Composites: Part A 58 (2014) 16

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

Effect of silica coating thickness on the thermal conductivity

of polyurethane/SiO2 coated multiwalled carbon nanotube composites
Jinchao Zhao a,b, Feipeng Du c, Wei Cui b, Ping Zhu a, Xingping Zhou b,, Xiaolin Xie b
a

School of Chemistry and Chemical Engineering, State Key Laboratory of New Textile Materials and Advanced Processing, Wuhan Textile University, Wuhan 430064, China
State Key Laboratory of Material Processing and Die & Mould Technology, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology,
Wuhan 430074, China
c
School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430073, China
b

a r t i c l e

i n f o

Article history:
Received 23 July 2013
Received in revised form 28 October 2013
Accepted 9 November 2013
Available online 21 November 2013
Keywords:
A. Polymermatrix composites (PMCs)
B. Electrical properties
B. Thermal properties
Carbon nanotubes

a b s t r a c t
Silica coated multiwalled carbon nanotubes (SiO2@MWCNTs) with different coating thicknesses of
4 nm, 3050 nm, and 7090 nm were synthesized by a solgel method and compounded with polyurethane (PU). The effects of SiO2@MWCNTs on the electrical properties and thermal conductivity of the
resulting PU/SiO2@MWCNT composites were investigated. The SiO2 coating maintained the high electrical resistivity of pure PU. Meanwhile, incorporating 0.5, 0.75 and 1.0 wt% SiO2@MWCNT (7090 nm) into
PU, produced thermal conductivity values of 0.287, 0.289 and 0.310 W/mK, respectively, representing
increases of 62.1%, 63.3% and 75.1%. The thermal conductivity of PU/SiO2@MWCNT composites was also
increased by increasing the thickness of the SiO2 coating.
2013 Elsevier Ltd. All rights reserved.

1. Introduction
With the rapid development of semiconductors and highly integrated circuit technology, high-performance thermal interface
materials are increasingly required. Due to their excellent thermal
conductivity, carbon nanotubes (CNTs) have attracted much attention as potential interface llers [1]. Unfortunately, CNTs have poor
dispersibility in, weak compatibility with, and poor interface interactions with polymer matrices due to their large specic surface
area, high aspect ratio, and high surface energy [2]. The resulting
high interfacial thermal resistance between CNTs and polymers
thereby hinders the phonon propagation at the interface, producing experimental results that fail to meet theoretical expectations
[38].
In theory, the thermal conductivity of polymer/CNT composites
is largely controlled by the thermal resistance on the interface
[9,10]. One option is to decrease the thermal resistance by improving the quality of the interface between CNTs and the polymer matrix. The covalent functionalization of CNT surfaces with reactive
groups, molecules, polymer chains, or inorganic materials was
once considered to be an effective method to achieve this goal
[11,12]. Among them, the linkage of inorganic materials to CNTs
which exhibits interesting structure, electrical and/or thermal
properties has attracted much attention. Im et al. [13] synthesized
Corresponding author. Tel.: +86 27 87540053; fax: +86 27 87543632.
E-mail address: xpzhou@mail.hust.edu.cn (X. Zhou).
1359-835X/$ - see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesa.2013.11.008

Al2O3 doped multiwalled carbon nanotubes (MWCNTs) and added

them to alumina-epoxy-terminated poly(dimethylsiloxane) to fabricate an electrically insulated and thermally conductive composite. The authors indicated that the good dispersability of the
resulting nanowires could affect the interconnectivity between
conducting particles (Al2O3) and the establishment of threedimensional, heat conducting percolating networks in a matrix.
The conducting networks were considered to affect the thermal
conductivity of composites [13]. The increasing thermal conductivity of Al2O3/epoxy-terminated poly(dimethylsiloxane) composites
brought out by Al(OH)3-covered MWCNT also supports the above
conclusion [14]. Furthermore, decreasing the elastic modulus mismatch between the stiff CNTs and soft polymer matrix helps to
overcome the heat ow barrier, also enhancing thermal conductivity [13,15,16]. Our previous work reported the thermal conductivity of the PU/SiO2-MWCNT composites was increased by 53.7% and
63.8% respectively by adding 0.5 wt% and 1.0 wt% SiO2-MWCNTs
with 3050 nm thick silica coating layer [15]. Our group also reported 67.8% increase in the thermal conductivity of epoxy composites by incorporating 1 wt% silica-coated MWCNTs compared
to epoxy matrix [16]. These works demonstrated that the silica
intermediate shell on the MWCNTs not only improves the interaction between the stiff MWCNTs and the soft polymer matrix, but
also alleviates the modulus mismatch between them [15,16].
Recently, molecular dynamic simulation results indicated that
the interfacial thermal resistance (Rk) was reduced with increasing
length and density of the grafting chains on CNTs [17]. Gojny et al.

J. Zhao et al. / Composites: Part A 58 (2014) 16

[18] suggested that decreasing the interfacial area of MWCNTs

could reduce the possibility of phonon-scattering at the interface,
promote the conduction of phonons, and minimize coupling losses.
Increasing the diameter of CNTs had also been shown to increase
the contact area among CNTs and decrease the contact interface
resistance [19]. Grafting thickness of CNTs could thereof alter the
grafting chain length, interfacial area, and contact area among
CNTs, causing the Rk and thermal conductivity of composites to
change with them. To date, little experimental or theoretical study
had focused on the inuence of coating thickness on the thermal
conductivity of CNT/polymer composites. Therefore, in this work,
the SiO2 coated MWCNT (SiO2@MWCNT) with different coating
thickness were incorporated into polyurethane matrix. The effect
of the grafted SiO2 shell thickness on thermal conductivity of the
polyurethane composites was investigated and evaluated.

2. Experimental
2.1. Materials
Poly(ethylene oxide-tetrahydrofuran) (PEOT; functional degree:
2, hydroxyl value: 0.427 mg KOH/g, weight-average molecular
weight: 3660 g/mol and viscosity: 9.68 Pa s) and N-100 (functional
degree: 3.62 and isocyanate concentration: 5.3 mmol/L), a solventfree aliphatic polyisocyanate resin based on hexamethylene diisocyanate, were provided by Liming Research Institute of Chemical
Industry (China). These were degassed in a vacuum oven at
60 C, 0.1 MPa for 3 h to remove any absorbed water before use.
Dibutyltin dilaurate, tetraethyl orthosilicate, and other commonly
used reagents were purchased from Sinopharm Chemical Reagent
Co., Ltd. (China). Pristine MWCNTs (p-MWCNTs) were purchased
from Shenzhen Nanotech Port Co. (China) with 95 wt% purity.
The p-MWCNTs were prepared using the CVD method, and their
diameters ranged from 40 to 60 nm and lengths from 5 to 15 lm.

2.2. Synthesis of SiO2@MWCNTs

The p-MWCNTs were puried and oxidized by reuxing in
mixed acid (HNO3/H2SO4, v/v = 3:1) as reported in our recent work
[20]. The resulting acid-oxidized MWCNTs (OAMWCNTs), now
containing the functional groups ACOOH, AOH and @O, can be easily dispersed in various solvents.
MWCNTs grafted with different SiO2 coating thicknesses were
synthesized by solgel methods as reported in our previous work
[21]. Here, we produced three different size classes of SiO2@MWCNTs: 4 nm, 3050 nm, and 7090 nm. To produce 4 nm
SiO2@MWCNTs, 1.000 g O-MWCNTs were ultrasonically dispersed
in a mixture of 52 mL anhydrous ethanol, 19 mL deionized water
and 0.24 mL HCl for 30 min, then subject to vigorous mechanical
agitation for another 30 min to obtain a stable, homogeneous suspension. Next, 21 mL tetraethoxysilane (TEOS) was added quickly
and the mixture was stirred for 3 h at room temperature. After
the reaction, the mixture was centrifuged at 4000 rpm. To remove
free silica particles, the resultant sediment was ultrasonically
re-dispersed in N,N-dimethylformamide (DMF) for 15 min and
vacuum ltered. This procedure was repeated at least four times.
Finally, the darkish product was obtained by ltering the
vacuum-ltered sediment through a 0.8 lm nylon membrane
and vacuum drying to yield the nal 4 nm SiO2@MWCNTs.
To produce 3050 nm SiO2@MWCNTs, 1.000 g O-MWCNTs
were ultrasonically dispersed in a mixture of 330 mL anhydrous
ethanol, 36 mL deionized water and 49 mL NH4OH for 30 min,
followed by vigorous mechanical agitation for another 30 min to
obtain a stable, homogeneous suspension. The reaction of the

suspension with TEOS and subsequent purication were carried

out as above.
Finally, to produce 7090 mn SiO2@MWCNTs, 1.000 g OMWCNTs were ultrasonically dispersed in a mixture of 250 mL
anhydrous ethanol, 90 mL deionized water and 8 mL NH4OH for
30 min, followed by vigorous mechanical agitation for another
30 min to obtain a stable, homogeneous suspension. The suspension was reacted with 37 mL TEOS using the same conditions as
previously and treated following the same process as above.
2.3. Preparation of PU/SiO2@MWCNT composites
Polyurethane (PU) composites have attracted considerable
attention as electronic packaging materials because of their high
exibility which can reduce thermal stresses caused by thermal
shock. The PU/SiO2@MWCNT composites, in this work, were prepared according to the fabrication process shown in Fig. 1. SiO2@MWCNTs were dispersed in acetone through mechanical shearing
and ultrasonication for 1 h at room temperature. After adding
PEOT, the mixture was ultrasonicated for another 1 h, followed
by vigorous stirring at 80 C for 1 h to ensure good homogeneity
and allow acetone to vaporize. The resulting slurry was mixed with
N-100 in a molar ratio of [OH]:[NCO] of 1:1.2 with 0.2 wt% dibutyltin dilaurate as catalyst, then degassed to remove any trapped air
bubbles. Finally, the mixture was cast in steel molds and cured at
90 C for 24 h. The nal product consisted of disk-like specimens
with 100 mm diameter and 2 mm thickness. The content of SiO2@MWCNTs in the PU matrix was xed at 0.5, 0.75 and 1.0 wt%. For
the control experiments, pure PU and p-MWCNT/PU composites
were prepared under the same conditions, with the loading of
p-MWCNTs in PU the same as that for SiO2@MWCNTs in PU.
2.4. Measurements
Transmission electron microscopy (TEM) was performed on a
Tecnai G2 20 electron microscope (FEI Co., Netherlands) at
20.0 kV. Scanning electron microscopy (SEM) was conducted using
a Quanta 200 environmental scanning electron microscope (FEI
Co., Netherlands) to examine the dispersion of the MWCNTs in
composite fracture surfaces obtained by brittle fracture of disk-like
specimens in liquid nitrogen. Thermogravimetric analysis (TGA)
was performed on a Pyris1 TGA (PerkinElmer Inc., USA) instrument heated from room temperature to 600 C at a heating rate
of 10 C/min and ow rate of 20 mL/min in argon. The cast disklike specimens were used to test the thermal conductivity and volume electrical resistivity with an HC-074 heat-ow meter (EKO
Instrument Co., Japan) according to ASTM C518-02 and a plate
electrode type ZC36 high resistance meter (Shanghai Cany Precision Instrument Co., China) according to GB/T 1410-2006. The reported results represented average values from ve samples.
3. Results and discussion
As shown in Fig. 2a, the p-MWCNTs were highly entangled and
randomly organized. Their surfaces were rough and contained
some impurities, such as catalyst particles and amorphous carbon.
After surface modication, SiO2 layers with different thickness
were coated onto the MWCNTs. The image of coaxial coreshell
structure was easily distinguished, and the thickness of the SiO2
layer synthesized by acid catalysis was 4 nm (Fig. 2b), while
those formed by alkaline catalysis were either 3050 nm (Fig. 2c)
or 7090 nm (Fig. 2d).
The content of SiO2 in the SiO2@MWCNTs was determined by
TGA. As shown in Fig. 3, the p-MWCNT was decomposed
completely at about 810 C in argon, which indicates leaving only

J. Zhao et al. / Composites: Part A 58 (2014) 16

Fig. 1. Fabrication schematic of PU/SiO2@MWCNT composites.

Fig. 2. TEM images of p-MWCNTs (a) and SiO2@MWCNTs with 4 nm (b); 3050 nm (c); 7090 nm (d) coating thickness.

Fig. 3. TGA curves of SiO2@MWCNTs with different coating thickness.

a residue of SiO2 for SiO2@MWCNTs sample. The grafted-SiO2

amount with thickness of 4 nm, 3050 nm and 7090 nm on
the surface of MWCNTs was therefore estimated to be 13.4, 67.2,
and 85.4 wt%, respectively.
The SEM images of fracture surfaces of PU/p-MWCNT and PU/
SiO2@MWCNT composites with different coating thickness are
shown in Fig. 4. The p-MWCNTs strongly tended to aggregate
and settle in the composites (Fig. 4a) due to the large surface area
of p-MWCNT as well as poor wetting and adhesion at the MWCNTPU interface. In case of a weak interfacial bonding simple pull-out
of the p-MWCNT from the matrix occurred and many corners left
[22] (Fig. 4b). However, SiO2@MWCNTs were uniformly dispersed
in the PU matrix (Fig. 4ce), and good interfacial bonding was observed between the SiO2@MWCNTs and PU matrix (Fig. 4d). The
SiO2 layer formed through the solgel method contains plentiful
OH groups, which are available to react with -NCO groups in N100 during curing. We suggest this is the likely cause of the good

J. Zhao et al. / Composites: Part A 58 (2014) 16

Fig. 4. SEM images of fracture surfaces of PU/p-MWCNT (0.5 wt%) composites (a), the high-magnication gure (b) of rectangle part in (a), and fracture surfaces of PU/
SiO2@MWCNT (0.5 wt%) composites with 4 nm (c); 3050 nm (d); 7090 nm (e) coating thickness. Aggregates of p-MWCNTs are circled in (a) and inset is the highmagnication gure in (d).

compatibility and strong interfacial adhesion between SiO2@MWCNTs and PU matrix.

The volume resistivity of PU and its composites were also tested
(Fig. 5). The results showed that volume resistivities of samples
with SiO2 layers of 4 nm, 3050 nm, and 7090 nm thickness
were 9.3  1013, 1.8  1014 and 2.1  1014 ohm cm, respectively,
for 0.5 wt% SiO2@MWCNT loading, 5.3  1013, 1.1  1014 and
1.2  1014 ohm cm, respectively, for 0.75 wt% SiO2@MWCNT loading, and 4.1  1013, 9.6  1013 and 10.0  1013 ohm cm, respectively, with 1 wt% SiO2@MWCNT loading. CNTs are known to be
excellent conductors, and the electrical conductivity of CNT/polymer composites depends on the form of electrical percolation network. Previous research from Moisala et al. [23] had shown that
percolation thresholds for MWCNTs were especially low, with
MWCNT loading in epoxy resin composites of <0.005 wt% capable
of forming a conductive network. In this work, 0.5 wt% p-MWCNTs
loading sharply decreases the volume electrical resistivity by only
56 orders of magnitude. With further loading to 0.75 and 1 wt%,
the electrical resistivity of PU/p-MWCNT composite slightly

Fig. 5. Electrical resistivity of pure PU (a); PU/p-MWCNTs (b) and PU/SiO2@MWCNT

composites with 4 nm (c); 3050 nm (d); 7090 nm (e) coating thickness.

J. Zhao et al. / Composites: Part A 58 (2014) 16

decreases. Overall, this indicates that an electrical percolating network is formed at a p-MWCNT loading of less than 0.5 wt% and that
volume resistivity does not decrease signicantly when increasing
the SiO2@MWCNT amounts. It is possible that the grafting modication disturbed the delocalization of p-electrons on the nanotube
surfaces, thus resulting in signicant deterioration of electrical
conductivity of MWCNTs, as what had been previously reported
[24,15]. Moreover, the SiO2 layer may act as an electrical insulator,
hindering the conduction of electrons between MWCNTs. Therefore, PU/SiO2@MWCNT composites retain almost the same volume
electrical resistivity as that of the pure PU. The results also showed
that volume resistivity slightly decreased with the increase of ller
content and decrease of SiO2 layer thickness. This suggested that
greater coating thickness led to improved electronic transmission
shielding; that is, the thicker SiO2 insulating layer improved the
electrical insulating performance of the composites.
Fig. 6 shows thermal conductivities of pure PU, PU/p-MWCNT,
and PU/SiO2@MWCNT composites. The thermal conductivity of
pure PU was 0.177 W/mK. With the addition of 0.5, 0.75 and
1 wt% of p-MWCNTs to pure PU, thermal conductivity increased
by 26.0%, 38.4% and 47.5%, respectively. Furthermore, thermal conductivity of 4 nm, 3050 nm, and 7090 nm SiO2 layers in PU/
SiO2@MWCNT increased separately by 50.3%, 53.7%, and 62.1%,
respectively, for 0.5 wt% SiO2@MWCNTs, 52.0%, 57.6%, and 63.3%,
respectively, for 0.75 wt% SiO2@MWCNTs, and 56.5%, 63.8%, and
75.1%, respectively, for 1 wt% SiO2@MWCNTs. These thermal conductivity values are clearly higher than those of PU/p-MWCNT
composites at the same loading.
In contrast with electrical conductivity, thermal transport in
CNTs is mainly related to phonon conduction. First, plentiful OH
groups on the surface of the SiO2 layer creates good compatibility
with the PU matrix, enhancing the interfacial interaction between
PU and MWCNTs and decreasing its thermal resistance. Second, the
SiO2 coating layer decreases the modulus mismatch between CNTs
and the polymer matrix, which may reduce thermal resistance at
the interface, thereby improving its phonon transmission. Haggenmueller et al. [25] showed that the thermal conductivity of a
SWCNT/high density polyethylene composite was higher than that
of SWCNT/low density polyethylene composite, linking the observation to the smaller modulus mismatch between the high density
polyethylene and SWCNT. By theoretical calculations, Youngs
modulus for single MWCNT and for SiO2 were 1 TPa [26] and
70 GPa [27], respectively, and Youngs modulus for polyurethane
elastomer was very low. Thus, SiO2 wrapped onto MWCNT surfaces
as a transition layer can decrease the modulus mismatch between

the high modulus MWCNTs and low modulus PU matrix, effectively reducing the interfacial thermal resistance of the composite.
Fig. 6 also shows that thermal conductivity of the
PU/SiO2@MWCNT composite increases with greater SiO2@MWCNT
coating thickness. According to Nans model [28] (Eq. (1)),
K

c
Ke
f p
Km
1
2a
k Kc
3 p dK
Km
m

where Ke, Km and Kc are the thermal conductivity of the composite,

matrix (0.177 W/m K) and CNTs (3000 W/m K for single MWCNT),
respectively, f is the ller content, d is the diameter of MWCNTs
(50 nm), p is the aspect ratio of CNTs (100), and ak is the Kapitza
radius (Eq. (2)),

ak Rk  K m

In Eq. (2), interface thermal resistance (Kapitza resistance, Rk) represents a barrier to heat ow between MWCNT and PU phases.
Based on the Eq. (1), the theoretical ak for PU/p-MWCNT and PU/
SiO2@MWCNT with 4 nm, 3050 nm, and 7090 nm SiO2 thickness are 14.16, 8.139, 7.616, and 6.557 nm, respectively. According
to Eq. (2), since the Rk vary along with ak, the SiO2 layer thickness
alone inuences the interfacial thermal resistance between the
MWCNTs and PU matrix. In particular, the interfacial thermal resistance will decrease by increasing the thickness of SiO2 layer.
Based on the CNT contact heat resistance model [29], when an
electricity percolation network has already formed in the composite material, contact heat resistance is lower for longer CNTs and
for CNTs with increased overlap area. Increasing the overlap area
has been suggested as a way to improve heat transfer efciency between CNTs [30]. In our work, the overlap area of SiO2@MWCNTs
was increased with greater SiO2@MWCNT content and greater
SiO2 coating thickness, which resulted in reduced contact heat
resistance of the SiO2@MWCNTs. Moreover, at a xed lling content, increased SiO2 coating thickness led to reduce specic surface
area of the SiO2@MWCNTs, resulting in decreased contact area between the polymer matrix and MWCNTs. This, in turn, decreased
the interfacial thermal resistance, leading to improved thermal
conductivity of the overall SiO2@MWCNT/PU composite.
4. Conclusions
Silica coated multiwalled carbon nanotubes (SiO2@MWCNTs)
with different coating thickness were synthesized by a solgel
method, then compounded with PU to prepare PU/SiO2@MWCNT
composites. We investigated the effect of SiO2@MWCNTs on thermal conductivity and electrical insulation of PU, showing that the
silica layer improved the interfacial interaction between MWCNTs
and PU and enhanced the dispersion of MWCNTs in the PU matrix.
Due to the electrical insulation of the silica layer, PU/SiO2@MWCNT
composites had almost similar electrical insulation to pure PU. The
silica intermediate layer also alleviated the modulus mismatch between the stiff MWCNTs and the soft PU, decreasing the probability of phonon scattering and enhancing the thermal conductivity of
the PU/SiO2@MWCNT composites. Furthermore, increased SiO2
coating thickness improved the thermal conductivity of the PU/
SiO2@MWCNT composites. We expect that the results of this study
will prove benecial for further improving of the thermal conductivity of polymer matrix composites, and can also be used to aid in
the design of efcient electronic packaging materials.
Acknowledgements

Fig. 6. Thermal conductivity of pure PU (a); PU/p-MWCNTs (b) and PU/SiO2@MWCNT composites with 4 nm (c); 3050 nm (d); 7090 nm (e) coating
thickness.

This work was supported by the National Natural Science Foundation of China (No. 51210004, 51303138), and the Educational
Committee Foundation of Hubei (No. Q20131606).

J. Zhao et al. / Composites: Part A 58 (2014) 16

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