Composites Part B 94 (2016) 102e108

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

Carbon fibre/graphene foam/polymer composites with enhanced

mechanical and thermal properties
Yun-Hong Zhao a, Ya-Fei Zhang a, Shu-Lin Bai a, *, Xiao-Wen Yuan b
a
Department of Materials Science and Engineering, CAPT/HEDPS/LTCS, Key Laboratory of Polymer Chemistry and Physics of Ministry of Education, College of
Engineering, Peking University, Beijing 100871, China
b
School of Engineering and Advanced Technology, Massey University, New Zealand

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

Article history: The effect of carbon fibre (CF) on the mechanical and thermal properties of graphene foam (GF)/poly-
Received 24 September 2015 dimethylsiloxane (PDMS) composites was investigated. The CFs with different weight percentages (2, 4,
Received in revised form 6, 8 and 10 wt%) were thoroughly dispersed in the PDMS matrix using a high-speed shearing and stirring
18 February 2016
method and then the GF was filled with the mixture. The CF/GF/PDMS composites were characterized in
Accepted 19 March 2016
Available online 28 March 2016
terms of microstructure, mechanical and thermal properties using various testing techniques. The results
reveal that the addition of CF observably improved the mechanical and thermal properties of GF/PDMS
composites. For 10 wt% CF/GF/PDMS composite, the tensile strength and Young's modulus are increased
Keywords:
Graphene foam
by 52% and 71% respectively compared with GF/PDMS composite. In addition, its thermal conductivity
A. Carbon fibre reaches 0.55 Wm
1 K
1, i.e., an increase by about 41% and 162% compared to GF/PDMS composite and
A. Polymer-matrix composites (PMCs) pure PDMS, respectively. SEM images show a strong interfacial bonding between CF and PDMS.
B. Mechanical properties © 2016 Elsevier Ltd. All rights reserved.
B. Thermal properties

1. Introduction [11] fabricated a GF electrode with high sulphur loading, reaching

During the past decade, graphene, a single-layered two-
dimensional (2D) structure, has been studied widely due to its
excellent mechanical, thermal and electrical properties [1e3].
Recently, graphene foam (GF) assembled from 2D graphene sheets
(GSs), graphene oxide (GO) or reduced GO (rGO) has attracted a
great attention because of its macroscopic three-dimensional (3D)
structure [4e7]. Among these, the GF fabricated using the chemical
vapour deposition (CVD) technique on a nickel foam template is
regarded as a material that best exhibits the superior thermal and
electrical properties of graphene. Pettes et al. [8] reported that the
thermal conductivity of GF varied from 0.26 to 1.7 Wm
1 K
1, being
influenced by different etchants and low internal contact thermal
resistance in the continuous GF structure. Zhang et al. [9] found that
the thermal interfacial resistance of GF at the SieAl interface was as
low as 0.04 cm2 KW
1, which is one order of magnitude lower than
conventional thermal interface materials (TIMs). Li et al. [10]
discovered that this thermal property of GF was improved with
rising temperature above room temperature, which is opposite to
the prediction by Umklapp phonon scattering theory. Zhou et al.
* Corresponding author. Tel.: þ86 10 6275 9379.
E-mail address: slbai@pku.edu.cn (S.-L. Bai).
10.1 mg cm
2, which presented an extremely high areal capacity of
13.4 mAh cm
2.
Precisely because of its integrated 3D structure and superior
properties, GF was chosen as a promising filler to greatly improve
the performance of polymer composites, such as the mechanical,
electrical and thermal properties [6,12,13]. In our previous work
[14], the thermal conductivity of 0.7 wt% GF/PDMS composite
reached 0.56 Wm
1 K
1, which was about 300% and 20% higher
than that of pure PDMS and graphene sheets/PDMS composite.
From the above studies, the amount of GF in the composites is very
limited by the CVD method and the density of Ni foam. Therefore, it
is necessary to add another type of filler such as carbon black [15],
etc. to further improve the properties of composites.
Carbon fibres (CFs) and their reinforced polymer composites
have already been investigated and applied extensively because of
their low weight, excellent mechanical properties, superior elec-
trical properties and high thermal conductivity [16e22]. Jin et al.
[23] introduced a model to predict the thermal conductivity of CF
reinforced polytetrafluoroethylene composites. Patton et al. [24]
prepared vapour grown carbon fibre (VGCF)/phenolic resin com-
posites and found that the average thermal conductivity reached
0.7714 Wm
1 K
1 at 40 wt% VGCF. Wu et al. [25] found that due to
CF's highly crystallinity, CF reinforced polyamide-6/clay composites

http://dx.doi.org/10.1016/j.compositesb.2016.03.056
1359-8368/© 2016 Elsevier Ltd. All rights reserved.
 Y.-H. Zhao et al. / Composites Part B 94 (2016) 102e108
showed a higher heat distortion temperature than the same com-
posite reinforced with glass fibre. Rezaei et al. [26] investigated the
effect of fibre length on the thermal properties of short carbon
fibre/polypropylene composites, and found that the longer CFs
endowed the composites with better thermomechanical properties
and thermal stability.
Due to the small size of graphene, its reinforcement effect on
mechanical properties of polymer composites is very limited.
Fortunately, carbon fibres can remedy this shortfall because of their
rigid and straight nature. The thermal conductivity of graphene is
much higher than that of carbon fibre. So, the combination of
graphene and carbon fibre may afford the composite with both high
thermal and mechanical properties, and find broad applications in
industry. Using 3D graphene foam as a filler can avoid the
agglomeration problem of 2D graphene sheets. Currently, com-
posites composed of 3D graphene foam and carbon fibre do not
exist and should be further investigated.
In this paper, a novel polymer matrix composite reinforced with
3D graphene foam and 1D carbon fibre was first prepared and
characterized in terms of mechanical and thermal properties. It is
expected to have better performance than single graphene and
single carbon fibre reinforced composites. As a result, the study will
provide a path for the development of new composite materials.
2. Materials and experimental methods
2.1. Preparation of the mixture of short CFs and PDMS
Nickel foam and CFs (T-300B) were supplied by Shanghai
Zhongwei Materials Co. Ltd. and Torayca, respectively. Poly(methyl
methacrylate) (PMMA) with molecular weight of 996,000 was
purchased from Sigma Aldrich. Polydimethylsiloxane (PDMS, Syl-
gard184) used as polymer matrix was supplied by Dow Corning.
Short CFs of about 1 mm long were dispersed in acetone and
sheared with high speed for 2 h. Then the base agent of PDMS was
added and sheared for another 1 h. Next, the acetone was removed
at 60  C with continuous magnetic stirring. At last, the curing agent
(base agent/curing agent ¼ 10/1 in weight) was added and the
mixture was stirred for 30 min.
2.2. Preparation of composites
The GF was fabricated by using the CVD method on a nickel
foam template which was reported in detail in our previous work
[15]. The mixture of CF and PDMS was poured into the mould filled
with freestanding GF in advance. Then it was vacuumized, pressed
mechanically under about 1.0 MPa and solidified at 80  C for 4 h. For
comparison, pure PDMS, GF/PDMS and CF/PDMS composites were
also prepared in a similar way. The GF loading of both GF/PDMS and
CF/GF/PDMS composites is 0.5 wt%, while CF's contents are 2, 4, 6, 8,
10 wt% for CF/PDMS and CF/GF/PDMS composites.
2.3. Characterization methods
The morphology of CF, GF and composites was observed by
scanning electron microscope (SEM, S-4800, HITACHI). The length
of short CF was measured with metalloscope (6XB-PC, Beijing
Shangguang). The thickness of graphene sheet (GS) composing GF
was identified by transmission electron microscope (TEM, JEM-
2100F, JEOL). The samples for tensile tests are standard dumbbell
pieces, 2 mm in thickness and 35 mm in length according to GB/T
528-92, and were tested on the MiniMat 2000 type tensile machine
at a loading rate of 1.5 mm/min. The valid parallel part of the
sample is 2 mm in width and 12 mm in length. The heat flux
method (DRL-III, Hunan Xiangyi Instruments Co. Ltd.) was applied
103
to measure the thermal conductivity with the sample dimension of
30 mm in diameter and 2 mm in thickness. Three samples of each
composite were tested to get average values both for tensile
strength and thermal conductivity measurements. Thermogravi-
metric analysis (TGA, Q600 SDT, TA) was utilized to evaluate the
thermal stability from room temperature to 900  C at a scan rate of
20  C/min in a N2 atmosphere.
3. Results and discussions
3.1. Morphology
SEM images in Fig. 1(a) and (b) present the morphology and length
distribution of CF. The diameter is about 8 mm, and the length dis-
tribution proves the reduction from initial 1 mm to about 150 mm on
average after the high-speed shearing and stirring. The surface shows
deep or shallow rill-like folds rather than being smooth. Fig. 1(c)
shows that the thickness of hollow arms and pore diameter of GF are
about 40 mm and 300 mm, respectively. Fig. 1(d) and (e) show a small
piece of graphene sheet (GS) taken from GF with thickness 3e4 nm.
Fig. 2 shows the SEM images of freeze-fractured surfaces of GF/
PDMS and CF/GF/PDMS composites with different CF loadings. As
shown in Fig. 2(a), the liquid PDMS not only filled the GF pores, but
also penetrated into the GF arms without any obvious bubbles. It can
be seen from Fig. 2(b)-(f) that the CF exists only in the space of the
interconnected network. Due to its longer length compared to the
arm thickness of GF, it could not penetrate into the interior of GF arms
as shown in Fig. 2(c) (Fig. 2(d)-(f) are similar, but with different CF
contents.). It is noted that the distribution of CF is uniform and
random within the PDMS matrix, which can be attributed to the effect
of high-speed shearing and stirring. Also, the interface between CF
and PDMS is good without evident pulling out of CF by freeze fracture.
3.2. Mechanical properties in tension
To investigate the reinforcement effect of different CF loadings
on the mechanical properties of CF/GF/PDMS composites, tensile
tests were carried out. Typical stressestrain curves are shown in
Fig. 3(a), from which values of Young's modulus, tensile strength
and elongation at break can be obtained, as presented in Fig. 3(b)-
(d). As can be seen in Fig. 3(b) and (c), both Young's modulus and
tensile strength display an important increase with the addition of
GF and CF. The Young's modulus and tensile strength of GF/PDMS
composite increase by 66% and 7% respectively compared with pure
PDMS. The adding of CF can further improve the mechanical
properties of composites. At 10 wt% CF, Young's modulus and ten-
sile strength reach 3.05 MPa and 2.50 MPa, i.e., an improvement of
71% and 52% respectively compared with the GF/PDMS composite,
and by 185% and 63% respectively compared with pure PDMS.
According to Halpin-Tsai's equations [27,28], Young's modulus E
of short fibre reinforced composite can be obtained by
" # " #
E 3 1 þ zhL Vf 5 1 þ 2hT Vf
¼ þ (1)
Em 8 1
hL Vf 8 1
hT Vf
where
z ¼ 2l=D (2)
.
Em
1
Ef
hL ¼ . (3)
Ef Em þ z
and
104 Y.-H. Zhao et al. / Composites Part B 94 (2016) 102e108

Fig. 1. (a) Surface morphology and (b) statistic length distribution of CF. (c) GF morphology. (d), (e) TEM images of GS composing GF.

Fig. 2. SEM images of freeze-fractured surfaces of (a) GF/PDMS composite, (b) 2 wt%, (c) 4 wt%, (d) 6 wt%, (e) 8 wt%, (f) 10 wt% CF/GF/PDMS composites.

. marginally higher than the experimental value. The gap between

Em
1
Ef
hT ¼ .
Ef Em þ 2
where Ef and Em are the moduli of fibre and matrix, respectively, l and
D are the average length and diameter of fibre, respectively, and vf is
the volume fraction of filler. In this work, the values are: Ef ¼ 230 GPa,
Em ¼ 1.78 MPa (matrix: GF/PDMS composite), l ¼ 150 mm, D ¼ 10 mm
and vf ¼ 5.8 vol% (equal to 10 wt%). By using the above equations, the
Young's modulus of 10 wt% CF/GF/PDMS is about 3.26 MPa,
experimental and theoretical values is, in our opinion, due to the
(4) limited CF distribution in the GF space and not being present in the
interior of the GF arms. CF length is greater than the width of GF arm,
so they can't enter into the GF arm. This means that a pure solid
PDMS tunnel with graphene skin constitutes the main structure,
while CF only reinforces the PDMS matrix in the space between the
interconnected GF structures. Therefore, due to the particular dis-
tribution of CF in the composite, the actual reinforcement efficiency
of CF to GF/PDMS composite is lower than that in theory. The latter
modulus can be well predicted by the theoretical model.
 Y.-H. Zhao et al. / Composites Part B 94 (2016) 102e108
Fig. 3. (a) Typical stressestrain curves, (b) Young's modulus, (c) tensile strength and (d) elongation at break of the materials studied.
The elongation at break of the materials studied initially in-
creases then decreases with the increasing content of CF as shown
in Fig. 3(d). This signifies that an appropriate content of CF can still
increase the deformation ability of CF/GF/PDMS composites. While,
higher content of CF compromises and reduces this ability.
Fig. 4 shows the SEM images of tensile fractured surfaces of the
materials studied, which give a better understanding of the
mechanism of tensile failure. The tensile fractured surface of pure
PDMS shown in Fig. 4(a) is smooth, indicating quick fracture. The
red arrows in Fig. 4(b) show the debonding of GF from PDMS,
indicating weak interface bonding. However, due to superior me-
chanical properties of graphene and the interconnected structure of
GF, a lot of energy was absorbed when the fracture of GF happened
as shown in Fig. 4(c), leading to the improvement of Young's
modulus and tensile strength [3,13,29,30]. The crack originated
from the GF fracture propagated either along the interface, or into
the PDMS matrix to cause final failure, resulting in the decrease of
elongation at break. Fig. 4(d)-(f) display the morphology of tensile
fractured surfaces of CF/GF/PDMS composite. Under tensile loading,
besides the interfacial debonding of GF from PDMS, the peeling and
fracture of GF are also observed as marked by the arrows in
Fig. 4(d). In Fig. 4(f), the protruding CF along the tensile direction
remains coated by PDMS and there is no obvious debonding be-
tween CF and PDMS. The red arrow in Fig. 4(f) indicates that the
extended direction of crack is not along the interface between CF
and PDMS, which clearly means a strong interface bonding
105
between CF and PDMS. In this case, the tensile load could be
effectively transferred from PDMS to CF. Also, the existence of CF
and good interface bonding between CF and PDMS obstructed the
propagation of cracks, and so made the tensile fracture surface of
composite coarse and multiplanar marked by the red arrows in
Fig. 4(e), bringing about an improvement in mechanical properties,
e.g., elongation at break. However, when the loading of CF exceeds
4 wt%, the decrease of elongation at break of composites may be
caused by local agglomeration of CF which could generate minor
cracks and holes.
The strong interfacial bonding may be attributed to the special
surface structure of CF that is covered with rill-like folds, rendering
the crack being deflected and pinned, as well as preventing the
cracks propagation [19]. This mechanism is similar to the contri-
bution of the wrinkled surface of graphene to the mechanical
properties improvement of its polymer composites [31].
3.3. Thermal properties
3.3.1. Thermal conductivity
The thermal conductivity of CF/PDMS and CF/GF/PDMS compos-
ites was examined as a function of CF content and the results are
shown in Fig. 5. With the increasing content of CF, the thermal
conductivity increases gradually. It increases from 0.21 Wm
1 K
1 for
pure PDMS to 0.39 Wm
1 K
1 for GF/PDMS composite, i.e., an in-
crease of 86%. The thermal conductivity is further improved by
106 Y.-H. Zhao et al. / Composites Part B 94 (2016) 102e108
Fig. 4. SEM images of tensile fracture surfaces of (a) PDMS, (b) (c) GF/PDMS (Red arrow in Fig. 4(b) shows the debonding of GF from PDMS and those in Fig. 4(c) indicate the rupture of
graphene layer and GF/PDMS arm.) and (d) e (f) 10 wt% CF/GF/PDMS composites (Red arrows in Fig. 4(d) show the fracture and peeling of GF and those in Fig. 4(e) show the multiplane and
that in Fig. 4(f) shows good bonding of CF and PDMS.). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
introduction of GF. The highest value is 0.55 Wm
1 K
1 for 10 wt%
CF/GF/PDMS composite, which is 41% and 162% higher than that of
GF/PDMS composite and pure PDMS, respectively. The two curves in
Fig. 5 are almost parallel. The gap between them is about
0.17 Wm
1 K
1, which is most likely due to the GF. In fact, the
improvement in thermal conductivity of composites derives from the
co-contribution of GF and CF. Due to the high thermal conductivity of
graphene and its interconnected structure, GF supplies an effective
heat conduction pathway [8,14,32,33]. The effect of CF on thermal
conductivity can be ascribed to two factors. The first is the formation
of self-thermal conductive network of CFs [23,34,35], and the second
is the connection of CFs to GF arms to form a big intensive network.
3.3.2. Thermal stability
To investigate the thermal stability, thermal degradation of ma-
terials studied was evaluated; corresponding TGA and differential
Fig. 5. Thermal conductivity of materials studied.
thermogravimetric (DTG) analysis curves are shown in Fig. 6. It can
be noted in Fig. 6(a) that pure PDMS and GF/PDMS composite exhibit
similar profiles of curves and almost the same rate of weight loss
below 450  C, then rapidly decrease above 450  C. Conversely to the
above results, the TGA curves of CF/GF/PDMS composites obviously
shift towards higher temperature above 550  C. Above 400  C, the
weight loss increases with elevated temperature, while they become
moderate from 550  C to 650  C, indicating descending rate of
weight loss. Above 650  C, the rate of weight loss increases again. For
10 wt% CF/GF/PDMS composite, the T25% (the temperature at 25%
weight loss) increases by 56  C and 116  C compared with GF/PDMS
composite and pure PDMS, respectively. Fig. 6(b) shows that the CF/
GF/PDMS composites decomposed with an apparent two-step pro-
cess, independent of CF loading values. Moreover, the incorporation
of CF brought about an obvious increase in the temperature of the
maximum weight loss rate compared with PDMS and GF/PDMS
composite. The improvement in thermal stability is due to the barrier
effect of CF to the movement of PDMS molecular chains and the
escape of volatiles generated during pyrolysis. Furthermore, the
strong interface bonding between CF and PDMS could increase the
physical and chemical crosslinking points to prevent decomposition
of PDMS [36,37].
4. Conclusions
A new type of composite was designed and manufactured. It is
composed of 3D graphene foam (GF) and short carbon fibre (CF) as
reinforcement, and polydimethylsiloxane (PDMS) as the matrix.
The mechanical and thermal properties of this composite were
investigated. A remarkable finding is the co-effect of graphene
foam and carbon fibre in the enhancement of performance of
polymer composites. Graphene foam with high thermal conduc-
tivity contributes much to the thermal properties of composites,
while the carbon fibre with its high rigidity and strength endows
the composites with improved mechanical properties. Another
finding is the importance of filler geometry. The rigid and straight
filler is very beneficial to both the mechanical and thermal
 Y.-H. Zhao et al. / Composites Part B 94 (2016) 102e108
Fig. 6. (a) TGA and (b) DTG curves of the materials studied.
properties of composites. At 10 wt% CF, the tensile strength, Young's
modulus and thermal conductivity of CF/GF/PDMS composites are
increased by 52%, 71% and 41%, respectively, compared to GF/PDMS
composite. Its thermal stability is also improved significantly.
Overall, the addition of CF and GF has effectively improved the
mechanical and thermal properties, as well as thermal stability of
pure PDMS, which makes CF/GF/PDMS composite a good candidate
for application in some fields requiring both superior mechanical
and thermal properties, such as thermal interface materials.
Acknowledgements
The authors would like to thank the support by NSFC and NSFC-
RGC Joint Research Scheme (Nos. 11272008, 11361161001, 11202005
and CUHK450/13).
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