J. Phys. Chem.

C 2007, 111, 17923-17927 17923

Improved Load Transfer in Nanotube/Polymer Composites with Increased Polymer

Molecular Weight†
Minfang Mu and Karen I. Winey*
Department of Materials Science and Engineering, UniVersity of PennsylVania, 3231 Walnut Street,
Philadelphia, PennsylVania 19104-6272
ReceiVed: February 25, 2007; In Final Form: June 18, 2007

Mechanical interactions between amorphous polymers and nanofillers were probed by measuring the tensile
moduli of nanocomposite fibers with aligned single wall carbon nanotubes (SWNT) and carbon nanofibers
(CNF). Polymer chains provide better load transfer and thereby higher tensile moduli when the polymer size
is large relative to the diameter of the filler. The specific interfacial area of the filler is not sufficient to
explain this observed increase in elastic modulus. The effective modulus of SWNT bundles was ∼250 GPa,
as calculated using a short fiber model.
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Introduction interactions and at a fixed filler/polymer interfacial area. When

the radius of gyration, Rg, of a nonassociating amorphous
Single wall carbon nanotubes (SWNT) have exceptional polymer is greater than the diameter of a high aspect ratio filler,
mechanical properties as illustrated by a tensile modulus as high the tensile modulus increases substantially.
Publication Date (Web): July 31, 2007 | doi: 10.1021/jp0715530

as 1 TPa,1 which makes them particularly attractive as reinforc-

ing nanoscale fillers in polymers. Given that the mechanical
properties of composites depend critically on the load transfer
efficiency at the filler/polymer interface,2,3 chemical function-
alization methods have been used to improve the load transfer
efficiency at nanotube/polymer interfaces.4-6 However, SWNT
functionalization adds numerous chemical steps to composite
fabrication and introduces defects on the nanotube surface that
compromise their electrical and thermal properties.7,8 An
alternative way to improve the interfacial load transfer is to
strengthen noncovalent bonding between carbon nanotubes and
polymers by introducing specific interactions such as π-π
interactions8 and CH-π interactions.9 With these specific
interactions, polymer wrapping of SWNT has been widely
observed experimentally10-13 and by simulation14 when the
polymer is a single strand of DNA or has specific functional
groups such as phenylenevinylene. DNA-SWNT or conjugated
polymer-SWNT complexes have proven useful in separating
SWNT by type15 but are not applicable to composites. In the
absence of specific interactions, it is unlikely that polymer chains
uniformly wrap SWNT and, even so, how does tight polymer
wrapping of SWNT improve load transfer? Another important
issue for load transfer is the interfacial area between filler and
polymer, as reported by Cadek et al.16 They observed a linear
dependence of tensile modulus on the interfacial area per unit
volume in carbon nanotube/semicrystalline polymer composites.
In this study, we probe the load transfer at the nanotube/
polymer interface in amorphous polymer composites. We
measured the mechanical properties of poly(methyl methacryl-
ate) (PMMA) nanocomposite fibers containing well-aligned
SWNT or carbon nanofibers (CNF) as a function of polymer
molecular weight. In these systems, there is no covalent bonding
or specific interactions beyond the weak van der Waals force
between the fillers and the PMMA matrix. Fibers with aligned
fillers provide insight into load transfer at filler/polymer
interfaces, because the filler-filler interactions are minimized.
We found that longer polymer chains more effectively transfer
mechanical load to SWNT bundles, even without specific
† The nanocomposites were spun into fibers from the melt state
Part of the special issue “Richard E. Smalley Memorial Issue”.
* Corresponding author. E-mail: winey@seas.upenn.edu. Phone: 215-
898-0593. Fax: 215-573-2128.
10.1021/jp0715530 CCC: $37.00 © 2007 American Chemical Society
Published on Web 07/31/2007
Experimental Section
SWNT were synthesized by a high-pressure carbon monoxide
conversion (HiPco) method. Raw SWNT was purified by
thermal oxidization, followed by a HCl treatment.17 The residual
metal is less than 5 wt %, as measured by scanning thermo-
gravimetric analysis (TGA). CNF was purified by the same
method. PMMA was purchased from Polysciences and used as
received. The molecular weights are 25 kg/mol and 100 kg/
mol (denoted as 25 k and 100 k), and the polydispersity indices
for the two polymers are ∼1.7, as measured by size exclusion
chromatography (SEC). SWNT/PMMA and CNF/PMMA nano-
composites were prepared by a coagulation method.18 The
SWNT/N,N-dimethylformamide (DMF) suspension was soni-
cated for 24 h to exfoliate SWNT aggregates into small bundles
or isolated tubes and then mixed with the PMMA/DMF solution
under sonication. This SWNT/PMMA/DMF solution was poured
into excess water, and the nanocomposite rapidly precipitated.
The resulting composites were dried in vacuum oven at 130 °C
for 24 h. Prior to coagulation, a substrate submerged into the
SWNT suspension and dried for atomic force microscopy
(AFM) to characterize the SWNT bundle size.19 The mean
diameter of these SWNT bundles is ∼9.6 nm and the mean
aspect ratio of SWNT is ∼35. Coagulation is sufficiently rapid
as to avoid agglomeration of the SWNT bundles.
Raman microspectroscopy was used to evaluate the spatial
distribution of SWNT in nanocomposites. The nanocomposites
prepared by coagulation were hot pressed into ∼30 µm films
at 150 °C. The Raman intensity of the nanocomposite film was
collected at a wavenumber of 1590 cm-1 (D band of SWNT)
using Ar ion laser excitation at 514.5 nm. The Raman imaging
scans were 10 × 10 µm2 with a step size of 0.5 µm, and multiple
regions were imaged on each sample. The Raman intensities
were scaled, so that the average intensity for each image was
100 au. The standard deviation of the intensity provides a
measure of the spatial uniformity of SWNT in the nanocom-
posites.18
using a DACA SpinLine at ∼200 °C. The diameter of the
spinneret was 0.5 mm, the extrusion speed was 1.0 mm/min,
 17924 J. Phys. Chem. C, Vol. 111, No. 48, 2007 Mu and Winey
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Publication Date (Web): July 31, 2007 | doi: 10.1021/jp0715530

Figure 1. (a) Raman mapping image (10 × 10 µm) collected at 1590

cm-1 from a 1.0 wt % SWNT/100 k PMMA composite film. Standard
deviation of the normalized intensity is less than 4/100, indicating a
uniform SWNT distribution. (b) The fwhm, as measured by SAXS,
indicating the alignment of SWNT bundles in 1.0 wt % SWNT/PMMA
composite fibers as a function of the fiber diameter. Similar SWNT
alignment was observed in composites with 25 k and 100 k PMMA.

and the winder speeds were 6, 11, 16, or 21 m/min to make

fibers with various diameters (50-120 µm) and extents of filler
alignment. The degree of filler alignment was characterized by
small-angle X-ray scattering (SAXS) for SWNT/PMMA com-
posite fiber, where the scattering arises from the form factor
scattering from SWNT bundles.20 The d002 spacing of graphite
in wide-angle X-ray scattering (WAXS) is used to characterize
the degree of CNF alignment. The intensity was integrated in a
q range of 0.015 to 0.15 Å-1 for SWNT composites and 1.7 to
2.0 Å-1 for CNF nanocomposites. The scattering intensity as a
function of azimuthal angle was fit using a Lorentzian function,
and the full width at half-maximum (fwhm) corresponds to the
degree of alignment: 0° is perfectly aligned, 180° is isotropic.
The tensile modulus of the nanocomposite fibers was
measured using an Instron Model 5564 table mounted materials
testing system at room temperature at a crosshead speed of 1.0
mm/min and a gauge length of 2.54 cm.
Results and Discusions
The SWNT bundles were observed to be uniformly dispersed
at a length scale of one micron according to Raman mapping,
Figure 1a, as previously demonstrated with our coagulation
method.18 The 1.0 wt % SWNT nanocomposites with either 25
k or 100 k PMMA have standard deviations of the normalized
Figure 2. Tensile moduli of composite fibers with different filler
loadings as a function of fiber diameter. (a) SWNT/100 k PMMA
composites. (b) SWNT/25 k PMMA composites. (c) CNF/100 k PMMA
composites. Only the SWNT/100 k PMMA composites exhibit an
increase in tensile modulus with loading.
Raman intensity < 4/100, indicating that the dispersion of
SWNT in the composite is very good and has not been
significantly affected by the matrix molecular weight. Figure
1b shows the degree of SWNT alignment in the nanocomposite
fibers. The alignment of SWNT increases somewhat with
decreasing fiber diameter, but all of the fwhm values are small
(∼7-11°), indicating a good alignment of SWNT bundles. The
molecular weight of the polymer matrix does not effect SWNT
alignment.
Figure 2a shows the tensile moduli of the 100 k PMMA
composite fibers with 0, 1.0, and 2.0 wt % SWNT as a function
of fiber diameter. The tensile moduli of PMMA fibers (Em)
increased from ∼3000 MPa to ∼4500 MPa as the diameter of
the fiber decreased from 120 to 50 µm. Decreasing fiber
diameter correlates with extending the polymer conformation,
 Load Transfer in Nanotube/Polymer Composites
TABLE 1: Relative Elastic Moduli (Ec/Em) of Various
Nanocomposite Fibers along with Their Relative Filler Size
(2Rg/D), Specific Interfacial Area (r), and Filler-Filler
Separation (a-D)
R [a-D] Ec/Ema
composite 2Rg/D (µm-1) (nm) (MPa)
1.0 SWNT wt %/100 k 1.79 3.33 85.5 1.25
2.0 SWNT wt %/100 k 1.79 6.66 57.7 1.53
1.0 SWNT wt %/25 k 0.90 3.33 85.5 1
2.0 SWNT wt %/25 k 0.90 6.66 57.8 1 well-aligned in the fiber, a simple construct can be applied to
6.4 CNF wt %/100 k 0.22 3.33 192.7 1 calculate their interfacial area. By assuming that the composite
17.7 CNF wt %/100 k 0.22 9.19 85.5 1 fibers are composed of tetragonal unit cells with one cylindrical
a
Obtained Ec for 50 µm diameter fibers by fitting the experimental
data in Figure 2; used a fiber diameter of 110 mm for 17.7 CNF wt
%/100 K.
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Publication Date (Web): July 31, 2007 | doi: 10.1021/jp0715530
Figure 3. Schematic of the interactions between polymers and fillers,
showing the importance of size. Note the lengths of the fillers are
considerably longer than shown here.
which explains the increase in the tensile modulus relative to
bulk PMMA (∼2000 MPa).21 The tensile moduli also increased
with the addition of SWNT (Figure 2a), which is consistent
with our previous work.22 In 50 µm diameter fibers, the increases
in modulus relative to PMMA are 25% and 53% for 1.0 wt %
and 2.0 wt % SWNT nanocomposites, respectively (Table 1).
The tensile moduli of the SWNT/25 k PMMA composite
fibers (Ec) also increase with decreasing fiber diameter, Figure
2b. However, in contrast to SWNT/100 k PMMA fibers, the
moduli do not change with 1.0 wt % or 2.0 wt % SWNT
indicating poor load transfer efficiency at the SWNT-polymer
interface. In nanocomposites with isotropic distributions of
SWNT, nanotube-nanotube interactions with attraction energies
of ∼40kBT obscure the SWNT-polymer interactions.23 During
melt fiber spinning, high extensional forces align the nanotube
bundles and thereby reduce nanotube-nanotube interactions.24
Du et al. observed a significant decrease in the electrical
conductivity of fibers with increased SWNT alignment,25 which
also originates from the reduced number of tube-tube contacts.
The decrease in tube-tube contact strongly suppresses the load
transfer through tube-tube interactions in the SWNT/PMMA
fibers. Therefore, the contribution of the SWNT to the tensile
moduli of these aligned composites relies predominantly on the
SWNT/polymer interaction, which is the interfacial load transfer.
Our results indicate that the SWNT/polymer interactions
become stronger and improve the composite fiber modulus (Ec)
as the PMMA molecular weight increases. The radius of
gyration (Rg) is ∼8.6 nm for 100 k PMMA and ∼4.3 nm for
25 k PMMA.26 In 100 k PMMA composites, the ratio of 2Rg to
the SWNT bundle diameter (DSWNT) is 1.79 (Table 1) indicating
a high probability that one high molecular weight polymer can
surround a SWNT bundle (Figure 3). In contrast, 2Rg/DSWNT
for 25 k PMMA composites is 0.90, so that the SWNT bundles
are larger than the polymer coil. The limited entanglement
J. Phys. Chem. C, Vol. 111, No. 48, 2007 17925
between 25 k PMMA and SWNT bundles provides poor load
transfer efficiency and no increase in moduli (Figure 2b). When
PMMA chains encompass the SWNT bundles, the composites
have higher load transfer efficiency and higher tensile modulus.
Longer polymer chains provide better load transfer efficiency
between the polymer matrix and the SWNT, but total load
transfer at the filler/polymer interface might also depend on the
specific interfacial area.16,27 Because the SWNT bundles are
filler in each cell, we find the weight fraction of the fillers, c,
can be expressed as:28
Ffπ(D/2)2L
c) (1)
Fma2L
where Ff and Fm are the densities of fillers and matrix,
respectively; D is the diameter of filler, L is the filler length,
which is the same as the unit cell length, and a is the width of
the unit cell. By rearranging eq 1, the interfacial area per unit
volume R is given by:
πDL 4Fmc
R) ) (2)
a2L FfD
With FSWNT ) 1.5 g/cm3 (ref 29) and FPMMA ) 1.2 g/cm3, the
interfacial area per unit volume or specific interfacial area of
the 1.0 wt % SWNT composite is 3.3 µm-1 (Table 1). This
value is independent of the molecular weight of the polymer
and only depends on the density ratio (matrix/filler), filler
diameter, and loading. In these well-aligned SWNT/PMMA fiber
composites, increasing R by increasing the filler concentration
(c) does not increase the observed Ec when the molecular weight
of the matrix is only 25 k. This observation points toward the
importance of 2Rg/D for interfacial load transfer.
We further evaluate the relative importance of specific
interfacial area (R) and the relative filler size (2Rg/D) by using
another carbon nanofiller, namely, carbon nanofiber (CNF),
having a graphene-like surface. The tensile modulus of the CNF
is in the range of 100-600 GPa,30 which is comparable with
the tensile modulus of SWNT bundles.31 The CNF diameter of
∼77 nm is much larger than the radius of gyration of 100 k
PMMA, so it is difficult for CNF to be embedded within a single
polymer chain coil. A 6.4 wt % CNF/PMMA composite has
the same specific interfacial area (R) value as the 1.0 wt %
SWNT/PMMA composites; the density of CNF is 1.2 g/cm3.
Cadek et al.16 have reported that the tensile moduli increase
linearly with the specific interfacial area in nanotube/polymer
composites with various nanotubes. However, we observed that
the tensile modulus of the 6.4 wt % CNF/100 k PMMA
composite fiber is the same as pure PMMA (Figure 2c). This
suggests that the load transfer at such CNF/100 k PMMA
interfaces is poor. The larger CNF is not surrounded by
individual PMMA coils (2Rg/D ) 0.22), which leads to a very
low load transfer efficiency and inhibits the reinforcing effect
of the filler. Naturally, the comparison of 1.0 wt % SWNT/100
k PMMA and 6.4 wt % CNF/100 k PMMA composites fibers
is complicated by possible differences in the weak van der Waals
forces due to the details of the graphene structures of the fillers.
Nonetheless, both composites have comparable filler moduli and
the same matrix and specific interfacial area, but only the system
with a large 2Rg/D value exhibits an improved modulus, thereby
 17926 J. Phys. Chem. C, Vol. 111, No. 48, 2007
suggesting that the specific interfacial area alone is insufficient
in predicting the mechanical properties in these polymer
nanocomposites.
Indirect filler-filler interactions that might arise when a
polymer spans the distance between fillers could also influence
the mechanical properties. Based on eq 1, the average interface-
to-interface distance [a-D] between the nearest SWNT bundles
in 1.0 wt % SWNT/PMMA composite fibers is 85.5 nm, which
is 9 times larger than the gyration of radius of 100 k PMMA.
Thus, the probability that one polymer chain will bridge two
fillers is very low. In 6.4 wt % CNF/PMMA composites, [a-D]
is 192.7 nm (Table 1). If the CNF-CNF separation is reduced
to be the same as in 1.0 wt % SWNT nanocomposites, which
corresponds to a CNF loading 17.7 wt %, the specific interfacial
area is almost 3 times larger than that in the 1.0 wt % SWNT
composites. The dispersion of 17.7 wt % CNF in PMMA is
still good at this high loading and the azimuthal fwhm value
for a 120 µm diameter fiber is ∼70°, on the basis of the d002
reflection. Though the alignment of CNF is not as good as the
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SWNT in the composite fibers, indicating a relatively high
filler-filler contact interaction, the tensile modulus of 17.7 wt
% CNF/PMMA composite fibers remains the same as the
PMMA fibers (Figure 2c). (Fibers with diameters less than 100
Publication Date (Web): July 31, 2007 | doi: 10.1021/jp0715530
µm were not obtained because of the brittleness of the 17.7 wt
% CNF/PMMA composite.)
We conclude that physical entanglements between nanoscale
fillers and polymer chains play an important role in load transfer
efficiency in polymer nanocomposites. Of the three parameters
considered in this study (2Rg/D, R, [a-D]), the parameter most
strongly correlated with modulus in these nanocomposites is
2Rg/D, the relative size of the amorphous polymer to the rod-
like filler. When the filler diameter is larger than ∼2Rg of the
matrix polymer, the polymer does not surround the high aspect
ratio filler, and the load transfer efficiency at the filler/polymer
interface is poor (Figure 3). Consequently, the tensile moduli
of the composites are equal to the modulus of the 25 k PMMA,
even when R is as large as 6.66 µm-1 in 2.0 wt % SWNT
composite. When the polymer size is larger than the filler
diameter (2Rg/DSWNT ) 1.79 for the SWNT/100 k PMMA
composites), the entanglement between polymer and filler
effectively transfers the load, and the tensile modulus increases.
A short fiber model was used to calculate the effective
modulus of SWNT bundles (Ef) in the composites.32 The short
fiber model assumes different strains on the filler and the
polymer matrix and an inhomogeneous load on the filler. Using
this model, the tensile modulus of the composite fiber (Ec) can
be calculated by the following equation:
Ec ) VmEm + VfEf{1 - tan h(ns)/ns} (3)
where Em and Ef are the tensile moduli of the polymer matrix
and filler, Vm and Vf are the volume fractions, s is the aspect
ratio of filler, and n is a dimensionless parameter given by n2
) 2Em/[Ef(1 + νm) ln(Pf/Vf)] , where νm is the Poisson’s ratio
of PMMA and Pf is the filler packing factor. We approximate
our fibers by assuming that all of the SWNT bundles have the
same size and are square packed, perfectly aligned, and
uniformly dispersed. Thus, the composite was divided into
tetragonal unit cells with one cylindrical filler in each cell,
consistent with eq 1, and ln(Pf/Vf) ) ln(π/Vf).
The calculated effective moduli of the SWNT bundles in 100
K PMMA composites is ∼250 GPa (Table 2). This bundle
modulus is smaller than the published value of one individual
SWNT tube, 1 TPa, but is comparable to the tensile modulus
of SWNT bundles with ∼10 nm diameter.31 The slight difference
Mu and Winey
TABLE 2: Effective Moduli of SWNT Bundles, Ef,
Calculated by Applying a Short, Aligned Fiber Model to the
SWNT/PMMA Nanocomposite Fibers
composite (SWNT/PMMA) Eca (MPa) Efb (GPa)
1.0 wt %/25 k 5000 5.32
2.0 wt %/25 k 5000 5.30
1.0 wt %/100 k 5600 246
2.0 wt %/100 k 6900 262
a Experimental data for fibers from Figure 2 with 50 µm diameter
where the highest degree of SWNT alignment was obtained in our
experiments. b Calculated from eq 3 using Em(100 k) ) 4500 MPa,
Em(25 k) ) 5000 MPa, FSWNT ) 1.5 g/cm3, FPMMA ) 1.2 g/cm3, νm ∼
0.4, and s ) ∼ 35, as observed by AFM. The 1.0 wt % and 2.0 wt %
composites correspond to 0.8 vol % and 1.6 vol %, respectively.
between the effective bundle modulus in the 1.0 wt % and 2.0
wt % SWNT composite might come from the increased tube-
tube interactions at the higher SWNT loading. In contrast the
effective bundle modulus is only ∼5 GPa in the SWNT/25 k
PMMA composite fibers. This low effective modulus indicates
low load transfer efficiency. The reinforcing effect of SWNT
bundles on a polymer matrix evidently requires SWNT-
polymer entanglement.
An alternative interpretation is suggested by earlier studies
of melt extruded PMMA fibers, in which the modulus increases
from 1500 to 3500 MPa at different draw velocities and
processing temperatures.33 The authors attributed this increase
in modulus to extended chain conformations of the PMMA. In
the nanocomposites studied here, the presence of cylindrical
fillers might promote polymer elongation during melt fibers
spinning because of increased viscosity and might also retard
polymer relaxations prior to cooling below the glass transition
temperature. We attempted to account for polymer elongation
in this study by (1) plotting the modulus as a function of fiber
diameter, which corresponds to the strength of the melt extrusion
process, and (2) reporting relative increases in modulus at fixed
fiber diameters. Future studies should probe the extent of
polymer anisotropy in nanocomposite fibers but are likely to
be complicated by the alignment of the cylindrical fillers.
Whether the molecular weight effect we report here is rooted
in interfacial load transfer or in chain conformation, the
molecular weight of the matrix polymer is critical for maximiz-
ing the mechanical properties of nanocomposite fiber.
In summary, while the molecular weight of an amorphous
polymer matrix has no significant effect on SWNT dispersion
and alignment in SWNT/PMMA composite fibers, the molecular
weight plays a crucial role in mechanical load transfer. The
relative size of the polymer, 2Rg/D, where Rg is the polymer
radius of gyration and D is the diameter of the cylindrical filler,
must be greater than one to improve load transfer at the filler-
polymer interface and increase the elastic moduli of the
composite. In contrast, the specific interfacial area did not
correlate with composite moduli in these nanocomposites with
an amorphous polymer matrix. Small filler sizes (D) and suitable
polymer molecular weight (Rg) are critical requirements for high
load transfer in nanocomposite through filler-polymer en-
tanglements.
Acknowledgment. This research was funded by the National
Science Foundation MRSEC-DMR05-20020. We thank Dr.
Fangming Du and Dr. Reto Haggenmueller for valuable
discussions. We are grateful to Professor Shu Yang of our
department for access to the SEC.
 Load Transfer in Nanotube/Polymer Composites
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