Effect of High-Shear Mixing by Twin-Screw Extruder on
the Dispersion and Homogeneity of Polyacrylonitrile/
Carbon Nanotube Composite Solution
Xuejia Yan,1 Hongming Dong,1 Zhiwei Xiao,2 Yaodong Liu,1 Tao Liu,2 Han Gi Chae,1 Satish Kumar1
1
School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332
2
High-Performance Materials Institute, Florida State University, Tallahassee, Florida 32310
High-shear mixing experiments using twin-screw
extruder were conducted to study the effect of shearing
on carbon nanotube (CNT) dispersion in polyacrylonitrile
(PAN) polymer solution. Different types of CNTs (few-
wall carbon nanotube and single-wall carbon nanotube)
were used to prepare composite solution at 0.5 wt%
with respect to the PAN polymer through various prepa-
ration conditions. The resulting PAN/CNT composite
solution was characterized using various techniques
including dynamic light scattering, preparative ultracen-
trifuge method, optical microscopy, solution rheology,
and high-resolution transmission electron microscopy.
With increasing the number of extrusion cycle, it was
observed that the CNT bundle size was moderately
reduced, while solution homogeneity and macroscopic
CNT dispersion was significantly improved. POLYM.
COMPOS., 38:719–726, 2017. V
C 2015 Society of Plastics
Engineers
INTRODUCTION
High-performance carbon fibers are of great interest
due to their good mechanical properties, low density, and
excellent thermal and chemical properties [1]. Applica-
tions have been found in aerospace, transportation, and
nuclear engineering areas. Polyacrylonitrile (PAN) has
been a predominant precursor for the carbon fiber indus-
try [2]. Carbon nanotubes (CNTs), with a long aspect
ratio and excellent mechanical properties, have become
an important reinforcement material for inorganic compo-
sites [3–7], polymer composites [8–11], and carbon fibers
as well [12–14]. PAN/CNT precursor fibers have been
successfully obtained by gel spinning from PAN compos-
Correspondence to: S. Kumar; e-mail: Satish.kumar@mse.gatech.edu
Contract grant sponsor: Army Research Office (ARO); contract grant
sponsor: DARPA; contract grant number: W911NF-10-1-0098.
Additional Supporting Information may be found in the online version
of this article.
DOI 10.1002/pc.23631
Published online in Wiley Online Library (wileyonlinelibrary.com).
C 2015 Society of Plastics Engineers
V extrusion process and extrusion on the CNT dispersion
POLYMER COMPOSITES—2017
ite solutions containing CNTs [1]. Upon stabilization and
carbonization treatment of the PAN/CNT precursor fibers,
the resultant carbon fibers clearly showed the CNT tem-
plate graphitic interphase that is critical in improving the
tensile strength and modulus of the final product [1, 12,
13]. Given the progress being made, the dispersion qual-
ity of CNTs in PAN solutions is still the biggest hurdle
that prevents their utilization from achieving the highest
potentials. The reason for this can be partially attributed
to the strong van der Waals interactions that make CNTs
commonly stay together as bundles [15]. Significant
efforts have been made to debundle CNTs as individual
tubes [16–20], which, in terms of processing methods,
mostly rely on ultrasonciation—a batch process that has
difficulty for large-scale and high-throughput production
of high-quality dispersion of CNTs in PAN/organic sol-
vent polymer solution. In this regard, an appropriate con-
tinuous process to debundle CNTs is highly desired.
Twin-screw extrusion, with its high shearing and mix-
ing capability, has been used to produce polymer compo-
sites on both lab scale and production scale.
Poly(ethylene terephthalate) (PET)/multiwall carbon nano-
tubes (MWNTs) composites were prepared via twin-screw
extrusion, showing improved MWNTs orientation and
mechanical properties [8]. In addition, CNT dispersion in
low-density polyethylene (LDPE)/CNT composites was
significantly improved by high shear mixing using twin-
screw extruder [21]. The mechanical properties of polyvi-
nylidene fluoride (PVDF)/CNT as well as poly(methyl
methacrylate) (PMMA)/PVDF/CNT composites were also
reported to increase after the extrusion process [22, 23].
The relationship between twin-screw extrusion conditions
and morphology of polycaprolactone/CNT composites,
showing that the optimized extrusion improved CNT dis-
persion has also been reported [24]. In this study, we
explored using twin-screw extruder in conjunction with
different processing methods for large-scale preparation
of high-quality PAN/CNT solution. The effect of pre-
(bundle size and length) was investigated using various
characterization methods (preparative ultracentrifuge,
dynamic light scattering, Raman spectroscopy, and trans-
mission electron microscope) [25, 26].
EXPERIMENTAL
Materials
PAN homopolymer with a viscosity average molecular
weight of 250,000 g/mol was obtained from Japan Exlan
(Osaka, Japan) and was vacuum dried at 70 8C for 1 day
before use. Three different batches of carbon nanotubes
were obtained from Continental Carbon Nanotechnologies,
Inc. (Houston, TX). Few-wall carbon nanotubes (FWCNT,
lot number XO122UA with a Raman IG/ID ratio of 19 and
aspect ratio of 1320, and XOC231U with a Raman IG/ID
ratio of 52 and aspect ratio 2820) and single-wall carbon
nanotube (SWCNT, lot number SPO300 with a Raman IG/
ID ratio of 17 and aspect ratio 485) were used for this
study. Raman spectra of different CNTs were collected by
a Horiba Scientific Xplora confocal microRaman system
(laser wavelength 5 785 nm). For solution preparation,
HPLC-grade dimethylformamide (DMF) was purchased
from Sigma-Aldrich Co. and used as-received.
PROCEDURE
Composite Solution Preparation
Three different PAN/CNT/DMF composite solutions
(A, B, and C) used for extrusion were prepared by fol-
lowing a two-step process. Namely, CNT/DMF dispersion
was first prepared by sonication and microfluidization,
which was then mixed with PAN/DMF solution to result
in the desired stock composite solutions. The sample
preparation details are provided as following.
Solution A. For solution A, FWCNT (XO122UA) was
used. The dried FWCNT1 (1.125 g) was added in 1 L
DMF and the mixture was bath-sonicated (Branson 3510-
MT, 100 W, 42 kHz) for 1 h. The sonicated CNT/DMF
mixture was processed with microfluidizer (M110P, chan-
nel diameter 5 125 mm, Microfluidics Inc.) for 10 cycles
with operating pressure of 20,000 psi. The mixture was
then diluted by adding 2.5 L DMF (CNT slurry). In order
to disperse CNT further, CNT slurry was diluted at a con-
centration of 30 mg/L and bath-sonicated for 24 h. PAN
polymer solution was separately prepared by dissolving
45 g of polymer in 500 mL DMF at 70 8C for 2 h. Then
the bath-sonicated CNT dispersion was added to the poly-
mer solution and the excess DMF was removed by vac-
uum distillation to obtain solution concentration of 9 g/
100 mL. This procedure was repeated until all the CNTs
(1.125 g) were added to the solution. In the last solution
preparation step, fresh PAN solution was prepared by dis-
solving 180 g polymer in 1 L DMF. Then, the PAN/
720 POLYMER COMPOSITES—2017
CNT/DMF solution was mixed with the freshly prepared
PAN solution and the excess DMF was removed by vac-
uum distillation to obtain the desired PAN/CNT/DMF
solution (1.7 L). The solid (polymer 1 CNT) concentra-
tion of the final solution was 15 g/dL and the CNT con-
tent was 0.5 wt% with respect to the polymer.
Solution B. The CNT slurry preparation for solution B
was the same as solution A, except that SWCNT (SPO300)
was used. The prepared CNT slurry was sonicated for 24 h
without further dilution and then it was transferred to the
separately prepared PAN solution (225 g PAN in 1 L
DMF). Then, the excess solvent was removed by vacuum
distillation while the solution was being stirred. The final
volume of PAN/SWCNT/DMF solution was 1.7 L. The
solid concentration and CNT content was 15 g/dL.
Solution C. For solution C, FWCNT2 (XOC231U) was
used. It should be noted that FWCNT2 was supplied in
wet state with water (98% of weight is water). There-
fore, solvent exchange step was taken to remove water.
This was done by repeating the following procedure three
times. The wet FWCNT2 (50.625 g, equivalent to 1.125 g
dried CNT) was added in 1 L DMF and the mixture was
bath-sonicated for 1 h. The mixture was placed in rotary
evaporator (Rotovapor, Buchi Co.) and 600 mL solvent
(DMF 1 water) was removed under vacuum (20 mbar)
using 70 8C water bath. Then, 600 mL DMF was added
to mixture. The mixture was bath-sonicated for 1 h and
600 mL solvent was evaporated. After completing solvent
exchange, CNT slurry preparation and final solution prep-
aration were the same as solution B.
Solution D. Solution D was the control PAN solution
and prepared by dissolving 225 g polymer in 1.5 L DMF
at 70 8C for 2 h.
All the solutions were kept at 50–60 8C to avoid gela-
tion before extrusion experiment.
Extrusion Experiment
For high-shear mixing, twin-screw extruder (Mini com-
pounder KETSE 12/36D, Brabender Co.) was used. The
configuration of screw assembly is shown in Supporting
Information. It is noted that there are two sets of 6 knead-
ing blocks to apply high-shear mixing effect. Solutions A,
B, and C were extruded for 2, 4, and 8 cycles, respec-
tively. All the heating zones for extruder (8 heating
zones) were maintained at 60 8C and screw speed was set
at 500 rpm. Samples were collected for each cycle for
characterization and the information is listed in Table 1.
Characterizations
Preparative Ultracentrifuge Method (PUM). The
preparative ultracentrifuge method (PUM) was applied to
the PAN/CNT/DMF composite solutions for determining
DOI 10.1002/pc
 TABLE 1. Extrusion processing parameters and the results of CNT dispersion study by DLS and PUM for various PAN/CNT composite solutions.

Sample ID/extrusion
cycle S* (310212 s) D** (310210 cm2/s) Length (lm) Diameter (nm) Length/diameter

A A0/0 14.5 6 2.9 36.6 6 1.83 5.4 6 0.4 8.8 6 1.0 617
A1/1 10.6 6 2.1 41.2 6 2.06 4.8 6 0.3 7.5 6 0.8 646
A2/2 10.0 6 2.0 41.2 6 2.06 4.8 6 0.3 7.2 6 0.9 674
B B0/0 100 6 20 16.5 6 0.83 11.6 6 0.7 23.4 6 2.7 494
B2/2 61.5 6 12.6 20.9 6 1.05 9.1 6 0.6 18.4 6 1.9 495
B4/4 37.4 6 7.5 20.9 6 1.05 9.6 6 0.6 13.9 6 1.6 689
C C0/0 46.0 6 9.2 10.8 6 0.54 20.2 6 1.2 14.9 6 1.6 1355
C2/2 36.7 6 7.3 11.2 6 0.56 20.7 6 1.3 12.9 6 1.4 1606
C4/4 42.1 6 8.4 11.2 6 0.56 20.4 6 1.3 13.9 6 1.5 1467
C6/6 50.0 6 10.0 12.7 6 0.64 17.2 6 1.1 15.5 6 1.7 1108
C8/8 58.2 6 11.6 12.9 6 0.65 16.7 6 1.0 16.8 6 1.9 994

*Sedimentation coefficient; **diffusion coefficient.

the bulk averaged length and diameter of CNT bundles.
Solution series A, B, and C (in specific, solution A0, A1,
A2; B0, B2, B4; C0, C2, C4, C6, and C8) were first
diluted 80 times by weight and stirred for 8 h at 70 8C.
The PUM was then performed according to the experi-
mental procedures described elsewhere [26] with an Opti-
maTM MAX-XP ultracentrifuge instrument (308 fixed
angle rotor, Beckman Coulter, Inc.) and a Cary 5000
UV–vis–NIR spectrometer (Agilent Technologies, Inc.).
The PUM is a sedimentation-based method for quantify-
ing the size of CNTs (bulk averaged length and bundle
diameter) in a dispersion [26, 27], which relies on meas-
uring and analyzing the sedimentation function for a
given CNT dispersion with preparative ultracentrifuge
instrument. The experimentally determined sedimentation
function can be subsequently fitted according to the ana-
lytical sedimentation solution derived by Mason [28] and
Shiragami [29]. Based on the fitting result, the bulk aver-
aged sedimentation coefficient (s) for a given CNT dis-
persion can be obtained. The bulk averaged length and
diameter of CNTs are accordingly calculated by following
the hydrodynamic model of rigid rods given by Yama-
kawa [30] with the PUM-determined s and DLS-
measured diffusion coefficient (D) as detailed below.
Dynamic Light Scattering (DLS). The DLS measure-
ments for the 80-times-diluted PAN/CNT/DMF composite
solution series A, B, and C were carried out at 25 8C
with Delsa Nano C (Beckman Coulter, Inc.) at a fixed
scattering angle of 1668 with a laser of 658 nm in wave-
length. In DLS measurements [31, 32], the time fluctua-
tion of the scattered light intensity, Is(t), is recorded, from
which the time correlation function, g1(s), of the scattered
electric field is accordingly determined and used for
extracting the particle diffusion coefficients with the well-
known CONTIN method [33, 34].
Transmission Electron Microscopy (TEM). The 80-
times-diluted PAN/CNT/DMF composite solution series
A, B, and C were dropped onto TEM copper grids (Lacey
Formvar/Carbon, 300 mesh). Excess solvent was removed
from the back side using filter paper. The samples were
then dried under ambient condition. All the samples were
examined by a JEOL JEM-ARM200F HRTEM with an
acceleration rate of 80 KV.
Optical Microscope and Rheology. Optical microscope
(DM2500P, Leica microsystems Co.) was used to obtain
optical images of various solutions. The image analysis
was conducted using analysis software ImageJ and a
method described in other paper [35]. Dynamic rheologi-
cal properties of solutions were measured by rheometer
(ARES, TA Instruments, Inc.) at room temperature. Paral-
lel plate geometry (25 mm diameter) was used for mea-
surement with a gap of 1 mm. Angular frequency was in
the range of 0.1–500 rad/s.
RESULTS AND DISCUSSION
The optical images for composite solutions before and
after extrusion cycles were shown in Fig. 1. For solution
C, it is clear that CNTs agglomerated into entangled fibril
morphologies. An image analysis method reported else-
where was used to compare the CNT macroscopic disper-
sion in PAN solutions [35]. It is noted that the smaller
FWHM value of the optical image contrast shown in
Fig. 2 suggests better macroscopic dispersion homogene-
ity of CNTs. It can be found that the macroscopic disper-
sion homogeneity of composite solution A was the best
among all the three types of composite solutions. As
noted previously, the CNT/DMF dispersion used for pre-
paring the stock solution A was bath sonicated for 24 h at
a concentration of 30 mg/L before mixing with PAN
solution; whereas, the CNT/DMF dispersions for prepar-
ing solutions B and C were bath sonicated for 24 h at a
much higher concentration (450 mg/L). The improved
CNT macroscopic dispersion in solution A could be
attributed to the lowest concentration of CNT/DMF dis-
persion that was used for preparing A. All solutions
passed extruder for various cycles. The macroscopic dis-
persions of CNT in all solutions were improved after
passing through extruder for 2 cycles (Fig. 2). For

DOI 10.1002/pc POLYMER COMPOSITES—2017 721

 FIG. 1. Optical images of various PAN/CNT composite solutions: (a1, a2) solution A0 and A1, (b1–b3)
solution B0, B2, and B4, (c1–c4) solution C0, C2, C4, and C8, respectively. [Color figure can be viewed at
wileyonlinelibrary.com]

composite solutions passing through extrusion for more For solutions A and B, the sedimentation coefficient
than 2 cycles, the improvement of CNT macroscopic dis- decreased with increasing extrusion cycles. In addition,
persion was not noticeable. the sedimentation coefficient of CNTs in solution A was
The quantitative characterization of CNT bundle size
was carried out by DLS and PUM experiments, where
one can determine diffusion coefficient and sedimentation
coefficient of CNTs in the solution, respectively [26].
The sedimentation coefficient, diffusion coefficient, and
the calculated average length and diameter of CNT bun-
dle are listed in Table 1. Diffusion coefficient is inversely
proportional to the CNT length, and a larger diffusion
coefficient indicates a shorter CNT bundle length. It can
be observed that the diffusion coefficients for solutions A
and B were saturated after one and two cycles of extru-
sion, respectively. For solution C, the diffusion coefficient
was marginally increased even after 8 cycles of extrusion.
Above results indicated a limited dispersion capability of
twin-screw extrusion on CNT bundle size. Sedimentation
coefficient is defined as the ratio of a particle’s sedimen-
tation velocity to the acceleration. The larger the sedi-
mentation coefficient is, the faster the sedimentation FIG. 2. Image analysis results from optical images in Fig. 1. A smaller
process and typically the larger the bundle diameter, since FWHM indicates better macroscopic dispersion of CNTs in a composite
it is proportional to the square of the bundle diameter. solution. [Color figure can be viewed at wileyonlinelibrary.com]

722 POLYMER COMPOSITES—2017 DOI 10.1002/pc

 FIG. 3. High-resolution transmission electron microscope images of various composite solutions: (a) solu-
tion A, (b) solution B, and (c) solution C. It can be noted that CNTs are covered by polymer and CNT bun-
dles (10–20 nm diameter) can be observed. In all cases, individual CNTs are also observed with polymer
wrapping, suggesting good interaction between PAN polymer and CNTs. [Color figure can be viewed at
wileyonlinelibrary.com]

much smaller than that of CNTs in solution B. This is
because of the difference on sonication efficiency in low-
and high-concentration PAN/CNT dispersion as noted ear-
lier. Moreover, solution B exhibits a more profound
decrease of the sedimentation coefficient with the number
of extrusion cycles than solution A. This may be due to
the fact that the initial bundle size of CNTs in solution B
is much larger to render effective debundling by high-
shear mixing. It is also interesting to note that the sedi-
mentation coefficient for solution C decreased in the first
two extrusion cycles and increased afterward, suggesting
that the CNTs rebundled or reaggregated under the pro-
longed high-shear mixing. As noted earlier, the length of
FWCNT2 used to prepare solution C is longer than the
other CNTs [36]. The longer CNT will tend to agglomer-
ate and rebundle easier even under high-shear mixing.
Based on the diffusion coefficient and sedimentation
coefficient results, the average length and diameter of
CNT bundle in the composite solution can be estimated
using the equations with the assumption of rod-like parti-
cle behavior of CNTs described elsewhere [25]. For solu-
tion A, both the average length and diameter of CNT

DOI 10.1002/pc POLYMER COMPOSITES—2017 723

 FIG. 4. Dynamic shear rheological behavior of various PAN/CNT solutions after extrusion experiment: (a1,
a2) solution A, (b1, b2) solution B, and (c1, c2) solution C. [Color figure can be viewed at wileyonlineli-
brary.com]

bundles slightly decreased after extrusion cycles and they
exhibited the shortest and smallest values among three
different solutions. CNTs in solution B showed the largest
bundle diameter (23.5 nm for initial solution), which may
be due to the fact that the CNT used to prepare solution
B was SWNT. However, with increasing extrusion cycle,
SWNT bundle diameter decreased rapidly, and after
fourth extrusion cycle, it was reduced to from 23.5 to
13.9 nm. This may be due to that the SWNT has the low-
est aspect ratio among all type of CNTs, and the exfolia-
tion of SWNT bundles was easier than other CNTs with a
higher aspect ratio. As reported previously [27], the
SWCNT rapidly exfoliates to a critical bundle size of
approximately 10–15 nm during sonication process (0.5–
4 h), and further exfoliation to individual SWCNT
requires a much longer sonication time (4–20 h) and
more energy input. In solution B, the SWCNTs may have
reached the critical bundle size after 4 cycles of extru-
sion. However, FWCNTs in solutions A and C may
already reach their critical bundle size before extrusion

FIG. 5. (a) log G0 vs log G00 plots of the solutions C0 and C8. The angular frequency range is from 0.1 to
10 rad/s. (b) the slopes of log G0 vs log G00 of the solutions as a function of extrusion cycle numbers. [Color
figure can be viewed at wileyonlinelibrary.com]

724 POLYMER COMPOSITES—2017 DOI 10.1002/pc

process, and the energy input was not enough to further
exfoliate them into individual tubes. It is noted that solu-
tion A had the smallest CNT bundle diameter. Similar to
the arguments made previously, this again can be attrib-
uted to that a much lower concentration of CNT/DMF
dispersion (30 mg/L) was used for the preparation of
solution A. Whereas, the concentration of CNT/DMF dis-
persion used for preparing solutions B and C was at very
high concentration (450 mg/L). It is worth noting that the
exfoliation of CNTs may depend on not only the extru-
sion processing conditions but also the intrinsic structures
of CNTs, e.g., SWNT vs FWNT. That is, the extrusion
and the CNT structures have a confounding effect to dic-
tate the exfoliation/debundling behaviors of CNTs.
Figure 3 shows the high-resolution TEM images of
various composite solutions. As seen from Fig. 4a-1, b-1,
and c-1, most CNTs are covered or wrapped by polymer
molecules, and most CNTs are in bundle form. Both
TEM and Raman results (Supporting Information) suggest
that limited CNT exfoliation could be obtained by extru-
sion. Additionally, exfoliated CNTs that were occasion-
ally found in all composite solutions (Fig. 4a2, a3, b2,
b3, c2, and c3) are at least partially wrapped by polymer,
indicating a good interaction between CNTs and PAN.
The rheological properties of the extruded dispersion
samples were measured. The complex viscosity and
tan(d) as a function of angular frequency of all solutions
before and after extrusion are shown in Fig. 4. It was
noted that the complex viscosities of all the composite
solutions decreased with two cycles of extrusion, and
then remained almost constant for more cycles of extru-
sion. The plateau of the solution complex viscosity after
long-time extrusion suggests that the polymer degradation
during extrusion is negligible. Otherwise, the complex
viscosity should decrease continuously after extended
extrusion. Additionally, the loss factor tan(d) at 0.1 rad/s
increased monotonously with increasing extrusion cycle
number. The tan(d) changes suggest that the elasticity of
the composite solutions became weaker after extrusion.
The Han-plots (log G0 vs log G00 ) of solutions C0 and C8
are shown in Fig. 5a. The theoretic value of a homoge-
nous polymer solution or melt has a slope of Han plot
equal to 2 in the low-shear-rate region. From Fig. 5b, the
slope of the Han plot increases with increasing the extru-
sion cycles for all composite solutions, suggesting an
increase in solution homogeneity after passing more
extrusion cycles. The improved solution homogeneity and
reduced elasticity are possibly ascribed to the disentangle-
ment of PAN and CNT networks during high-shear
extrusion.
CONCLUSIONS
The PAN/CNT composite solutions were prepared
using various processing conditions, followed by high-
shear mixing in a twin-screw extruder. The macroscopic
CNT dispersion and solution homogeneity were observed
DOI 10.1002/pc
to be significantly improved after extrusion, although
CNT bundle diameter and length were found to only
moderately reduce. The extrusion has limited ability to
exfoliate CNT bundles, and the pre-extrusion processing,
such as preparation of CNT dispersion, is very important
to achieve small diameter CNT bundles.
ACKNOWLEDGMENT
TEM effort from Dr. Yi-Feng Su in Florida State Univer-
sity is highly appreciated.
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