , oxygenhydrogen
bonds at about 3414 cm1 , respectively. After modification with
TDI, the characteristic peaks of the TDI are observed at about
3373, 2924, 2886, 2278, 1562 and 1480 cm1 , respectively. The
two new peaks at 3373 and 2278 cm1 are attributed to NH
and OCN stretching mode, respectively. In addition, the new
peaks observed at 1562 and 1480 cm1 should be attributed to
benzenoid unit of TDI. Together with the FTIR results, it was
concluded that the surface of CF was coated with TDI through
covalent bond and physical attraction. After CF were treated
P S Cr Ni Cu Fe
0.035 0.035 0.25 0.25 0.25 Balance
 Z.-Z. Zhang et al. / Wear 264 (2008) 599605
with HNO3 , the hydroxy groups and carboxylic groups were
introduced on the surface of CF. So, these functional groups are
very beneficial to anchor TDI molecule on the surface of CF
through the covalent bond between the hydroxy groups of CF
and OCN groups of TDI. The complete scheme for the CF
surface modification can be illustrated:
2.4. Coating preparation
The manufacture process of the composite coating was as fol-
lows: the powders of PFW were dispersed in the mixed solvent
with ultrasonic stirring for 5 min. The quantity of the solid lubri-
cant of PFW used was 30% of the binder of PU mass. In order to
have an even dispersion of CF or TDI-CF in PU binder, both the
PU binder and the CF fillers with desired proportion were care-
fully mixed by mechanical stirring and ultrasonication before
the lubricant additive (PFW) was added. The surface of steel 45
substrates was rinsed with acetone and roughened by spraying
corundum. The coatings on blocks were prepared by spraying
the prepared mixture with 0.2 MPa nitrogen gas using spray gun.
All the samples were cured in a container with relative humidity
of 5060% and temperature of 25 C. After solvent evaporation,
a thin film was obtained on the substrate. The thickness of the
wet coatings was controlled by regulating the spraying speed
and the composition of nonvolatile constituents in the coating
precursors. The thickness of the cured coatings were measured
with a MINITEST 1100 microprocessor coating thickness gauge
which works on the principle that the attractive force between a
coating and a magnetic metal was inversely proportional to the
distance between them. The thickness of the cured coatings was
5060 m.
2.5. Characterization of coating
Fig. 2 shows the SEM pictures of the PU coating filled with
3 wt.% TDI-CF surfaces and cross-section. TDI-CF are seen
to be well bonded with the coating matrix, and gaps are not
apparent at the filler/matrix interface. Additionally, we find that
there are not cavities in the coating matrix. This attributes to
good adhesion between the CF and the PU matrix.
2.6. Evaluation of the tribological behavior of the PU
coating
An MHK-500 ring-on-block wear tester (made by the Jinan
Testing Machine Factory, China) with a similar configuration
Fig. 2. The SEM photograph of the PU coating filled with 3 wt.% TDI-CF.
601
Fig. 3. Contact diagram for the frictional couple.
to a Timken tester was used to evaluate the friction and wear
behavior of the bonded solid lubricant coatings. The contact
diagram of the frictional couple is shown in Fig. 3. A steel ring
was rotated against the PU coatings filled with CF or TDI-CF at
a speed of 1.283.84 m/s and a load of 320820 N. The sliding
time of 60 min was used in all friction tests. Before each test,
the steel ring was abraded with 900 grade water proof abrasive
paper. Then the steel ring was cleaned with acetone followed
by drying. The sliding distance was calculated from the prod-
uct of the sliding speed and the sliding time. The wear life of
the coatings was calculated after dividing the sliding distance
by the corresponding coating thickness in micrometers. All the
friction and wear tests were carried out at 2025 C and a relative
humidity of 4060%.
3. Results and discussion
3.1. Friction and wear behaviors of PU composite coatings
The steady-state friction coefficient and the wear life of the
unfilled and filled PU coatings under 320 N at a speed of 3.84 m/s
are shown in Table 2. It can be seen that CF and TDI-CF can
reduce the friction coefficient of the composite coating/stainless
steel ring sliding pairs and enhance the wear life of the PU
coating to various extents. Compared with the unfilled and the
CF-filled PU coating, the TDI-CF-filled PU coating holds the
lowest friction coefficient and the highest wear life under high
speed and low applied load conditions.
The effect of content of TDI-CF on the friction coefficient
and the wear life of the PU coating sliding against the steel ring
is shown in Fig. 4 under dry friction. It can be seen that the
friction coefficient of the unfilled PU coating is quite high. The
Table 2
The friction coefficient and the wear life of PU composite coating under dry
sliding (320 N, 3.84 m/s, 60 min)
Composite coating Friction coefficient Wear life (m/m)
PU + 30% PFW 0.121 296
PU + 30% PFW + 3% CF 0.109 1782
PU + 30% PFW + 3% TDI-CF 0.096 2388
602 Z.-Z. Zhang et al. / Wear 264 (2008) 599605
Fig. 4. Friction coefficient and wear life of TDI-CF-filled PU coating as a
function of filler content (320 N, 2.56 m/s, 60 min).
situation changes greatly when TDI-CF are incorporated. It is
seen that there is a significant reduction in the values of friction
coefficient at filler content as low as 1.0 wt.%. With a rise in the
concentration of the TDI-CF, the declining trend becomes gentle
and is replaced by a slight increase from 5.0 to 10 wt.%. This
reason is that carbon fibers are composed of many laminated
graphite planes, which endows it with self-lubricating charac-
teristics [8]. However, it is also found that the wear life of the
unfilled PU coating is adversely affected by the filling of TDI-CF.
The PU coating filled with the lower content (below 6.0 wt.%) of
TDI-CF exhibits an increased wear life in comparison with the
unfilled PU coating. For TDI-CF content between 0 and 3 wt.%,
the wear life obviously increases with content of TDI-CF going
up. Above 3 wt.%, the wear life linearly decreases with increas-
ing TDI-CF content. For best combination of friction coefficient
and wear life, the optimal content of TDI-CF in the PU coating
appears to be 3 wt.%. This proportion is chosen to investigate
the effects of sliding speed and applied load on the friction and
wear behaviors of the PU coating filled with CF or TDI-CF.
Variations of the friction coefficient and the wear life with
applied load for the PU coating filled with 3 wt.% CF or TDI-CF
at 2.56 m/s are shown in Fig. 5. It can be seen that the fric-
tion coefficient of CF or TDI-CF-filled PU coating decreases
with increasing applied load, and the wear life slightly increases
up to approximately 720 N addition and then decreases but at
a quicker rate with further increase of applied load. The rea-
son is that these coatings fail in many cases since high-applied
load will lead to severe plastic deformation of the PU coating
Fig. 5. Effect of applied load on the friction coefficient and the wear life of the PU coating filled with 3 wt.% CF or 3 wt.% TDI-CF (2.56 m/s, 60 min).
owing to the mechanical incompatibility between the PU coat-
ing and the substrate under high-applied load [13]. Moreover,
we find that the TDI-CF-filled PU coating shows lower friction
coefficient and higher wear life than those of CF-filled PU coat-
ing throughout applied load ranges. It is well known that the
fiber/matrix adhesion strength plays an important role on the
mechanical properties of fiber reinforced polymer composites.
When load is applied to composite coatings, it will be distributed
and transferred through fiber/matrix interfaces. It can be inferred
that an increase in the surface polarity or active sites for van der
Waals linking and hydrogen bonding can improve the interfa-
cial adhesion between the fiber and the surrounding polymer
matrix, leading to better stress transfer from the matrix to the
fiber materials [14].
Fig. 6 shows the variations in the friction coefficient and the
wear life of the filled PU coatings with sliding speed at 320 N.
It can be seen that the friction coefficient of the TDI-CF-filled
PU coating is lower than that of the CF-filled PU coating, and
the friction coefficient of them sharply decreases with increasing
sliding speed. This reduction in the friction coefficient attributes
to surface softening arising from frictional heating. The wear
life of the CF or TDI-CF-filled PU coating signally increases
as sliding speed goes up. Accordingly, it should be pointed out
here that the PU coatings filled with CF or TDI-CF have the best
friction and wear behaviors at a speed of 3.86 m/s under 320 N.
Presented in Fig. 7 are the typical evolutions of the friction
coefficient of CF or TDI-CF-filled PU coating as a function
of the sliding time at 2.56 m/s under different load. It can be
seen that the friction coefficient significantly follows a parabolic
pattern: the friction coefficient of the CF or TDI-CF-filled PU
coating slightly decreases as sliding time goes up and eventually
arrives a stable state value with further increasing sliding time.
Moreover, the friction coefficient shows an obvious decrease
with increasing applied load. When applied load is increased,
the newly formed debris would come into being a more inte-
grated but thinner films on the worn surface and as a result, the
smaller debris and more integrated but thinner film on the worn
surface would bring about smaller friction coefficient because
of the decreased degree of two-body abrasive wear [15]. Hence
the decrease of friction coefficient for the filled PU coating is
inevitable.
 Z.-Z. Zhang et al. / Wear 264 (2008) 599605 603

Fig. 6. Effect of the sliding speed on the friction coefficient and wear life of the PU coating filled with 3 wt.% CF or 3 wt.% TDI-CF (320 N, 60 min).

Fig. 7. Effect of sliding time on the friction coefficient of the PU coating filled with 3 wt.% CF or 3 wt.% TDI-CF (2.56 m/s): (a) The 3 wt.% TDI-CF-filled PU
coating and (b) the 3 wt.% CF-filled PU coating.

3.2. SEM analysis
Fig. 8(ac) shows the worn surface of the PU coatings filled
with 1, 3 and 10 wt.% TDI-CF under 320 N and at a speed of
2.56 m/s, respectively. It is seen that there existed remarkable
differences in the worn surface morphologies of the PU coating
filled different compositions. Namely, the worn surfaces of the
coatings filled with 1 and 3 wt.% TDI-CF are smooth, and adhe-
sion and plough marks of the worn surfaces are nearly invisible
(see Fig. 8(a and b)), and there are obvious transfer films on
the counterpart ring surfaces. Contrary to the coating filled with
low content of TDI-CF, the one filled with 10 wt.% TDI-CF

Fig. 8. SEM photographs of the worn surfaces of the PU coating and the optical micrographs of transfer films formed on the surface of counterpart ring (320 N,
2.56 m/s): (a) with 1.0 wt.%; (b) 3.0 wt.%; (c) 10.0 wt.%; (d) transfer film of (a); (e) transfer film of (b); (f) transfer film of (c).
604 Z.-Z. Zhang et al. / Wear 264 (2008) 599605
is characterized by de-bonding and pullout of the reinforcing
fibers and severe scuffing and adhesion (see Fig. 8(c)), which
could be due to the lack of a good transfer films on the sur-
face of the counterpart ring in the absence of friction modifiers.
This observation conformed to the larger wear rate of the high
content TDI-CF-filled PU coating. It is supposed that the fric-
tion modifiers TDI-CF at a proper content of 1 and 3 wt.% in
the PU coating were well embedded on the worn surfaces of the
counterpart ring to form good friction films, thus the friction and
wear of the low content TDI-CF-filled PU coating are effectively
reduced.
A polymer film layer can be transferred to the steel counter-
part, which results in a new counter surface producing primarily
an adhesive wear mechanism. This mechanism is generally less
dangerous for polymer coating sliding surface than an abrasive
one, resulting in a lower frictional coefficient and specific wear
rate. Fig. 8(df) shows the steady-state transfer films of the PU
coating filled with 1, 3 and 10 wt.% of TDI-CF, respectively.
The transfer films of the PU coating filled with 10 wt.% TDI-CF
have features that are different from those with 1 and 3 wt.%
TDI-CF. It can be seen that the transfer films for 1 wt.% TDI-
CF are thinner and more uniform. The transfer films for 3 vol.%
TDI-CF are also similar. When TDI-CF wt.% increased to 10,
the transfer films become non-uniform and it does not cover the
counter-face completely. Thus, it appears that the presence of an
excess amount of filler hinders the formation of uniform transfer
films.
The PU coating filled with 3 wt.% TDI-CF was selected as
an example to investigate the effects of the sliding speed and
applied load on the worn surface, as is shown in Fig. 9. It
can be seen that the worn surfaces of the filled PU coating are
smooth at 2.56 m/s under 320 N, and the adhesion and plough
marks on the worn surfaces are nearly invisible (see Fig. 9(a)).
When load is increased, some big particle-shaped debris in the
wear surface would be crushed or sheared into smaller parti-
cles. It generally resulted in the formation of thin compacted
wear debris layers, which appears on both surfaces of the slid-
ing components (Fig. 9b). These two layers could reduce the
Fig. 9. The SEM morphologies of the worn surfaces of the coating filled with 3 wt.% TDI-CF: (a) at 320 N and 2.5 m/s; (b) at 720 N and 2.5 m/s; (c) at 820 N and
2.5 m/s; (d) at 1.28 m/s and 320 N; (e) the high multiple of (d); (f) at 3.8 m/s and 320 N.
direct contact between the specimen and the counterpart ring,
accordingly reducing the contact pressure and the shear stresses.
As a result, the thinner films on the worn surface would bring
about smaller friction coefficient because of decreased degree
of two-body abrasive wear [15]. However, with further increase
of applied load, the wear changed from mild to severe, which
could be seen from the comparison between Fig. 9(a and c). As
is seen from Fig. 9(c), the worn surface of 3 wt.% TDI-CF-filled
PU coating sliding under 820 N clearly shows large amounts of
cracks vertical to the sliding direction, which indicates that the
serious fatigue wear is the main wear mechanism of the filled PU
coating when sliding under high applied load. It can be inferred
that large area of friction surface of the filled PU coating would
flake away if the applied load increases further and the material
would be seriously damaged.
When sliding speed is at 1.28 m/s, some adhered and plough
marks appears on the wear scar of the coating reinforced with
TDI-CF under 320 N (Fig. 9(d)). Fig. 9(e) shows the high
multiple SEM micrographic of the worn surface of the PU
coating at 320 N and 1.28 m/s. the TDI-CF removal seriously
aggravated since the soft polymer matrix could not effectively
protect TDI-CF from peeling-off. Contrary to the worn sur-
faces of the coating at a speed of 1.28 m/s, those of the coating
at a speed of 3.84 m/s are smooth and adhesion and plough
marks of the worn surface are nearly invisible (Fig. 9(f)), which
agrees well with its relatively excellent wear-resistance prop-
erty as compared with the filled PU coatings at low sliding
speed.
Fig. 10 shows SEM micrographs of the wear debris of the PU
coating filled with 3 wt.% TDI-CF under different applied load.
It is seen that the size of the TDI-CF pulled out varies from each
other under different applied load. When load is increased, some
big particle-shaped debris in the wear surface would be crushed
or sheared into smaller particles. As a result, the smaller debris
and more integrated but thinner film on the worn surface would
bring about smaller coefficients of friction because of decreased
degree of two-body abrasive wear [15]. Hence the decrease of
friction coefficients for the coatings is inevitable.
 Z.-Z. Zhang et al. / Wear 264 (2008) 599605
Fig. 10. The SEM morphologies of the debris and worn surfaces of the coating filled with 3 wt.% TDI-CF: (a) at 320 N and 2.56 m/s; (b) at 720 N and 2.56 m/s; (c)
at 820 N and 2.56 m/s.
4. Conclusion
(1) After modification with TDI, carbon fibers perform a good
bonding behavior to the PU matrix. Compared with the
unfilled PU coating, the PU coating filled with low con-
tent TDI-CF exhibits lower friction coefficient and higher
wear life. However, when content of it is above 3 wt.%, the
friction and wear behaviors of the PU coating deteriorates
with further increasing content of TDI-CF.
(2) The differences in friction and wear behaviors of the PU
coatings filled with 3 wt.% CF or 3 wt.% TDI-CF under
different sliding speed appeared to be mainly ascribed to
the influence of the contact temperature of the two rela-
tive sliding parts of the coatings. The friction coefficient of
the coating filled with CF or TDI-CF decreases with the
increasing sliding speed.
(3) Applied load has great effect on the friction and wear behav-
iors of the CF or TDI-CF-filled PU coating. As applied load
goes up, some big particle-shaped debris in the wear sur-
face would be crushed or sheared into smaller particles.
The smaller debris and more integrated but thinner film on
the worn surface would bring about smaller coefficients of
friction. Moreover, the plastic deformation becomes more
obvious when applied load is above 820 N and the surfaces
of the coatings appear to be big cracks, which deteriorates
the tribological and mechanical properties of the PU coating
filled with CF or TDI-CF.
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