Journal of The Electrochemical Society, 154 共6兲 H495-H499 共2007兲 H495

0013-4651/2007/154共6兲/H495/5/$20.00 © The Electrochemical Society

Integration and Distribution of Carbon Nanotubes

in Solution-Processed Polyaniline/Carbon Nanotube Composites
Praveen C. Ramamurthy,a William R. Harrell,b,z Richard V. Gregory,c and
Apparao M. Raod
a
Therm-O-Disc, Incorporated, Mansfield, Ohio 44907, USA
b
Holcombe Department of Electrical and Computer Engineering and dDepartment of Physics and
Astronomy, Clemson University, Clemson, South Carolina 29634, USA
c
Department of Chemistry and Biochemistry, Old Dominion University, Norfolk, Virginia 23529, USA

Composites of high-molecular-weight polyaniline 共PANI兲 and single-walled carbon nanotubes as well as composites of PANI and
multiwalled carbon nanotubes of various weight percentages were prepared using solution processing. The integration and distri-
bution of the carbon nanotubes 共CNTs兲 in the PANI matrix were investigated by various characterization methods. CNT distribu-
tion was evaluated using scanning electron microscopy, while CNT dispersion and alignment were characterized by transmission
electron microscopy. The specific gravity of the composite material was measured using a density gradient column, which
indicates how well the nanotubes are integrated into the polymer matrix. Results indicate that effective integration and distribution
of CNTs into a PANI matrix can be achieved with solution processing for composites containing between 1 and 5% CNTs by
weight.
© 2007 The Electrochemical Society. 关DOI: 10.1149/1.2719609兴 All rights reserved.

Manuscript submitted October 24, 2006; revised manuscript received January 22, 2007. Available electronically April 6, 2007.

Since the first report of the preparation of composites of poly-
mers and carbon nanotubes 共CNTs兲,1 there has been considerable
interest in investigating this new class of materials for functional
applications.2,3 The discovery of CNTs has generated significant in-
terest in recent years in carbon-based materials for nanostructure
and materials technology,4 because CNTs are known to possess ex-
ceptional electronic, mechanical, and thermal properties.2,5-7 Simi-
larly, conducting polymers have received much attention for use in
microelectronics due to their high potential to provide low cost,
lightweight, and flexible electronic and photonic materials using
relatively simple processing methods.8-11 Although both CNTs and
conducting polymers have very promising physical properties, there
are significant challenges in bringing them to their full potential in
practical applications. Combining these two materials to form com-
posites can potentially exploit the strengths of each while overcom-
ing some of the challenges involved in utilizing the individual ma-
terials. In fact, it has been shown that nanoengineered conducting
polymer/CNT composites provide synergistic effects, whereby
CNTs enhance the thermal and mechanical stability as well as in-
crease the overall conductivity of the neat polymer.12-15 It has been
suggested that uniformly distributed nanotubes in the polymer act as
nanometric heat sinks, preventing the buildup of large thermal ef-
fects, thereby reducing material and device degradation.16 The po-
tential of these nanocomposite materials has motivated many inves-
tigations into their properties and applications to devices such as
supercapacitors,17,18 sensors,19,20 photovoltaics,21 organic light-
emitting diodes 共OLEDs兲,22 Schottky diodes,23 and transistors.24,25
There are essentially two perspectives with which to view or
approach this class of nanocomposites. Either conducting polymers
functionalize CNTs, or CNTs effectively dope the polymer.2 For
example, incorporating CNTs into a polymer matrix can be an ef-
fective means of fabricating CNT-based devices. CNTs have been
shown to increase the thermal stability and mechanical strength of
conducting polymers as well as to increase their conductivity.16,26-28
Combining the unique properties of conducting polymers and CNTs
into functional nanocomposites offers many opportunities for re-
search into basic materials science as well as technological applica-
tions, and these materials are receiving increasing attention as evi-
denced by recent review papers.2,3
Many conducting polymer materials have been investigated, both
in their neat form and in composites with CNTs. However, polya-
niline 共PANI兲 in particular has attracted a significant amount of at-
tention due to its excellent thermal and environmental stability as
z
E-mail: rod.harrell@ces.clemson.edu
compared to other conducting polymers.29,28 Composites of PANI
and CNTs have been shown to possess promising electronic
properties,27,28,30,31 as well as potential applications in organic poly-
mer electronics.17,23,32-34 Recently we have investigated basic me-
chanical and electrical properties of nanocomposites of high-
molecular-weight PANI and CNTs prepared by solution
processing.35,15 In this paper, we investigate the integration and dis-
tribution of both single-walled carbon nanotubes 共SWNTs兲 and mul-
tiwalled carbon nanotubes 共MWNTs兲 in such composites. This is
accomplished by examining thin films of these materials with elec-
tron and transmission electron microscopy, and by measuring the
change in specific gravity of the nanocomposite with CNT loading
in PANI 共SWNT + PANI and MWNT + PANI兲. The change in spe-
cific gravity of a sample indicates the change in free volume of the
material system, which indicates how well blended the nanotubes
are in the composite material.
Experimental
Chemicals used.— Aniline 共99%兲, from Fisher, was distilled un-
der reduced pressure prior to the synthesis of PANI. Hydrochloric
acid 共37%兲, ammonium persulfate 共99%兲 from Aldrich,
N,N⬘-dimethyl propylene urea 共DMPU兲 from Lancaster, and lithium
chloride from Mallinckrodt were used as received.
PANI synthesis.— PANI was chemically synthesized by oxida-
tive polymerization of aniline. The synthetic method described by
Beadle et al., Y. Wei et al., and M. Angelopoulos et al. was
investigated,36-38 and then a combined procedure incorporating this
method was adopted to obtain high-molecular-weight PANI. The
procedure followed is summarized in Fig. 1. Aniline 共C6H5–NH2兲 is
polymerized by oxidation with ammonium persulfate in aqueous
hydrochloric acid solutions at subzero temperature in the presence
of LiCl.
PANI synthesis was performed in a nitrogen atmosphere. Aniline
was purified by immersing potassium hydroxide 共KOH兲 pellets into
aniline followed by continuous stirring for 24 h to remove moisture.
After 24 h, aniline was filtered to remove the potassium hydroxide
pellets. Filtered aniline was then double distilled at reduced pres-
sure. The purified aniline was mixed with 1.0 M hydrochloric acid
and kept at −30°C ± 1°C. 6 M lithium chloride was added to re-
duce the freezing temperature of the mixture. This aniline solution
was kept in a Cryocool immersion cooler, CC100-II, with isopro-
panol as the cooling agent. A mixture of ammonium persulfate
共APS兲 关共NH4兲2S2O8兴, also in 1.0 M HCl, and 6 M LiCl was pre-
pared and kept at −30°C. When the temperature of the reaction
mixture was stabilized to −30°C, polymerization was initiated by

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 H496 Journal of The Electrochemical Society, 154 共6兲 H495-H499 共2007兲
Figure 1. Flow chart of the PANI synthesis procedure adopted in this work.
adding the ammonium persulfate solution to the stirred aniline solu-
tion at the rate of 3 mL/min using an external pump. The tempera-
ture of this reaction was controlled at −30°C ± 1°C. Open-circuit
potential 共OCP兲 and temperature of the reaction mixture were mea-
sured and recorded continuously during the syntheses. A Keithley
2000 multimeter connected by means of Pt and Ag/AgCl reference
electrodes was used to monitor the redox potential of the reaction
similar to the method of Wei et al.37 A Ag/AgCl reference electrode
immersed in solution was mounted using an intermediary custom-
made LiCl electrolytic bridge.
Several oxidative polymerization mechanisms of PANI have
been proposed. According to the mechanism proposed by Y. Wei et
al.,39 the oxidizer in the reaction mixture oxidizes aniline and simul-
taneously oxidizes the growing polymer chain. The oxidation poten-
tial of the monomer and that of the growing chain are different.
Once most of the aniline is oxidized, oxidation of the growing chain
predominates. This is an exothermic reaction and is indicated by a
change in oxidation potential.37 When a drop in potential and an
increase in the temperature of the mixture were observed, the reac-
tion was quenched by adding excess aniline to the mixture, which
was kept at −30 ± 1°C. From the quantity of APS used in the reac-
tion, the aniline to oxidant molar ratio was found to be 0.7:0.5. The
total reaction time was 6 h. The reaction mixture was continuously
stirred during polymerization, and in the course of the reaction, the
color of the mixture turned from pink to copper; however, toward
the end of the reaction, the mixture turned from green to coppery
blue indicating the progress of the reaction.39 The reaction mixture
was separated by vacuum filtration, and the resulting coppery blue
precipitate, which is emeraldine salt, was washed repeatedly with
deionized water. The emeraldine salt was deprotonated by stirring in
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3 wt % ammonium hydroxide 共NH4OH兲 for 18 h to produce emer-
aldine base 共EB兲. EB was then washed with deionized water and
methanol repeatedly to remove any oligomers, until the extracted
solution became a light blue color which is indicative of decreasing
oligomer concentration. Finally, copious amounts of deionized water
were used to vacuum filter the remaining methanol. The purified EB
powder was vacuum dried at 50°C and the yield obtained was ap-
proximately 40%. The weight average molecular weight was deter-
mined by gel permeation chromatography using polystyrene stan-
dards with N-methyl-2-pyrrolidinone 共NMP兲 and LiBr 共0.05 M兲 as
the eluent at a column temperature of 80°C. This secondary weight
determination method yielded a weight average molecular weight of
135,000, with a polydispersity index of 3.
CNT synthesis.— Chemical vapor deposition 共CVD兲 is one of
the most promising methods for the synthesis of CNTs because of
the many advantages that mass production, high purity, selective
growth, and vertical alignment at relatively low temperature
provides.40,41 This method involves controlled decomposition of hy-
drocarbons 共xylene, benzene, or toluene兲 over substrates coated with
thin films of transition metals 共Fe, Ni, Co兲. The MWNTs used in this
work were produced from a solution of o-xylene containing fer-
rocene 共with ⬃0.75 atom % Fe/99.25 atom % C ratio兲, which was
fed continuously into a two-stage tubular quartz reactor 共operated at
near atmospheric pressure兲 using a syringe pump at a rate of
1 mL/h. In this CVD process, the synthesis apparatus consists of a
quartz tube reactor inside a combined preheater and furnace setup.
The xylene-ferrocene mixture is introduced inside the reactor
through a syringe and is carried by a gas flow of Ar/10% H2.40 The
reaction temperatures are in the range of ⬃700 to 800°C, which is
sufficient to break the transition metal film into nanosized particles
on the quartz substrates. The hydrocarbon decomposes over these
nanosized particles to seed the growth of CNTs. The MWNTs grow
perpendicular to the quartz substrates and form thick mats that are
readily harvested.40 The deposits are routinely extracted and charac-
terized using scanning electron microscopy 共SEM兲 and transmission
electron microscopy 共TEM兲 in order to verify the purity of the nano-
tubes. The as-prepared nanotubes were suspended in ethanol and
sonicated for better dispersion.15 These dispersed MWNTs were
used in the fabrication of the composite materials presented in this
paper.
SWNT bundles were prepared by the electric arc discharge
method, as described in Ref. 17. This method provides a simple tool
for generating the high temperatures needed for the vaporization of
carbon atoms into a plasma 共⬎3000°C兲.42,43 The SWNTs in this
work were prepared by striking an electric arc discharge between a
catalyst-impregnated graphite cathode and a graphite anode in a he-
lium atmosphere.
Sample preparation.— A PANI 共EB兲 solution 共3.5 wt % EB兲
was prepared at room temperature by dissolving the EB powder in
DMPU. It has been shown that DMPU is a better solvent than NMP
for preparing stable solutions of PANI.44 The EB powder was added
slowly into the solvent, using a powder funnel, over several days to
avoid gelation. The PANI solution was then processed through a
50 ␮m filter to create a smooth, consistent stock solution.38 From
the stock solution, equal quantities of PANI were collected in small
glass bottles, and the quantity of PANI by weight was calculated.
Composite solutions were prepared with various mass fractions of
CNTs in PANI. MWNTs and SWNTs of 0.5, 1, 5, and 10 wt % of
PANI, measured to five decimal places, were gradually added to
these PANI solutions. These mixtures were further stirred for 24 h.
From the solution prepared, 0.2 mL of the composite solution was
poured onto glass slides in order to form thin films. The slides were
then dried under a vacuum of 20 mm Hg at 50°C for 360 h in order
to effectively remove the solvent by evaporation, which is a crucial
step in obtaining stable electronic properties.45 The thickness of the
resulting freestanding films was determined to be 15 ± 2 ␮m. Dop-
ing of the dried composite films was achieved by a vapor deposition
 Journal of The Electrochemical Society, 154 共6兲 H495-H499 共2007兲
Figure 2. SEM micrograph of the edge of a PANI/MWNT composite film.
technique,46,47 where the films were exposed to a 1 M HCl solution
for 48 h at room temperature in a closed chamber. For convenience,
the following nomenclature has been adopted in this paper
for MWNT composites: PM-1 = 100% PANI, PM-2 = 99.5%
PANI + 0.5% MWNT, PM-3 = 99% PANI + 1% MWNT,
PM-4 = 95% PANI + 5% MWNT, and PM-5 = 90% PANI + 10%
MWNT; while for SWNT composites: PS-1 = 100% PANI,
PS-2 = 99.5% PANI + 0.5% SWNT, PS-3 = 99% PANI + 1%
SWNT, PS-4 = 95% PANI + 5% SWNT, and PS-5 = 90% PANI
+ 10% SWNT.
Nanocomposite samples for TEM imaging were fabricated by
microtoming a standard epoxy mold. Small samples of the free-
standing films were mounted in an epoxy mold which was cured at
an elevated temperature. From the pointed end of these prepreg
materials, thin slices of the samples were obtained.
Instrumentation.— A Hitachi S4800 field emission scanning
electron microscope 共SEM兲 was employed for imaging the samples.
Specimens for the SEM were prepared by tearing the composite
films instead of cutting. Tearing is preferred because it assists in
pulling the nanotubes at the interface, in contrast to chopping the
protruding nanotubes while cutting, which would make them diffi-
cult to identify in a SEM micrograph. Composite samples were
mounted on double-sided carbon tape on an SEM stub. The stub was
placed in a platinum coater to assist in easier electron mapping of
the surface and to reduce charging of the sample. Once the platinum
coating was complete, specimens were viewed on the SEM. The
instrument was operated at an accelerating potential of 1 kV and an
8 mm working distance.
TEM studies were conducted using a Hitachi H7600T TEM at
120 kV and a Hitachi 9500 TEM at 300 kV. From the cured epoxy
mold, cross sections of the samples were obtained using a Riechert
Ultramicrotome equipped with a diamond cutter. The cross sections
obtained ranged in thickness from approximately 100 to 150 nm for
use in the 120 kV TEM, and from approximately 130 to 180 nm for
use in the 300 kV TEM. Sectioning of the thicker samples was
performed to ensure that the CNTs would not fracture, and to facili-
tate higher magnification imaging at 300 kV.
Specific gravity of the composite material was measured using a
density gradient column using liquids of known specific gravity.
The density gradient column was prepared by using xylene
共d = 0.866 g/cm3兲 and carbon tetrachloride 共d = 1.584 g/cm3兲.
PANI film samples were tested for nonreactivity with the solution.
Films of a specific size and weight were introduced into a glass vial.
Size and weight of the samples were monitored for about 3 weeks.
The standard apparatus consists of a 1000 mm long glass column
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H497
Figure 3. TEM micrograph, 120 kV, of a PANI/MWNT composite film.
tube containing the solution of xylene and carbon tetrachloride,
which has a linear density gradient from the top 共lower density兲 to
the bottom 共higher density兲 of the column.
The specific gravity test was carried out as described in ASTM D
1505. The column was prepared by making layers of mixtures of
xylene and carbon tetrachloride. First, 20 mL of carbon tetrachloride
was poured to the bottom of the column which is clamped into a
vertical position. Then the mixtures of carbon tetrachloride/xylene
were prepared in various volumetric ratios V/V: 90/10, 80/20,
70/30, 60/40, 50/50, 40/60, 30/70, 20/80, and 10/90. Each mixture
was carefully poured down the sides of the gradient tube to avoid
mixing of the layers. Finally, 20 mL of xylene was poured onto the
top of the column. Standard density markers in the form of glass
beads obtained from American Density, Inc., along with various
nanocomposite film samples, were dropped into the column slowly
using a wire mesh attached to a string. The glass beads will stop
their descent when they reach the corresponding specific gravity.
The specific gravity of the PANI/CNT composite films was deter-
mined by comparing the position of the films with that of the stan-
dard glass beads.
Results and Discussion
The distribution of the CNTs is an important factor when they are
used to fabricate a composite material. For a nanocomposite consist-
ing of a conducting polymer and CNTs to behave uniformly, the
nanotubes must be well distributed within the polymer matrix. Elec-
tron microscopy is a useful tool for investigating nanotube distribu-
tion in a host matrix. Figure 2 shows a typical SEM image of the
edge of a torn sample of a PANI/MWNT composite film. Individual
MWNTs are observed protruding from the core of the polymer film.
None of the multiwalled CNTs were observed on the surface, indi-
cating the absence of aggregation as well as the migration of the
nanotubes to the top or bottom surfaces. This figure indicates that
the nanotubes are well dispersed within the PANI matrix. Similar
results were observed for PANI/SWNT composite films.
 H498 Journal of The Electrochemical Society, 154 共6兲 H495-H499 共2007兲

Figure 5. Specific gravity measurements of PANI/MWNT composite films

against standard glass beads in a density gradient column. The best fit line
equation along with the correlation coefficient are also shown.

ferent nanotube concentrations, both single and multiwalled, to

avoid cumbersome labeling. In the case of the PANI/SWNT
composites, the specific gravity decreases from 1.334 g/cm3 for P-1
共neat PANI兲 to 1.264 g/cm3 for P-2, indicating the formation of
voids and free space due to less efficient packing of the two mate-
rials. With a further increase in SWNT loading, the SWNTs appear
Figure 4. TEM micrograph, 300 kV, of a PANI/MWNT composite film. to incorporate well within the PANI matrix, decreasing the voids and
free space as indicated by the increase in specific gravity for 1 and
5% loaded composites. For composites containing 10% SWNTs, the
specific gravity increases sharply to 1.371 g/cm3. This indicates that
The dispersion and the alignment of CNTs inside a polymer ma-
the high concentration of nanotubes mixes well in the PANI matrix,
trix can be well characterized by TEM, and this technique was used
forming a composite of continuous phase. This supports the data
to study several samples of the PANI/MWNT composite material. In
from electrical measurements on such materials that a 10% loading
Fig. 3 an image of a composite material sample is shown which was
of SWNTs in PANI is above the percolation limit, and thus the
taken at 80 K magnification on the 120 kV TEM instrument, while composite behaves like a conductor.17 Similarly for the PANI/
in Fig. 4 an image of a composite material sample is shown which MWNT composites, the specific gravity decreases with nanotube
was taken at 20 K magnification using the 300 kV instrument. Both concentration up to 5%; however, the change is very small, indicat-
of these micrographs clearly demonstrate that the majority of the ing that the MWNTs integrate well within the PANI matrix for all
CNTs are well dispersed, and the absence of clusters or agglomer- but the highest nanotube loading. For composites containing 10%
ates of CNTs is apparent in these TEM images. In Fig. 3 and 4 it is MWNTs, however, the specific gravity decreases contrary to the
evident that most of the nanotubes are about 26–80 nm in diameter, SWNT composite, indicating the MWNTs do not integrate well at
and these multiwalled nanotubes are separated from each other for
the most part. Only a few of them are dimerized, and a couple of
them are grouped together with three or more nanotubes with an
aggregate size of about 100–200 nm. Furthermore, such images in-
dicate good adhesion between the CNTs and the PANI matrix, which
is important for good performance of the material in electronic
applications.48 Similar results were observed from nearly 20 other
images of these nanocomposites.
Specific gravity was measured using the standard glass beads of
known density as a reference, and the change in specific gravity with
nanotube concentration in PANI/MWNT and PANI/SWNT nano-
composite films was determined. The specific gravity values indicate
how densely the material is packed within a given volume. This
indicates how well the nanotubes are integrated into the polymer
matrix without the formation of any entrapped voids, i.e., free space.
In Fig. 5, the specific gravity measurements of some PANI/MWNT
composite films are shown along with the standard glass beads. This
graph illustrates the linearity of the specific gravity gradient column Figure 6. Specific gravity measurements of both PANI/MWNT and PANI/
constructed. The best fit line, the equation of which is listed in Fig. SWNT composite films.
5, yields a correlation coefficient of R2 = 0.9994, and the specific
gravity values of the composite films follow the linear curve quite Table I. Specific gravity measurements of the PANI/CNT
well, indicating that the density gradient column is of robust design nanocomposites.
and construction for measuring the specific gravity of materials in
the range of 1–1.5 g/cm3. Similar results were obtained for mea- Samples P-1 P-2 P-3 P-4 P-5
surements on PANI/SWNT films. In Fig. 6, the relative changes in PANI/MWNT 1.334 1.327 1.322 1.320 1.293
specific gravity with CNT concentration for both the PANI/SWNT composite g/cm3
and PANI/MWNT composites are shown. The measured numerical
values are also summarized in Table I. In both Fig. 6 and Table I we PANI/SWNT 1.334 1.264 1.304 1.304 1.371
have used the general notation P-1 through P-5 to refer to the dif- composite g/cm3

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 Journal of The Electrochemical Society, 154 共6兲 H495-H499 共2007兲
this loading. Therefore, these measurements indicate that this
method of preparing nanocomposites of PANI and CNTs results in
well-integrated films as long as the nanotube loading is not too
large.
Conclusions
These experimental results illustrate that effective integration of
CNTs into a PANI matrix can be achieved with the solution mixing
technique. Furthermore, specific gravity measurements illustrate that
nanotubes disperse and mix well within the polymer matrix in com-
posites containing between 1 and 5% CNTs. This supports the data
from earlier work on the electronic properties of PANI nanocompos-
ites showing that a composition of between 1 and 5% CNTs is
optimal for application to microelectronics.17,15
Acknowledgment
The authors thank Dr. JoAn Hudson of the Clemson University
Electron Microscope Facility for performing the TEM sample prepa-
ration and imaging.
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