Composites: Part A 41 (2010) 215221

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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa

Enhanced thermal conductivity of epoxy nanocomposites lled with hybrid

ller system of triethylenetetramine-functionalized multi-walled carbon
nanotube/silane-modied nano-sized silicon carbide
Kai Yang *, Mingyuan Gu
State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240, China

a r t i c l e

i n f o

Article history:
Received 5 May 2009
Received in revised form 23 October 2009
Accepted 23 October 2009

Keywords:
A. Polymermatrix composites
B. Thermal properties
D. Thermal analysis
E. Surface treatments

a b s t r a c t
Multi-walled carbon nanotubes (MWCNTs) were rst treated by a 3:1 (v/v) mixture of concentrated
H2SO4/HNO3, and then triethylenetetramine (TETA) grafting was carried out. Nano-sized silicon carbide
particles (SiCnp) were modied by the silane coupling agent. Epoxy nanocomposites lled with hybrid ller system containing TETA-functionalized MWCNTs and silane-modied SiCnp were prepared. The investigation on the thermal conductivity of epoxy nanocomposites lled with single ller system and hybrid
ller system was performed. Chemical surface treatment is conducive to the enhancement of thermal
conductivity of epoxy composites. The thermal conductivity of epoxy composites with hybrid ller system is higher than that of epoxy composites with any single ller system (functionalized MWCNTs or
modied SiCnp), which is due to the effective combination of MWCNT-to-MWCNT and SiCnp-to-SiCnp
conductive networks. Hybrid ller system could provide synergistic effect and cost reduction
simultaneously.
2009 Elsevier Ltd. All rights reserved.

1. Introduction
The development of polymer composites with nanoscaled
modiers has become an attractive new subject in materials science. The thermal conductivity of polymer composites is an
important material property for many applications [15]. Due
to the fact that most polymers show a rather low thermal conductivity, the introduction of conductive llers is an effective
method to enhance the thermal transport of polymer-based composites. Carbon nanotubes (CNTs) are considered to be a type of
very attractive ller for the improvement of thermal transport
property of polymer composites because of their extremely high
thermal conductivity (about 6000 W/mK for single-walled CNTs
(SWCNTs) [6] and about 3000 W/mK for multi-walled CNTs
(MWCNTs) [7]). According to this, a certain enhancement of the
thermal conductivity of polymer-based nanocomposites by an
incorporation of CNTs can be expected and have also been reported for CNT/polymer nanocomposites [812]. However, the
potential application of CNTs is hindered by manipulation difculties owing to their insolubility and poor dispersion in polymeric matrices [13,14]. In order to optimize the thermal
conduction of polymer-based CNT nanocomposites, it is essential
to modify the sidewalls of CNTs by chemical functionalization
* Corresponding author. Fax: +86 021 62822012.
E-mail address: kyang_80@yahoo.com.cn (K. Yang).
1359-835X/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2009.10.019

[15,16]. The thermal resistance of the interface, also called the

Kapitza resistance (RK), represents a barrier to the heat ow associated with the differences in the phonon spectra of the two
phases and possible weak contact at the interface. These lead
to backscattering of thermal energy waves (phonons). The thermal resistance to heat transfer through an interface becomes
important when the high conductivity inclusions are small in
size, and their surface to volume ratio is high. The case of polymer-based CNT nanocomposites falls in this category. Acoustic
phonon mismatch and weak bonding between various polymeric
matrix materials and unfunctionalized nanotube walls can be addressed by introducing a better developed interfacial bonding
(such as covalent bonding) between the CNTs and the polymer
matrix, which can be engineered by chemical functionalization
process. Moreover, chemical functionalization is benecial to
the dispersion of CNTs and facilitates the formation of CNT network. Therefore, chemical functionalization greatly contributes
to the thermal conduction improvement of CNT/polymer
nanocomposites.
Theoretically, the thermal resistance is caused by phonon
scattering [17]. Polymer composites with high thermal conductivities can be obtained by the addition of llers with high intrinsic thermal conductivity. However, as discussed by Bigg [18],
when the intrinsic thermal conductivity of the ller is 100 times
greater than that of the polymer matrix (typical thermal
conductivity values of polymers are 0.20.4 W/mk), there is no

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K. Yang, M. Gu / Composites: Part A 41 (2010) 215221

remarkable improvement in the thermal conductivities of polymer composites. Obtained thermal conductivity values by experiments are much lower than those estimated by a rule of mixture
approach. On the contrary, the aspect ratio of the ller is a more
important parameter dictating the thermal conductivity of a
composite, because the llers with large aspect ratios easily form
the bridges between them, known as conductive network. At this
time, conductive networks from llers will be more important for
the thermal conductivities of polymer composites. The formation
of random bridges or networks from conductive llers facilitates
phonon transfer leading to high thermal conductivities. CNTs
possess the large aspect ratios and easily form the bridges or networks. The tube-to-tube networks facilitate phonon transfer
leading to high thermal conductivities of polymer composites.
Bonnet et al. [19] have reported that the thermal conductivity
of SWCNT/PMMA composites is dominated by the SWCNT network contribution. Thick MWCNTs with a high aspect ratio are
suggested to be the most favorable type of nanotube for an
enhancement of a polymer composites thermal conductivity
[20]. On the other hand, the large nanotube volume fraction
may cause some problems, such as the agglomeration of nanotubes, the increase of composite melt viscosity and the corresponding mechanical performance degradation. This means that
hybrid ller system with large formation of conductive networks
is signicant for the fabrication of the next generation heat dissipation materials.
In this current study, we report the effectiveness of hybrid ller system consisting of triethylenetetramine (TETA)-functionalized MWCNTs and silane-modied nano-sized silicon carbide
particles (SiCnp) on the preparation of thermally conductive
epoxy nanocomposites. We attempt to efciently make tube-totube and particle-to-particle networks be combined to optimize
thermally conductive paths. In order to establish the comparison,
we also study the thermal conductivity of epoxy nanocomposites
lled with single ller system (functionalized MWCNTs or modied SiCnp). Additionally, unfunctionalized MWCNTs and unmodied SiCnp are also investigated in order to evaluate the effect of
the surface modication. Chemical surface treatment of the llers
would improve the interfacial interaction, which is conducive to
good wettability and homogeneous dispersion. Interfacial thermal resistance is closely correlated with the differences in the
phonon spectra of llers and epoxy matrix. Heat transport along
isolated MWCNTs occurs by phonons with a wide range of
frequencies; in MWCNT/epoxy nanocomposites, this requires
phonon transfer from tube to tube via the epoxy [7]. Due to
the difference in stiffness, the MWCNTs and the epoxy matrix
are coupled by only a small number of low-frequency vibrational
phonon modes in the absence of covalent bonds at the interface.
Accordingly, thermal energy contained in high-frequency phonon
modes within the nanotubes must rst be transferred to lowfrequency phonons through phononphonon couplings before
being exchanged with the surrounding medium. This is the origin
of the high interfacial thermal resistance in MWCNT/epoxy
nanocomposites [21]. The similar mechanism is also indicated
for the interface between SiCnp and epoxy matrix. Therefore,
the goal of chemical surface modication is to introduce the
covalent bonds at the interfaces between the llers and epoxy
matrix. This is very benecial to the improvement of llermatrix interfacial interaction. Simultaneously, it can enhance the
wettability of the llers and facilitate their good dispersion.
Homogeneous dispersion is a positive factor to form combined
MWCNT-to-MWCNT and SiCnp-to-SiCnp conductive networks.
More effective llerller thermal conduction in the case of good
dispersion state is conducive to the enhancement of thermal conductivity of epoxy nanocomposites (llermatrixller transfer

would result in a higher thermal resistance than llerller

transfer).
2. Experimental
2.1. Materials
As-received MWCNTs used in this study were obtained from the
Nanotech Port Company, Shenzhen, China. The MWCNTs synthesized by the chemical vapor deposition (CVD) had the diameter of
4080 nm and the length of 515 lm. The purity of MWCNTs is
98%. The thermal conductivity of raw MWCNTs was reported to be
2000 W/mK (the data was supplied by the Nanotech Port Company).
SiCnp with an average particle size of 50 nm was obtained from Karl
Company and its thermal conductivity was 120 W/mK (the data was
supplied by Karl Company). Epoxy resin utilized in this work was a
nominally difunctional epoxy resin, bisphenol-A glycidol ether
epoxy resin (DGEBA). The curing agent was 2-ethyl-4-methylimidazole (EMI-2,4). MWCNTs were rst treated by a 3:1 (v/v) mixture
of concentrated H2SO4/HNO3 (the reason for applying this kind of
acid treatment method has been elaborated in our previous research
work [22]), and then TETA grafting was carried out (shown in
Fig. 1a). SiCnp was modied by the silane coupling agent, c-aminopropyl-triethoxysilane (NH2CH2CH2CH2Si(OC2H5)3). The detailed
process can be presented in Fig. 1b. TETA-functionalized MWCNTs
and silane-modied SiCnp were washed with acetone many times
and subsequently dried in a vacuum oven for 1 day.
2.2. Preparation of epoxy nanocomposites
Functionalized MWCNTs and modied SiCnp were dispersed in
chloroform and sonicated for 1 h (0.0112 g of total solids
(MWCNTs + SiCnp), dispersed in 44.52 g of chloroform during the
1 h sonication for 5% ller volume fraction; 0.0374 g of total solids
(MWCNTs + SiCnp), dispersed in 66.78 g of chloroform during the
1 h sonication for 10% ller volume fraction; 0.0644 g of total solids
(MWCNTs + SiCnp), dispersed in 89.04 g of chloroform during the
1 h sonication for 15% ller volume fraction; 0.0929 g of total solids
(MWCNTs + SiCnp), dispersed in 111.30 g of chloroform during the
1 h sonication for 20% ller volume fraction; 0.1191 g of total solids
(MWCNTs + SiCnp), dispersed in 133.56 g of chloroform during the
1 h sonication for 25% ller volume fraction; 0.1543 g of total solids
(MWCNTs + SiCnp), dispersed in 155.82 g of chloroform during the
1 h sonication for 30% ller volume fraction). The dispersion was
mixed with DGEBA and the volume ratio of DGEBA to MWCNT to
SiCnp was adjusted for the different contents of MWCNTs and SiCnp
(volume fraction ratio of MWCNTs to SiCnp was 1:1). The mixture
was sonicated and stirred for homogenization at 60 C. This treatment increased the viscosity of the dispersion, which in turn limited the respective aggregations of MWCNTs and SiCnp.
Subsequently, the mixture was treated by a post heating at 90 C
in order to completely remove the solvent. And then, the mixture
was kept in a vacuum oven for 24 h to get rid of air bubbles. After
adding the curing agent (EMI-2,4), the mixture was stirred by using
a magnetic bar for 30 min under sonication. Finally, the mixture
was poured into a mold and the whole system was placed in an
oven. The epoxy/MWCNT/SiCnp compound was precured at 70 C
for 1 h, cured at 110 C for 1.5 h and postcured at 140 C for
1.5 h. The similar preparation process was applied to epoxy composites with any single ller system (functionalized MWCNTs or
modied SiCnp). In addition, Unfunctionalized MWCNTs and
unmodied SiCnp were also used to prepare epoxy nanocomposites
for the comparison of thermal conductivity so as to show the inuence of chemical surface treatment. The ller volume fractions can
be listed in Table 1.

K. Yang, M. Gu / Composites: Part A 41 (2010) 215221

Fig. 1. (a) Scheme for the process of grafting TETA onto the MWCNT and (b) scheme for chemical modication of SiCnp.

217

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K. Yang, M. Gu / Composites: Part A 41 (2010) 215221

Table 1
The ller volume fractions of epoxy nanocomposites lled with different types of
llers.
Systems

Filler volume fractions (%)

Epoxy nanocomposites with

hybrid ller system
TETA-functionalized MWCNT/
epoxy nanocomposites
As-received MWCNT/epoxy
nanocomposites
Silane-modied SiCnp/epoxy
nanocomposites
Unmodied SiCnp/epoxy
nanocomposites

0, 5, 10, 15, 20, 25, 30 (Vfunctionalized

MWCNTs:Vmodied SiCnp = 1:1)
0, 5, 10, 15, 20, 25, 30

used to coat the fracture surface of the sample for better observation. Thermal conductivity measurement was conducted by
employing ASTM E1225-87, which was based on temperature difference between reference and specimens at steady state and room
temperature. A minimum of four individual measurements was
performed on bulk specimens. The detailed information about
these measurements (ASTM E1225-87) can be referred in Ref. [23].

0, 5, 10, 15, 20, 25, 30

0, 5, 10, 15, 20, 25, 30

3. Results and discussion

0, 5, 10, 15, 20, 25, 30

MWCNTs and SiCnp were dispersed in chloroform and the corresponding dispersions were placed for 72 h to check the ller dispersibility. The functionalized MWCNTs usually present better
dispersion in solvents. A stable dispersion was obtained in the case
of TETA-functionalized MWCNTs when equal amounts of as-received MWCNTs and TETA-functionalized MWCNTs were respectively added to the same volume of chloroform and mechanically
mixed (shown in Fig. 2a). With respect to untreated SiCnp and treated SiCnp by silane coupler, the similar phenomenon could be observed (exhibited in Fig. 2c). Moreover, the surface analytical
characterization of the llers was carried out. The XPS survey spectra (revealed in Fig. 2b) of as-received MWCNTs and TETA-functionalized MWCNTs were recorded to identify the chemical
composition of the surfaces. All the spectra exhibit C 1s and O 1s
peaks, whereas the XPS spectrum of TETA-functionalized MWCNTs
shows the remarkable intensication of O 1s peak. The reason for
this phenomenon could be attributed to the great effect of
H2SO4/HNO3 treatment on the MWCNT surface. Additionally, a N
1s peak is also found in this spectrum, which indicates that TETA
has been successfully grafted onto the MWCNT surface. The FT-IR
spectra of unmodied and modied SiCnp are displayed in
Fig. 2d. The bands at 930.45 cm 1 and 1101.03 cm 1 are found in

2.3. Instrumental analysis

X-ray photo-emission spectroscopy (XPS) analysis was executed in an ultra high vacuum system equipped with a Kratos AXIS
Ultra hemispherical electron analyzer, using a monochromated Al
Ka source (1486.6 eV), at a base pressure of 2  10 10 mbar. The
Fourier transform infrared spectroscopy (FT-IR) experiments were
recorded between 400 and 4000 cm 1 using a Bruker EQUINOX 55
FT-IR spectrometer. Transmission electron microscopy (TEM) and
high-resolution TEM (HRTEM) images were taken on JEM 2100F
to characterize the microstructures of MWCNTs and SiCnp
(MWCNTs and SiCnp were respectively dispersed in chloroform
and sonicated for 30 min. And then, the corresponding dispersions
were separately dropped onto the copper grids coated with ultrathin carbon lms for further observation). The fracture surface of
epoxy nanocomposite lled with hybrid ller system was observed
by a eld emission scanning electron microscope (FESEM) (FEI
SIRION 200, USA). Conventional gold sputtering technique was

Fig. 2. (a) Photograph of as-received MWCNTs (marked with 1) and TETA-functionalized MWCNTs (marked with 2) dispersed in chloroform and wait for 72 h; (b) XPS
survey spectra of as-received MWCNTs and TETA-functionalized MWCNTs; (c) photograph of untreated SiCnp (marked with 1) and silane-treated SiCnp (marked with 2)
dispersed in chloroform and wait for 72 h; (d) FT-IR spectra of untreated SiCnp and treated SiCnp by silane coupler.

K. Yang, M. Gu / Composites: Part A 41 (2010) 215221

these spectra. The former could be assigned to the SiC characteristic absorption peaks and the latter to the SiO antisymmetric
stretching vibrations, which denotes that the surface of unmodied
SiCnp has been partly oxidized in the ller manufacture. The band
at 474.86 cm 1 could be assigned to the SiO bending vibrations.
In the FT-IR spectrum of unmodied SiCnp, the intensity of the peak
at 930.45 cm 1 (SiC bonds) is greater than that of the peak at
1101.03 cm 1 (SiO bonds). However, in the spectrum of modied
SiCnp, the latter is greater and CH2 characteristic absorption peaks
(the wavenumbers at 28302960 cm 1) are remarkable, which
indicates that more SiOSi bonds appear in the surface of SiCnp
and a coating of silane coupler has been formed.
The microstructures of an as-received MWCNT and a TETAfunctionalized MWCNT were further characterized by HRTEM. In
Fig. 3a, the tube wall of the as-received MWCNT is rather smooth.
However, in Fig. 3b, the surface of the TETA-functionalized
MWCNT is rather rough, which could be due to a TETA layer
formed on its tube wall. Fig. 3c shows the TEM image of silanemodied SiCnp.
Optimization of the epoxy-ller interfacial interaction is
signicant for the enhancement of thermal transport of epoxy
composites. Fig. 4 reveals the thermal conductivity of epoxy nanocomposites lled with different types of llers (error bars are also
shown in Fig. 4). It can be observed that the thermal conductivities
of silane-modied SiCnp/epoxy composites are larger than those of
unmodied SiCnp/epoxy composites. Silane coupler treatment
could bridge the connection of SiCnp to the epoxy matrix and decrease the resistance to the heat ow caused by epoxySiCnp interface. TETA functionalization would make tube carbon atoms be
covalently attached to matrix molecules. These carbon atoms will
therefore act as scattering centers for the heat carrying wave packages (phonons) and reduce tube thermal conductivity. In addition,
H2SO4/HNO3 treatment would shorten the length of MWCNTs, and
thus the aspect ratio would decrease. These factors are adverse to
the enhancement of thermal conductivity of MWCNT/epoxy composites. However, it can be clearly seen that with respect to different nanotube volume fraction, the thermal conductivities of TETAfunctionalized MWCNT/epoxy composites are larger than those of
as-received MWCNT/epoxy composites. The phenomenon denotes
that TETA functionalization improves the interfacial heat transport
between the epoxy matrix and the MWCNTs and facilitates better
dispersion of MWCNTs in the matrix, which is benecial to the
enhancement of the thermal conductivity of MWCNT/epoxy composites. Therefore, in the case of single ller system, chemical surface treatment contributes to the improvement of the thermal
conduction property of epoxy nanocomposites. It is due to increasing wettability and dispersion of nano-llers in epoxy matrix.
With regard to the single ller system, there is another similar
phenomenon that large ller volume fraction may lead to the decrease of the thermal conductivity of epoxy composites due to
the formation of large agglomerates (when ller volume fraction
is large, the viscosity of the composite (pre-curing) is massive
and the mixing is very difcult. Therefore, large agglomerates easily form. In the consolidation of the composite, voids or air pockets
would exist in these large agglomerates and lead to lower thermal
conductivity of the composite). This phenomenon would be more
remarkable in the composites lled with nano-structured llers
because these inclusions are small in size and their surface-to-volume ratios are high. In an attempt to simultaneously obtain high
thermal conductivity and prevent the appearance of large agglomerates, we applied hybrid ller system to epoxy composites. Hybrid
ller system could mitigate large agglomerates. On the one hand,
the application of hybrid ller system relatively decreases the content of functionalized MWCNTs. On the other hand, the spherical
modied SiCnp is lled in the brous MWCNT-to-MWCNT network,
which indicates that the space formed in MWCNT-to-MWCNT net-

219

Fig. 3. (a) HRTEM image of an as-received MWCNT; (b) HRTEM image of a TETAfunctionalized MWCNT; (c) TEM image of silane-modied SiCnp.

work can be fully used. Consequently, the hybrid ller system

would lower the viscosity of the composite (pre-curing) and correspondingly lessen the phenomenon of large agglomerates. The

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K. Yang, M. Gu / Composites: Part A 41 (2010) 215221

Fig. 4. Thermal conductivity of epoxy nanocomposites lled with different types of llers.

thermal conductivity of epoxy nanocomposites containing

MWCNTSiCnp hybrid ller system (volume fraction ratio of
MWCNTs to SiCnp was 1:1 and the two kinds of llers were chemically modied, respectively) is shown in Fig. 4. The thermal conductivities of epoxy composites with hybrid ller system are
higher than those of epoxy composites with any single ller system. Moreover, when ller volume fraction exceeds 20%, the thermal conductivity of epoxy composites lled with chemically
modied MWCNTs and SiCnp still increases (in the case of single ller system, thermal conductivity of epoxy nanocomposites decreases as ller volume fraction is greater than 20%). Thus, the
effectiveness of hybrid ller system is well revealed. In addition,
when hybrid ller volume fraction is 30%, the thermal conductivity
of epoxy composite is about 2 W/mK. Only MWCNTs are added (ller volume fraction is 20%), the corresponding thermal conductivities are lower than 1.6 W/mK. The thermal conductivity of asreceived MWCNTs is 2000 W/mK and that of TETA-functionalized
MWCNTs should be lower than 2000 W/mK. Heat transport in
nanotube/epoxy nanocomposites will be limited by the interfacial
thermal resistance between nanotubes and epoxy matrix and the
thermal resistance at nanotube/nanotube junctions. The thermal
conductivity of 2000 W/mK is the longitudinal thermal conductivity of MWCNTs. The MWCNT network contribution is dominated
by transverse heat transport as well as by nanotube/nanotube or
bundle/bundle transfer which occurs with a high thermal resistance. Therefore, the obtained thermal conductivity values in the
experiments are much lower than those estimated with the thermal conductivity of 2000 W/mK and the corresponding ller volume fractions.
The efcient application of hybrid ller system in the thermal
transport of epoxy composites is due to enhanced conductive network induced by hybrid shape llers. The improved dispersion of
hybrid ller can be obtained due to altered interparticle interactions [24,25]. MWCNT-to-MWCNT and SiCnp-to-SiCnp networks
are well combined to generate the synergistic effect of hybrid ller.
The scheme for epoxy nanocomposites lled with hybrid ller system is shown in Fig. 5. Considering relatively low thermal conductivity of structuring ller (SiCnp) compared to MWCNTs, higher
thermal conductivity of epoxy composites containing hybrid ller
successfully demonstrates the usefulness of the concept of synergistic effect of hybrid ller in enhancing the thermal conductivity
of the composites for given ller loading. It can be inferred that
the conducting path or network is the most signicant factor over
the intrinsic conductivity of llers and loading concentration. In
brief, MWCNTs is the best candidate as a nano-ller in thermally
conductive composites. Additionally, hybrid ller system is more

Fig. 5. Scheme for epoxy nanocomposites lled with hybrid ller system.

Fig. 6. FESEM image of epoxy nanocomposites lled with hybrid ller system (the
total ller volume fraction is equal to 20%).

K. Yang, M. Gu / Composites: Part A 41 (2010) 215221

considerable to be utilized to obtain high thermal conductivity

with relatively low cost. This type of ller system could supply synergetic effect and cost reduction simultaneously. FESEM image of
epoxy nanocomposites lled with hybrid ller system is revealed
in Fig. 6. A good dispersion state of hybrid ller can be seen. The
HRTEM image showing the enhanced conductive network induced by the hybrid shape llers would be benecial to the readers. However, due to the hardness of SiCnp is very high, in the
thinning process of the sample, SiCnp easily drops out. Obtaining
a good HRTEM image to present enhanced conductive network induced by the hybrid shape llers is very difcult. Consequently,
this HRTEM image is not supplied in the article. Figs. 5 and 6 can
show the dispersion of hybrid llers and the formation of enhanced
conductive network.
4. Conclusions
The study on the thermal conductivity of epoxy nanocomposites lled with single ller system and hybrid ller system was performed. In order to acquire good dispersion of llers and improve
epoxyller interfacial interaction, we carried out TETA functionalization of MWCNTs and silane coupler modication of SiCnp. Chemical surface treatment is conducive to the enhancement of thermal
conductivity of epoxy composites. The application of hybrid ller
system not only obtains high thermal conductivity of epoxy composites, but also restricts the existence of big ller agglomeration.
The thermal conductivity of epoxy nanocomposites with hybrid ller system is larger than that of epoxy nanocomposites with any
single ller system; thereby hybrid ller system could provide synergistic effect and cost reduction simultaneously.
Acknowledgement
The authors are grateful to Instrumental Analysis Centre of
Shanghai Jiao Tong University for providing the support for this
work.
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