Composites: Part B 57 (2014) 120–125

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Composites: Part B
journal homepage: www.elsevier.com/locate/compositesb

Tribological performance of carbon nanotube–graphene oxide

hybrid/epoxy composites
Xiao-Jun Shen a,b, Xian-Qiang Pei c, Yu Liu a, Shao-Yun Fu a,⇑
a
Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190, China
b
Materials and Textile Engineering College, Jiaxing University, Jiaxing 314001, Zhejiang Province, China
c
Institute for Composite Materials (IVW GmbH), Technical University of Kaiserslautern, 67663 Kaiserslautern, Germany

a r t i c l e i n f o a b s t r a c t

Article history: An investigation is conducted on the effect of the hybrid of multi-wall carbon nanotubes (MWCNTs) and
Received 25 June 2013 graphene oxide (GO) nanosheets on the tribological performance of epoxy composites at low GO weight
Received in revised form 16 September 2013 fractions of 0.05–0.5 phr. The MWCNT amount is kept constant at 0.5 phr, which is typical for CNT/epoxy
Accepted 27 September 2013
composites with enhanced mechanical properties. Friction and wear tests against smooth steel show that
Available online 5 October 2013
the introduction of 0.5 phr MWCNTs into the epoxy matrix increases the friction coefficient and decreases
the specific wear rate. When testing the tribological performance of MWCNT/GO hybrids, it is shown that
Keywords:
at a high GO amount of 0.5 phr, the friction coefficient is decreased below that of the neat matrix whereas
A. Hybrid
A. Polymer–matrix composites (PMCs)
the wear rate is increased above that of the neat matrix. At an optimal hybrid formulation, i.e., 0.5 phr
B. Wear MWCNTs and 0.1 phr GO, a further increase in the friction coefficient and a further reduction in the
specific wear rate are observed. The specific wear rate is reduced by about 40% down to a factor of 11
relative to the neat epoxy when the GO content is 0.1 phr.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction tronic, thermal and mechanical properties [11–16]. However, to

Epoxy resins are widely used as matrices for composites in anti-
wear materials although neat epoxy resins normally have poor
wear resistance. Therefore, it is of great importance to improve
the tribological performance of epoxy resins [1–8]. In conventional
routes, the combined usage of short carbon fibers and internal
lubricants (e.g., graphite or polytetrafluoroethylene) in an epoxy
matrix leads to a significant improvement in the dry sliding wear
performance against metallic counterparts [5]. On the other hand,
inorganic nano-fillers, e.g., boron nitride, SiO2, nano-diamond, tita-
nium dioxide nanoparticles, Na-montmorillonite and carbon nano-
tubes (CNTs), are often employed to improve the tribological
performance of the epoxy resins [4–8]. The extremely large surface
area is one of the most attractive characteristics of nanoparticles,
which contributes to the improvement in the tribological perfor-
mance [9].
Very recently, we used graphene oxide (GO) to improve the
tribological performance of epoxy resins and obtained promising
results [10]. The CNT–graphene oxide hybrids have been employed
as reinforcing and functional fillers in polymer composites [11–16].
Composite materials filled with the hybrid of carbon nanotubes
(CNTs) and graphene showed unique synergistic effects on elec-
⇑ Corresponding author. Fax: +86 010 82543752.
E-mail address: syfu@mail.ipc.ac.cn (S.-Y. Fu).
the best of our knowledge, no work has been reported on the effect
of the MWCNT–GO hybrid on the tribological performance of
epoxy composites.
In this work, hybrid composites were prepared by incorporating
MWCNTs and GO nanosheets into an epoxy matrix in order to en-
hance the tribological performance. It was observed that the signif-
icant enhancements in tribological performance were achieved by
introducing the hybrid of MWCNTs and GO nanosheets at proper
contents into the epoxy matrix. Also, we investigated the glass
transition temperature (Tg) of the hybrid composites.
2. Experimental section
2.1. Materials
Epoxy resin (WSR615) based on bisphenol-A with an epoxy va-
lue of 0.50–0.56 was purchased from Wu Xi Resin Factory, China.
The curing agent (DETDA) with an amine equivalent weight of
44.3 was purchased from Kun Shan Chemical Co., Ltd., China, which
is a mixture of 2,4- and 2,6-isomers. Natural graphite powder was
obtained from Qingdao AoKe ShiMo Co., Ltd., China. MWCNTs with
a diameter of 30–50 nm, a length of 10–20 lm, and a purity of
>95 wt% were purchased from Chengdu Organic Chemicals Co.,
Ltd., China [17,18]. Hydrochloric acid, ethanol, potassium perman-
ganate and concentrated sulfuric acid were purchased from Beijing

1359-8368/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesb.2013.09.050
 X.-J. Shen et al. / Composites: Part B 57 (2014) 120–125 121

Chemical Works and used as received. Sodium nitrate was pur-
chased from Tianjin JinKe Fine Chemical Industry Research
Institute.
2.2. Preparation of GO and epoxy composites
Graphite oxide was prepared by oxidizing natural graphite
powder using a method similar to the Hummer’s approach [19].
The resultant graphite oxide was dispersed in ethanol to form a
suspension of 0.5 mg ml 1. The latter was treated by an ultrasonic
process (1000 W) for 1 h in order to exfoliate the graphite oxide to
layered GO. To prepare the GO/epoxy composites, epoxy resin was
firstly mixed with the GO suspension, then the mixture was
mechanically stirred for 2 h, and the resultant mixture was treated
by the ultrasonic technique (1000 W) for another hour. The mix-
ture was put in an oven at 80 °C for 24 h to remove the ethanol.
The MWCNTs were added to the mixture using a three-roll miller.
Afterwards, the curing agent was added to the mixture in a ratio of
23.6 (DETDA) to 100 (DGEBA), whereby degassing was carried out
with a vacuum pump to eliminate air bubbles and residual ethanol.
The final mixture was casted into an open mold. The blends were
cured at 80 °C for 8 h, then at 130 °C for 12 h. After curing, the
specimens were cooled naturally to room temperature. Epoxy
composites containing weight fractions of 0.05, 0.1, 0.2 and
0.5 phr GO were then prepared. All the composite samples contain
0.5 phr MWCNTs.
frequency of 10 Hz, raising the temperature from 120 to 250 °C
at a heating rate of 2 °C/min.
Wear tests were carried out by a Wazau pin-on-disc machine
using the following conditions: a nominal pressure of 1 MPa and
a sliding speed of 1 m/s at room temperature and dry sliding. The
size of the wear pins was 4 mm  4 mm  12 mm. In order to re-
duce the running-in period, all the samples were pre-worn before
testing with different grinding papers (firstly P 800 and then P
1200) placed between the pin and the disc. This process could re-
sult in the same roughness of the pins before testing and in a good
matching of the counterpart configuration. A disc of 100Cr6 steel
(German standard; ball bearing steel) was used as the counterpart,
which was cleaned by isopropanol and acetone before testing. The
worn surfaces and wear debris of the epoxy composites were ana-
lyzed by SEM after being coated with a thin gold layer.
3. Results and discussion
3.1. Characterization of GO and MWCNTs
Fig. 1 shows the SEM and TEM images of GO nanosheets and
MWCNTs. A thin, wrinkled film morphology is seen for GO
(Fig. 1a). Consistent with the SEM results, the TEM image of GO re-
veals a similar morphology as shown in Fig. 1b and c displays that
the diameter of MWCNTs is 30–50 nm, and the TEM image (Fig. 1d)

2.3. Characterization

Scanning electron microscope (SEM) images for MWCNTs and

GO were obtained using a Hitachi S-4300 microscope (Japan),
and SEM images for the worn surfaces of the epoxy composites
were obtained by a JEOL JSM-6300 microscope (Japan). Transmis-
sion electron microscopy (TEM) images were carried out on a JEOL
JEM-2010 instrument in bright field. The phase purity of MWCNTs
and GO was characterized by X-ray diffraction (XRD) on an X-ray
diffractometer with Cu Ka radiation (k = 1.5418 Å). Dynamic
mechanical thermal analysis (DMTA) was carried out by a Gabo
Qualimeter Explexor under the tension configuration. The size of
the samples for DMTA testing was 55 mm  10 mm  2 mm. The
DMTA data of each sample were determined at a constant Fig. 2. XRD patterns of the GO and the MWCNTs.

Fig. 1. (a) SEM and (b) TEM images of GO, (c) SEM and (d) TEM images of MWCNTs.
122 X.-J. Shen et al. / Composites: Part B 57 (2014) 120–125
Fig. 3. The DMTA curves (damping factor tan d) of the pure epoxy and the hybrid
MWCNT–GO/epoxy composites with 0.5 phr MWCNTs and various GO contents.
Fig. 4. Friction coefficient for the GO/epoxy composites [10] and the hybrid
MWCNT–GO/epoxy composites with 0.5 phr MWCNTs and various GO contents
tested under the condition of 1 MPa and 1 m/s.
confirms the SEM results. The XRD patterns of the GO and
MWCNTs are displayed in Fig. 2. Typical (0 0 2) and (1 0 0) peaks
of MWCNTs are obtained at 2h of 26° and 43°, respectively,
Fig. 5. Microphotographs of the counterpart for the hybrid MWCNT–GO/epoxy composites with various GO contents: (a) 0 phr, (b) 0.1 phr and (c) 0.5 phr. The samples were
tested under the dry sliding conditions of 1 MPa and 1 m/s for 10 h.
which is in consistent with the previous results [20]. For GO, a
broad peak at 2h = 10.2° is obtained, which is assigned to the dif-
fraction of the (0 0 2) plane. The observed weak peak indicates that
the graphene layers are sufficiently disordered [21]. This means
that the graphite oxide was exfoliated sufficiently to form GO
nanosheets.
3.2. DMTA results of epoxy composites
The glass transition temperature (Tg) of a polymer characterizes
the segmental motion of macromolecules [22]. In order to under-
stand the synergistic effect of the MWCNT–GO hybrids on the Tg
of the neat epoxy, DMTA studies are carried out. Fig. 3 shows that
a tan d peak is observed at 126 °C for the neat epoxy, and the cor-
responding peaks shift to 155.5 °C and 160.1 °C after the addition
of 0.5 phr MWCNTs and 0.5 phr MWCNT–0.05 phr GO hybrid,
respectively, i.e., an evident increase of 29.5 °C and 34.1 °C. The
drastic shift of the Tg to a higher temperature can be ascribed to
the restricted molecular mobility of the epoxy matrix by the
MWCNTs and GO [23,24].
However, as the GO content is increased to 0.1 phr, the Tg is
slightly lowered to 158.0 °C. With a further increase of the GO con-
tent to 0.5 phr, a reduction of Tg becomes evident, i.e., down to
112.7 °C, which is even lower than that of the neat epoxy. The
reduction of Tg with increasing GO content may be attributed to
a consumption of the curing agent by the GO nanosheets with
epoxy groups [25,26], which can decrease the crosslinking density
of the epoxy resin since the stoichiometric amounts of epoxy pre-
cursor and curing agent are formulated initially [10].
3.3. Tribological performance of epoxy composites
Fig. 4 shows the friction coefficient of the hybrid composites as
a function of GO content. The data refer to the mean values mea-
sured in the steady state range of the wear process. When the
nanofiller consists of only 0.5 phr MWCNTs, the friction coefficient
of the composite is twice as high as that of the neat epoxy. Adding
up to a 0.2 phr GO to the MWCNT/EP sample keeps the friction
coefficient of the hybrid composite on the same high level. This
 X.-J. Shen et al. / Composites: Part B 57 (2014) 120–125
can be due to the wrinkled surface morphology of GO and the wavy
morphology of MWCNTs (as shown in Fig. 1), which would rough-
en the surface of the composite [27,28]. However, the friction coef-
ficient of the composites is decreased once the GO content is
increased to 0.5 phr. This result is different from that for the GO/
epoxy composites [10], as also shown in Fig. 4. The significant de-
crease in the friction coefficient for the hybrid composites can be
associated with the formation of a solid transfer film on the coun-
terpart (Fig. 5). With the formation of a uniform and tenacious
transfer film, sliding occurs between the surface of the composite
block and the transfer film [29], and not between the rough surface
of the composite and the steel counterpart.
Fig. 6 shows that contrary to the variation of the friction coeffi-
cient, the specific wear rate of the neat epoxy drops drastically
after the incorporation of only a small amount (0.5 phr) of
MWCNTs into the epoxy matrix. Then, the specific wear rate is fur-
ther lowered by about 40% once 0.1 phr GO is added. The specific
rate is reduced down to a factor of 11 relative to the neat epoxy
when the GO content is 0.1 phr. However, as the GO content is fur-
Fig. 6. Specific wear rate for the GO/epoxy composites [10] and the hybrid
MWCNT–GO hybrid/epoxy composites with 0.5 phr MWCNTs and various GO
contents tested under the condition of 1 MPa and 1 m/s.
Fig. 7. SEM images of the worn surfaces of the hybrid MWCNT–GO/epoxy composites with 0.5 phr MWCNTs and various GO contents: (a) 0 phr, (b) 0.1 phr and (c) 0.5 phr; (d)
TEM image of the worn surface of the composite with 0.5 phr MWCNTs and 0.5 phr GO.
123
ther increased to 0.5 phr, the specific rate is drastically increased,
and it becomes even much higher than that of the pure epoxy.
As shown in Fig. 7a, an aggregation of MWCNTs can be seen on
the worn surface of the composite containing 0.5 phr MWCNTs.
But the interfacial adhesion between MWCNTs and epoxy matrix
seems to be reasonably good, which is beneficial to the stress
transfer between the MWCNTs and the epoxy matrix. As a result,
the specific wear rate of the composite is reduced drastically by
the introduction of MWCNTs into the epoxy resin. Compared to
the composite containing only 0.5 phr MWCNTs, the specific wear
rate of the composite with the additional 0.1 phr GO is further re-
duced by about 40%. There are two reasons for this superiority of
employing both MWCNTs and GO nanosheets. On the one hand,
when the composite contains both 0.5 phr MWCNTs and 0.1 phr
GO, the dispersion of MWCNTs is greatly improved compared to
that for the corresponding MWCNT/epoxy composite (Fig. 7b). This
result is consistent with the literature [11]. GO nanosheets which
can stably disperse in the epoxy [10], as ‘‘soft’’ two-dimensional
macromolecules containing multiple aromatic regions and hydro-
philic oxygen groups, can adsorb pristine MWNTs through p-stack-
ing interaction, which would lead to a more stable dispersion of
MWNTs in epoxy [30]. On the other hand, the existence of reactive
OH, carboxyl and epoxy groups on the GO nanosheets and their
good mechanical interlocking arising from the wrinkled rough sur-
face of GO would lead to an excellent interfacial adhesion between
GO and epoxy. OH and carboxyl groups might react with the epoxy
precursor while epoxy groups might react with the curing agent
[10]. The excellent interfacial adhesion is also beneficial to the
stress transfer between the GO and the epoxy matrix. However,
unlike the GO/epoxy composites [10], the specific wear rate of
the hybrid composites is drastically increased again as the GO con-
tent is increased to 0.5 phr. This may be attributed to two reasons:
(1) an aggregation of GO nanosheets at high contents, as shown in
Fig. 7c and d, results in stress concentrations at GO aggregate sites,
leading to a higher specific wear rate and (2) a high GO content
consumes a certain amount of the curing agent [25,26], thus
decreasing the crosslinking density of the epoxy resin (since the
stoichiometric amounts of epoxy precursor and curing agent were
formulated initially [10]).
124 X.-J. Shen et al. / Composites: Part B 57 (2014) 120–125

Fig. 8. SEM images of the worn surfaces of the hybrid epoxy composites with 0.5 phr MWCNTs and various GO contents: (a) pure epoxy, (b) 0 phr, (c) 0.1 phr and (d) 0.5 phr;
the wear debris of the hybrid composites with various GO contents: (e) pure epoxy, (f) 0 phr, (g) 0.1 phr and (h) 0.5 phr.

If the amount of the GO exceeds the limit given in this study,
the wear resistance may be further reduced. Possible explanations
are given herein. GO has an extremely large specific surface where
the epoxy matrix is adsorbed [10]. Therefore, only a small amount
of GO can be mixed in the epoxy matrix if every GO sheet needs to
be properly wetted as CNTs [31]. At high contents, aggregates of
GO nanosheets will appear, as shown in Fig. 7c and d. This means
that the dispersion of GO nanosheets will become worse at higher
contents. As a result, weak interfaces will appear and the compos-
ites subjected to the frictional force may be easily damaged [32],
leading to a higher specific wear rate (namely a further reduction
in tribological performance).
Fig. 8a shows cracking signs covering the whole worn surface of
the pure epoxy, and relatively large wear debris is seen accordingly
(Fig. 8e). In the case of the composite containing 0.5 phr MWCNTs
(with 0 phr GO), almost no cracking signs can be seen on the worn
surface of the composite (Fig. 8b), and the wear debris (Fig. 8f) be-
comes smaller than that of the pure epoxy. For the case of the hy-
brid MWCNT–GO/epoxy composite containing 0.1 phr GO, a
different wear surface morphology is observed. Namely, almost
no microcracks can be observed (Fig. 8c). Meanwhile, smaller par-
ticle-shaped wear debris is formed (Fig. 8g). However, when the
GO content goes up to 0.5 phr, the nanofillers aggregate (Fig. 8d)
and the corresponding wear debris is very large (Fig. 8h). All these
observations are consistent with the wear rate results.
4. Conclusions
The incorporation of MWCNT–GO hybrid at a low content into
an epoxy matrix has led to a significantly enhanced tribological
 X.-J. Shen et al. / Composites: Part B 57 (2014) 120–125
performance. Compared to the MWCNT/epoxy composites, the hy-
brid composite with 0.1 phr GO nanosheets next to the MWCNTs
displayed an obvious superiority. This is based on two reasons.
Firstly, the dispersion of MWCNTs in the epoxy matrix was greatly
improved as 0.1 phr GO was employed. Secondly, the introduction
of GO could enhance the nanofiller-epoxy adhesion/interlocking
and the glass transition temperature.
Acknowledgments
This work was supported by the Beijing Municipal Natural Sci-
ence Foundation (No. 2122055), the National Natural Science
Foundation of China (Nos. 10972216 and 51073169), the National
Basic Research Program of China (No. 2010CB934500), the Science
and Technology Plan Projects of Jiaxing City Technology Bureau
(No. 2013AY11016) and the Scientific Research Projects of Zhejiang
Province Education Department (No. Y201330172). Prof. Fu thanks
the Alexander von Humboldt Foundation for supporting his visit to
the Institute of Composite Materials at the Technical University of
Kaiserslautern (TUK), Germany, in 2011–2012. The authors also
thank the Institute for Composite Materials (IVW GmbH) at the
University of Kaiserslautern for the experimental support and Prof.
Dr. Klaus Friedrich for his critical comments and revisions on the
manuscript.
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