J Polym Eng 2016; 36(5): 465–471
Ayesha Kausar* and Muhammad Siddiq
Epoxy composites reinforced with multi-walled
carbon nanotube/poly(ethylene glycol)
methylether-coated aramid fiber
DOI 10.1515/polyeng-2015-0191
Received April 30, 2015; accepted August 24, 2015; previously published
online November 26, 2015
Abstract: A novel type of aramid fibers coated with
poly(ethylene glycol) methyl ether (PEGME)-modified
multi-walled carbon nanotubes (MWCNTs) was designed
using electrophoresis. Owing to the good interaction of
MWCNT-PEGME with the matrix, the coated fibers were
well dispersed in epoxy resin. Thin films of epoxy/aramid-
MWCNT-PEGME were prepared by placing the modified
aramid fibers in molds, and the epoxy resin was infused
into them. 4,4′-Diaminodiphenylmethane was dissolved
in epoxy before the resin was poured over the aramid fib-
ers coated with MWCNT-PEGME. According to fracture
surface studies, the modified fibers were completely mis-
cible with the epoxy resin and the filler was dispersed
well in the space between the aramid fibers. The tensile
strength of neat resin was increased from 658 to 1198 MPa
in 40 wt.% of fiber-loaded epoxy/aramid-MWCNT-PEGME
40 composite. The maximum flexural strength was also
found to be higher for epoxy/aramid-MWCNT-PEGME
40 (1593 MPa). The glass transition temperature (Tg) was
studied using differential scanning calorimetry, in the
range of 164–173°C. The tensile strength, modulus, flex-
ural strength, and Tg of epoxy/aramid fiber composites
with unmodified fibers were found to be lower than those
of epoxy/aramid-MWCNT-PEGME composites.
Keywords: aramid fibers; electrophoresis; epoxy; fracture
surface; MWCNTs.
*Corresponding author: Ayesha Kausar, Nanosciences and
Catalysis Division, National Center For Physics, Quaid-i-Azam
University Campus, Islamabad, Pakistan,
e-mail: dr.ayeshakausar@yahoo.com
Muhammad Siddiq: Department of Chemistry, Quaid-i-Azam
University, Islamabad, Pakistan
1 Introduction
The properties of aramid fibers make them suitable for
use in numerous industries. Aramid fibers are employed
in cables, optical fibers, ballistics, conveyer and trans-
mission belts, linear tension members, tires, and cut and
heat protection [1]. Owing to their stiffness, low density,
and noble resistance to crack, these fibers are widely
utilized in transportation and marine industries for
constructing stronger, stiffer, lighter, and more durable
materials [2]. In recent times, carbon nanotubes (CNTs)
have been the focus of considerable research on inno-
vative, next-generation materials with high stiffness
and high strength [3]. CNTs have presented potential
requisitions in composites based on their outstanding
thermal, electrical, and mechanical properties, and on
their low density and high aspect ratio [4]. For these
reasons, there have been numerous efforts to use CNTs
in the consolidation of composite resources to overcome
the extent of performance of traditional materials. Nev-
ertheless, research in this field has dealt with polymer/
CNT composites that offer remarkable strengthening
impact for the subsequent materials [5]. Moreover, the
literature has shown that the fracture toughness, shear,
thermal, flexural, and tensile properties of polymer-
based composite materials improve considerably with a
0.1–5 wt.% loading of CNTs [6, 7]. Because of the inter-
facial interactions, mainly in the interphase of superfi-
cially functionalized polymer/CNT composite, recently
few investigations have focused on the preparation and
design of hybrid fiber/CNT composites by developing
CNTs over fibers [8, 9]. The CNT coated fibers have poten-
tial to increase the thickness features of polymer-based
composites and to harden the matrix/fiber interface [10,
11]. The CNTs in multi-scale hybrid composites not only
can be grown directly over the fabric surface or fiber,
but also can be disseminated in the matrix. The CNTs
provide a potential to mend the thermal, electrical, and
mechanical properties of the base materials [12]. It has
been verified that the addition of a mere 1 wt.% of CNTs
into the material matrix can increase the stiffness of the
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466      A. Kausar and M. Siddiq: Epoxy/modified MWCNT-coated aramid fiber
subsequent composites by as much as 36–42% and their
tensile strength by 25% [13]. Furthermore, the existence
of CNTs in the host matrix may alleviate the various
downsides of traditional fiber composites, particularly
the interlaminar properties and longitudinal compres-
sion [14, 15].
Thermosetting polymer matrices have contributed
in fiber-integrated composites. In the thermosets, epoxy
resin is the imperative resin. Generally, thermoplastic
resins are amalgamated with epoxy resin to enhance the
toughness [16, 17]. Typically, it is problematic to achieve
homogeneous blends as intermolecular contacts are intri-
cate in thermosetting blends relative to linear polymer
blends. In recent times, several miscible epoxy blends
have been investigated such as the blend of epoxy and
polyethylene oxide (PEO). The epoxy/PEO blend was
found to be miscible on treatment with phthalic anhy-
dride (PA) and 4,4′-diaminodiphenylmethane (DDM).
In aromatic amine curative systems, the miscibility was
attributed to the formation of intermolecular hydrogen-
bonding interactions [18]. The methods of melt blend-
ing and slurry (solution) approaches have been used
for obtaining epoxy composites. Each of these methods
yields a different set of mechanical properties. A dis-
advantage of the slurry method is the requirement of
organic solvent for polymer solubilization, whereas the
melt method often suffers from poor filler dispersion. An
alternative technique is the use of infiltration to obtain
composites with fine matrix-reinforcement interaction.
Thermoset epoxy EPON Resin 862 (bisphenol F) and
a curing agent (3:1 by weight) were introduced into the
residue of a 1 wt.% nanocomposite after nitrogen gasifi-
cation at room temperature under vacuum. A two-stage
curing process is used to form epoxy/single-walled CNT
(SWCNT) composites at 80°C for 2  h up to 150°C for 2  h
[19]. In another attempt, epoxy-infiltrated hydroxyapatite
composites were prepared [20]. A monoglycidyl ether-
based epoxy resin and an Epodur 231 curing agent with
a 100:27.5 ratio (wt/wt) were used. The epoxy and the
hardener were mixed and heated to 60°C. Afterwards, the
mixture was poured into a mold, permitting the immer-
sion of hydroxyapatite pieces. Composites reinforced
with epoxy aramid fibers have been reported to cure in
an autoclave, under a pressure of 0.69 MPa, following a
heating cycle of up to 181°C [21]. Epoxy hybrids reinforced
with CNTs and aramid fibers have been produced. The
thermoplastic nanocomposites were packed by CNTs, and
the films of the nanocomposites were casted by CNT dis-
persion. The epoxy resin was thermally treated up to the
melting point of the thermoplastic resin. The resin was
permeated into preformed fibers, and the nanocomposite
film was liquefied by means of the epoxy resin. The
CNT particles were distributed in the sections between
the aramid fibers. Finally, the epoxy resin was treated
and the hybrid CNT/aramid fiber composite was manu-
factured. In this study, multi-walled carbon nanotubes
were first functionalized with carboxylic acid (MWCNT-
COOH) and then with poly(ethylene glycol) methyl ether
(MWCNT-PEGME). The latter was adopted as the ther-
moplastic polymer because CNTs are known to disperse
well in PEGME and to become miscible with the epoxy.
Furthermore, the PEGME may reduce the processing tem-
perature and time, which has become the current focus in
the aerospace industry [22]. The aramid fibers were then
coated with the homogeneous dispersion of MWCNT-
PEGME using electrophoresis. Finally, the epoxy/aramid-
MWCNT-PEGME composites were prepared. The epoxy/
aramid-MWCNT-PEGME hybrid composites consisted of
four components, namely, aramid fibers, carbon nano-
tubes, PEGME, and epoxy resin. Thermal and morpholog-
ical characterization of the composites were performed to
confirm the dispersion state of MWCNTs via differential
scanning calorimetry (DSC) and field emission scanning
electron microscopy (FESEM).
2 Materials and methods
2.1 Materials
4,4′-Diaminodiphenylmethane ( ≥ 97.0%), poly(ethylene
glycol) methyl ether (average Mn~550), and MWCNTs
(O.D. × L 6-9 nm × 5 μm,  > 95% (carbon)) were purchased
from Aldrich (St. Louis, USA). The epoxy resin selected
in this study was diglycidyl ether of bisphenol A (DGEBA,
YD-128), with an epoxide equivalent weight of 185–190.
2.2 Acid functionalization and PEGME
­modification of MWCNTs (MWCNT-COOH
and MWCNT-PEGME)
Pristine MWCNTs were first functionalized using a mixture
of 8 mol/l of sulfuric acid and 5 mol/l of nitric acid (3:1,
respectively). The mixture was refluxed and sonicated at
70°C for 6 h [23]. One gram of functionalized MWCNTs was
dispersed in ethanol through sonication for 2 h, and then
1 g of PEGME was added. The mixture was sonicated for
1 h at 100°C and then kept in a vacuum oven for 12 h to
remove the ethanol.
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2.3 P
 reparation of modified MWCNT–coated unmodified fibers were also prepared using the same
aramid fibers by electrophoresis technique. Sample designations used are given in Table 1.

Because of the ability of MWCNTs to respond to an elec-

tric field, electrophoresis was used as a simple technique
2.5 Experimental methods
for the deposition of nanotubes on the surface of aramid
fibers [24]. PEGME-MWCNTs were deposited uniformly on
Field emission scanning electron microscopy (FE-SEM)
the surface of aramid fibers from aqueous nanotube dis-
was performed using JSM5910 (JEOL Ltd., Tokyo, Japan).
persions when a DC potential was applied between the
SEM was used to examine the freeze-fractured samples.
aramid fibers and the counter electrode. Because of the
First, the samples were completely submersed in liquid
negative charge, the MWCNTs migrated towards the posi-
nitrogen for several minutes. Then the frozen specimens
tive aramid fiber electrode and were subsequently depos-
were fractured, fixed in a holder, and coated with carbon
ited on the fiber surface [25, 26]. Forty weight percent of
for SEM analysis. Transmission electron microscopy
aqueous nanotube dispersion was deposited uniformly on
(TEM) was performed using a LEO 912 Omega instrument
the surface of the aramid fibers. The weight percent of the
(Zürich, Switzerland) at 120 kV. Ultrathin sections were
CNT solution was taken to be constant each time for elec-
prepared at 60°C with an Ultracut E ultramicrotome using
trophoresis to ensure the uniform coating of nanotubes on
a diamond knife. Differential scanning calorimetry (DSC)
the fibers. Figure 1 shows the deposition of the nanotubes
was performed using a METTLER TOLEDO DSC 822 instru-
on the surface of the aramid fibers via electrophoresis [27].
ment (Columbus, USA). Five-milligram samples were
encapsulated in aluminum pans and heated at a rate of
2.4 P
 reparation of the epoxy and aramid- 10°C/min under a nitrogen atmosphere. The tensile and
MWCNT-PEGME fiber composites flexural testing processes were carried out using a WP 310
universal material tester (Schleswig-Holstein, Germany).
To prepare the epoxy and aramid-MWCNT-PEGME hybrid For the tensile test, the molds were made according to
composites, the aramid fibers were placed in a Petri dish. ASTM D638, with the following dimensions: width 11 mm,
The mixture of the epoxy resin and the curing agent was thickness 6 mm, and length 60 mm. For the flexural test,
poured on the modified fibers (3:1 by weight). The mixture
was heated up to 100°C and smoothly shaken to allow
the aramid-MWCNT-PEGME fibers to interact with the
epoxy. Finally, the Petri dish was kept in a vacuum oven
to cure the resin at 80°C for 4 h. The schematic formation
of MWCNT-coated aramid fibers and epoxy composites is
shown in Figure 2. Epoxy/aramid fiber composites using

Figure 1: Deposition of carbon nanotubes on the fiber surface by Figure 2: Formation of MWCNT-coated aramid fibers and epoxy
electrophoresis. composites.

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Table 1: Sample designations used.

Sample code   Sample   Fiber content (wt.%)

MWCNT-PEGME   Poly(ethylene glycol) methyl ether-functionalized multi-   –

walled carbon nanotube
Aramid-MWCNT-PEGME   Poly(ethylene glycol) methyl ether-functionalized multi-   40 wt.% CNTs coated on 10 g of fibers
walled carbon nanotube-coated aramid fibers
Epoxy/aramid-MWCNT-PEGME 10  Epoxy and poly(ethylene glycol) methyl ether-functionalized   10
multi-walled carbon nanotube-coated aramid fibers
Epoxy/aramid-MWCNT-PEGME 20  Epoxy and poly(ethylene glycol) methyl ether-functionalized   20
multi-walled carbon nanotube-coated aramid fibers
Epoxy/aramid-MWCNT-PEGME 30  Epoxy and poly(ethylene glycol) methyl ether-functionalized   30
multi-walled carbon nanotube-coated aramid fibers
Epoxy/aramid-MWCNT-PEGME 40  Epoxy and poly(ethylene glycol) methyl ether-functionalized   40
multi-walled carbon nanotube-coated aramid fibers
Epoxy/aramid 10   Epoxy and unmodified aramid fibers   10
Epoxy/aramid 20   Epoxy and unmodified aramid fibers   20
Epoxy/aramid 30   Epoxy and unmodified aramid fibers   30
Epoxy/aramid 40   Epoxy and unmodified aramid fibers   40

the mold was made according to ASTM D790. The speci- 1200
men dimensions were as follows: length 125 mm, width 13
mm, and thickness 3 mm. For both the tensile test and the 1000
flexural test, a cross-head speed of 1 mm/min was used.
Tensile strength (MPa)

800

3 Results and discussion

600

400

3.1 Tensile strength and modulus 200

The addition of modified nanotube-coated aramid fibers

to the matrix may significantly improve the composite 0 10 20 30 40
mechanical properties. The tensile properties are an impor- Filler content (wt.%)

tant indicator of the composite mechanical properties. The

improvement in tensile properties may be attributed to the
formation of a better interface structure that allows the
stress transfer from the matrix to the reinforcement [28].
Figure 3 shows the improvement in the mechanical proper-
ties of modified CNT-coated aramid fiber-reinforced epoxy
composites. The figure shows a comparison of the proper-
ties of epoxy/aramid-MWCNT-PEGME 10, epoxy/aramid-
MWCNT-PEGME 20, epoxy/aramid-MWCNT-PEGME 30, and
epoxy/aramid-MWCNT-PEGME 40 composites. The tensile
strength increased from 658 to 1198 MPa. In the compos-
ites, different reinforcements caused dissimilar tensile
properties. As can be seen in the figure, the lowest tensile
strength was found for neat epoxy at 658 MPa. The epoxy/
aramid-MWCNT-PEGME 10 showed a tensile strength of
697 MPa; the epoxy/aramid-MWCNT-PEGME 20, around
999 MPa; and the epoxy/aramid-MWCNT-PEGME 30,
1030 MPa. The tensile strength was found to be higher for
Figure 3: Comparison of the tensile strength of epoxy/aramid-
MWCNT-PEGME composites.
the epoxy/aramid-MWCNT-PEGME 40, which was around
1198 MPa. Literature studies have shown that even very
low loadings of nanotubes may result in beneficial effects
on the tensile strength of fiber-reinforced epoxy compos-
ites [29, 30]. Figure 4 shows a comparison of the tensile
modulus of epoxy/aramid-MWCNT-PEGME composites.
This study shows that the tensile modulus increased from
62 GPa (neat resin) to 96 GPa in the epoxy/aramid-MWCNT-
PEGME 10 composite and to 180 GPa in the epoxy/aramid-
MWCNT-PEGME 40 composite. The tensile modulus was
found to be comparable to that found in the literature for
fabricated epoxy/glass-fiber composites [31]. To assess the
results, epoxy/aramid fiber composites using unmodified
fibers were also studied. In this series, the tensile strength

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 A. Kausar and M. Siddiq: Epoxy/modified MWCNT-coated aramid fiber      469

200 the highest flexural strength, whereas the epoxy/aramid-

180
MWCNT-PEGME 10–30 composites exhibited a lower
strength. The maximum flexural strength for the epoxy/
160
aramid-MWCNT-PEGME 40 composite was 1593  MPa,
Tensile modulus (GPa)

140
whereas that for the epoxy/aramid-MWCNT-PEGME 30 was
120 1525 MPa. The improved performance may be attributed
100 to the enhanced interfacial adhesion between the matrix
80 and the fibers. The epoxy/aramid-MWCNT-PEGME 20 and
60 epoxy/aramid-MWCNT-PEGME 10 composites showed a
40
relatively lower flexural strength of 1470 and 1338 MPa,
respectively. In contrast, neat resin showed the lowest flex-
20
ural strength of 1158 MPa. Here, the fiber-matrix adhesion
0 10 20 30 40 and stress transfer at the interface are important param-
Filler content (wt.%) eters influencing the flexural properties of fiber-reinforced
composites [32, 33]. In the series of epoxy and unmodified
Figure 4: Comparison of the tensile modulus of epoxy/aramid-
MWCNT-PEGME composites. aramid fiber, the flexural strength of all the composites was
lower relative to that of the modified fiber series. Epoxy/
aramid 10, epoxy/aramid 20, epoxy/aramid 30, and epoxy/
aramid 40 had a flexural strength of 1298, 1320, 1395, and
increased from 422 to 888 MPa. Moreover, the modulus
1412 MPa, respectively. Here, the epoxy/aramid 40 com-
increase was in the range of 34–89  GPa. The increase in
posite again had the highest flexural strength among the
the tensile strength and modulus was less pronounced
unmodified fiber series; however, the value was lower than
as compared to that of the modified fiber series. The
that of the functional series.
results indicated that the coating of the modified MWCNTs
may ­significantly improve the tensile properties of the
composites.
3.3 Fracture surface analysis

The tensile fracture surface of the tested specimens was

3.2 Flexural properties
examined using SEM (Figure 6). In order to examine the
failure mechanism of the composites, the micrographs
The flexural strength of the composites is shown in Figure 5.
of epoxy/aramid-MWCNT-PEGME 10 (Figure 6A), epoxy/
The flexural strength of the epoxy/aramid-MWCNT-PEGME
aramid-MWCNT-PEGME 30 (Figure 6B), and epoxy/ara-
composites was found to be a function of filler content.
mid-MWCNT-PEGME 40 (Figure 6C and D) are presented.
The epoxy/aramid-MWCNT-PEGME 40 composite showed
The micrographs show that the fiber filaments were fully
covered with the epoxy resin. As can be seen clearly in the
1800 figure, there was no separation of the fibers from the matrix
1600
owing to the fine interaction between the components. In
Figure 6A–C, there were very few fibers where the pull-out
1400
phenomenon was observed. Interface debonding, matrix
Flexural strength (MPa)

1200 cracking, or interlaminar delaminations were not observed

1000 either. For comparison purposes, the micrograph for neat
800
epoxy is presented in Figure 6F. Pure epoxy showed a gyroid-
type morphology with fewer pores in the structure. To study
600
the interfacial interaction between the epoxy and the fibers,
400 a higher resolution image of epoxy/aramid-MWCNT-PEGME
200 40 was made at 20 μm, which provided some interest-
ing information about the matrix/fiber bonding. A strong
0 10 20 30 40 adhesion was observed at the interface that encapsulated
Filler content (wt.%)
the fibers in the matrix, which caused a strong bonding. At
Figure 5: Comparison of the flexural strength of epoxy/aramid- higher resolution (Figure 6E), micro-cavities were observed
MWCNT-PEGME composites. due to fiber pull out. The occurrence of smaller arches

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470      A. Kausar and M. Siddiq: Epoxy/modified MWCNT-coated aramid fiber

A B

200 µm 200 µm

C D

200 µm 200 µm

E F

20 µm 2 µm

Figure 6: FESEM images of (A) epoxy/aramid-MWCNT-PEGME 10, (B) epoxy/aramid-MWCNT-PEGME 30, (C) epoxy/aramid-MWCNT-PEGME
40, (D) epoxy/aramid-MWCNT-PEGME 40, and (E) epoxy/aramid-MWCNT-PEGME 40 at 20 μm, and (F) neat epoxy at 2 μm.

means that the interfacial bonding between the fiber and
the matrix was strong, which could provide an efficient
stress transfer from the matrix. This caused an improvement
in the mechanical properties of the composites.
3.4 DSC study
To investigate the effects of loading of aramid fibers coated
with modified MWCNTs on the thermal properties of
epoxy resin, thermal analysis was performed using DSC.
Figure 7 shows that the Tg value of neat epoxy was 162°C,
whereas for varying weight percentages of reinforced (10,
20, 30, and 40 wt.%) composites the Tg value was 164°C,
168°C, 170°C, and 173°C, respectively. The higher values of
Tg may be attributed to the introduction of MWCNT-coated
aramid fibers, which interacted with the matrix to restrict
the mobility of the epoxy network. Hence, the matrix-filler
interaction between MWCNT-coated fibers and epoxy
caused a chain confinement. The Tg value of the unmodi-
fied epoxy/aramid composites was found to be relatively
lower, in the range of 163–165°C. Moreover, electrophoresis
was found to be an efficient technique for forming MWCNT-
coated aramid fibers for use as a reinforcement [34].
4 Conclusions
The purpose of the current research was to determine
whether electrophoresis is an efficient method for coating
aramid fibers homogeneously with modified nanotubes.

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 A. Kausar and M. Siddiq: Epoxy/modified MWCNT-coated aramid fiber      471
1 Epoxy
Epoxy/Aramid-MWCNT-PEGME 40
0 [5] Zhu J, Imam A, Crane R, Lozano K, Khabashesku VN, Barrera EV.
Heat flow (Exo)
-1
-2
-3
-4
50 100 150 200
Temperature (°C)
Figure 7: DSC thermograms of epoxy/aramid-MWCNT-PEGME at
10°C/min in N2.
Reinforcement with modified aramid-MWCNT-PEGME
fibers made it possible to tailor the mechanical proper-
ties of novel epoxy composites by means of selective
content. In order to completely inject the epoxy resin into
the aramid fibers, PEGME-MWCNTs were coated over the
fiber surface via electrophoresis. In this way, it was pos-
sible to distribute the nanotubes in the desired region
between the fibers. FESEM observation indicated that the
composites have a fine matrix-filler interaction, with least
fiber pull-out phenomenon. The epoxy/aramid-MWCNT-
PEGME 40 composite showed superior mechanical prop-
erties compared with the other composites. The difference
in the property was significant compared with the neat
epoxy as well as with the composites with lower loading
level. Epoxy/aramid fiber composites were also pre-
pared using unmodified fibers, and the tensile strength,
modulus, flexural strength, and Tg were studied. The prop-
erties were found to be lower than those for the epoxy/
aramid-MWCNT-PEGME composites. The manufacture of
novel high-performance multi-scale hybrid composites is
particularly important to achieve advanced engineering
applications.
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