Advances in Chemical Engi neering and Science , 2011, 1, 140-146
doi:10.4236/aces.2011.13021 Published Online July 2011 (
Copyright © 2011 SciRes. ACES
Supported TritonX-100 Polyaniline Nano-Porous
Electrically Active Film onto Indium-Tin-Oxide
Probe for Sensors Application
Raju Khan
Analytical Chemistry Division, North East Institute of Science & Technology,
Council of Scientific & Industrial Research, Jorhat, India
Received April 8, 2011; revised May 13, 2011; accepted May 29, 2011
Supported tritonX100 polyaniline nano-porous electrically active film has been fabricated successfully onto
indium-tin-oxide conducting probe using electrochemical polymerization process. The doping of TX-100 in
the polymeric network of PANI was suggested using cyclic voltammeter, UV-vis spectroscopy, and Fourier
Transform Infrared spectroscopy. The change in the surface morphology of PANI thin film due to incorpora-
tion of tritonX-100 was investigated using Atomic Forced Microscopy and porosity has been confirmed
scanning electron microscopy, respectively. The surface morphology, uniformly disperse hexagonal close
packing of TX-100 in PANI matrices due to the incorporation of TX-100 in polymeric network of PANI was
confirmed by Atomic Force Microscopy. The electrical conductivity of PANI-TX-100 increases from 1.06 ×
10–2 S/cm–1 to 4.95 × 10–2 S/cm–1 as the amount of TX-100 increases during the polymerization. The change
in the morphology and electrical conductivity of PANI due to incorporation of TX-100 prove as a promising
material for the sensing application.
Keywords: Electrochemical Polymerization, Non ionic surfactant, Conducting Polyaniline, Atomic Force
Microscopy, Scanning Tunneling Microscopy
1. Introduction
The unique optical and electrical properties of conduct-
ing polymer make them a novel organic semi conducting
material with great promise of their wide range of poten-
tial application includes storage batteries [1,2], electro-
chromic devices [3,4], light emitting diodes [5], non lin-
ear optics [6], and corrosion inhibitors [7] and sensors
[8-11]. Among the conducting polymers, polyaniline
(PANI), has attracted the interest of the researchers be-
cause of its good stability in air [12], simplicity of dop-
ing [13], improved electronic properties [14], electro
chromic effect [15], well behaved electrochemical prop-
erties [16,17] and moderately high conductivity in the
doped state [18]. The changes in electrical and optical
properties with interaction of oxidizing or reducing agents
make them suitable for sensing applications. However,
the difficult processability and poor thermal stability of
PANI has to overcome for the successful application in
sensors. In order to overcome this obstacle, different
strategies for synthesis of PANI with colloids are a better
alternate. Better processability may be achieved either by
the synthesis on PANI in nano-micro scale particle,
which are easier to disperse in a polymer matrix or by
using an appropriate emulsifier which enhance the opti-
cal and electrical properties of PANI. Polymeric stabiliz-
ers (surfactant) affect the polymerization condition, ki-
netics, and also the final properties of the polymer
[19,20]. Surfactants used as additives during the polym-
erization of aniline to effect the locus polymerization by
using the emulsion [21,22] or inverse emulsion [23-25]
pathways, and thus to modify the molecular and super-
molecular structure of the resulting PANI, and to im-
prove the properties of the PANI with respect to conduc-
tivity, stability, solubility in organic solvents, and proc-
essibility. Surfactants have important implications in
wetting, formation of foams, etc., in addition to aggrega-
tion of surfactants at interfaces [26]. Polymeric nanos-
tructures are formed on surfaces due to combination of
interfacial, intra- and intermolecular forces [27].
Copyright © 2011 SciRes. ACES
Surfactants affect the preparation of PANI in three
ways: 1) the presence of surfactant micellar and aqueous
phases, thus altering the locus and the course of polym-
erization [23,28], 2) anionic surfactants may act as
counter ions for conducting-polymer polycations, and 3)
the hydrophobic part of the surfactant molecules may
adsorb on the produced conducting polymer, a surfactant
thus becoming a part of the resulting material. The role
of non-ionic surfactants, e.g. those based on poly (ethyl-
ene oxide) and Triton X-100 (TX-100) are less frequent
and those dealing with cationic types are rare in the lit-
erature [29-31]. The nonionic surfactant Triton X-100
(TX-100) is a commercial product obtained by ethoxyla-
tion of p-(1,1,3,3-tetramethylbutyl) phenol and contains
9.5 oxyethylene units per molecule [32]. There are sev-
eral theoretical [33-35] and experimental [31] studies
concerning micellar properties of the TX100 system.
PANI with TritonX-100 chemical synthesis has been
reported [36,37]. However, no attempts have been made
electrochemically polymerization towards the prepara-
tion of conductive thin film of PANI with the nonionic
surfactant i.e., Triton X-100. In this study, we are re-
porting electrochemical polymerized conductive thin
film of PANI-Triton X-100, [4-(1,1,3,3-tetramethylbutyl)
phenyl polyethylene glycol, TX-100]. The effect of the
nonionic surfactant i.e., TX-100 on the electropolymeri-
sation of aniline (An), at different surfactant ratios and
potential windows is investigated. The doping of TX-100
changes the surface morphology of PANI. It is also
found that electrical conductivity of PANI-TX-100 was
better then that of PANI and governed by changing the
concentration of surfactant during the polymerization of
aniline. The present methods have been simpler, less
expensive and more convenient route to electrochemi-
cally synthesize PANI nanostructures with tunable elec-
trical properties.
2. Experimental Section
2.1. Materials and Methods
Hydrochloric acid (32%) and aniline monomer (99.5%)
of analytical grade were purchased from Fluka, India,
respectively. Nonionic surfactants i.e., TritonX-100 (TX-
100, 99%) was purchased from Sigma Aldrich, USA.
Other chemicals, NaH2PO4·H2O, Na2HPO4, HCl, and
NaOH were from Fisher. Aqueous solutions were pre-
pared using analytical grade regents and 18Mcm- resis-
tance water (NANO pure Diamond, Barnstead, Dubuque,
IA). Sodium phosphate buffer solution (50 mM, pH 7.0,
containing 0.9% NaCl) was prepared and used as com-
mon supporting electrolyte for cyclic voltametry experi-
ments. Most measurements were carried out in a phos-
phate buffer (50 mM, pH 7.0, containing 0.9% NaCl)
supporting electrolyte medium. Electrochemical polym-
erization and cyclic voltametric measurements were car-
ried out using Potentiostate/Glavan-ostat (Princeton Ap-
plied Research model).
2.2. Thin Film Formation
Polymerization of aniline on ITO electrode was carried
out by electrochemical methods by applying an appro-
priate oxidation potential. In this study, chronoam-
perommetry method has been used for film formation by
adjusting potential at –0.2 to 0.9mV in 150 seconds from
solutions containing 0.2M aniline into 1M HCl solution
prepared in 10mL of de-ionized water. Aniline in elec-
trolyte was added to support electrochemical polymeri-
zation of TritonX-100 at different (0.05, 0.1, 0.2, and 0.4
M in 0.2 M aniline based 1M HCl solution). The active
electrode surface area for sensor was 0.25cm2 which was
controlling by placing a physical mask during thin film
2.3. Surface Characterization
The structural properties of electrochemically polymer-
ized PANI-TX-100 films have been characterized using
Fourier Transform Infrared spectrophotometer (Perkin
Elmer) in the frequency range from 400 - 4000 cm–1.
UV-visible spectrophotomer (Ocean Optics) in the wave-
length range from 300 - 1000 nm is used to study the op-
tical properties of deposited thin films. The surface mor-
phology of thin film was investigated using Atomic
Force Microscopy (AFM). Atomic Force Microscopy
(AFM, Digital Instruments, Multi mode III) was used
under the tapping mode. The surface conductivities of rec-
tangular materials pallet were measured using four- point
probe method by Kithley four-probe system with 224
programmable current source, 181 nano voltameter and
195A digital multimeter.
3. Results and Discussion
3.1. Optical Properties
The UV-visible absorption spectra of electrochemically
polymerized thin film of PANI doped with HCl and
TX-100 is shown in Figure 1(A). The absorption band at
320 nm is attributed to the л-л* transition within benzoid
segment (excitation of the nitrogen atom in benzoid
segment) and at 420 nm is related to the polaron band -
л* transition in of PANI (protonation in PANI backbone,
polaron/bipolaron transition that occurred in doped
PANI). The absorption band at 850 nm is assigned to the
Copyright © 2011 SciRes. ACES
л-localised polaron bands of doped PANI in its emar-
aldine salt form (conductive emaraldine salt state of
PANI is represented by the letter two absorption bands)
[8-11]. The absorption band at 320 nm and 440 nm are
merged with the broadness in PANI-TX-100 and shifted
towards the higher wavelength. The broadness and the
intensity of merged absorption band increases on further
increasing the amount of TX-100 during the polymeriza-
tion. This may be due to the overlapping of absorption
band due to the л-л* electronic transition in PANI and
TX-100 and affinity of TX-100 with PANI matrices.
This also may be due to the interaction of TX-100 with
the benzoid ring system of PANI. This interaction of
TX-100 with PANI will support conjugation (i.e., delo-
calization of electron in the polymeric network of PANI)
and decrease the band gap of PANI. A little shift in the
absorption band at 850 nm towards the lower wavelength
is observed with the introduction of TX-100 into the
polymeric network of PANI. The intensity of this ab-
sorption band is increases on further increasing the
amount of TX-100. This shows that TX-100 stabilized
the quinoid ring system of PANI and PANI-TX-100 is
found in the doped state.
Figure 1(B) shows the infrared transmission spectrum
of electrochemically polymerized thin film of PANI-HCl
and PANI-TX-100 in the frequency range from 800 to
1700 cm–1. The infrared peak at 1570 and 1469 cm–1 are
assigned to the non-symmetric vibration mode of C=C in
quinoid and benzenoid ring system in polyaniline respec-
tively. The C-N stretching vibration mode in aromatic
amine nitrogen (quinoid system) in doped polyaniline is
observed at 1297 cm–1, which is corresponds to the oxi-
dation or protonation state of emareldine salt form [9,10].
The absorption band at 1237 cm–1 is attributed to C-N
stretching vibration mode in benzenoid ring system of
polyaniline assigned to conducted protonated form. The
absorption band at 1156 cm–1 is assigned to in-plane vi-
bration of C-H bending vibration mode in N=Q=N,
Q-N+H-B or B-N+H-B (where Q=quinoid and B=ben-
zenoid). This absorption band should occur during the
polymerization i.e., polar structure of the conducted pro-
tonated form. The absorption bands at 884 and 816 cm-1
are attributed to the aromatic ring and out of plane C-H
deformation vibrations for 1,4-disubstituted aromatic ring
system. The infrared spectrum of PANI-TX-100 consist
the entire absorption band, markers of PANI along with
the characteristics infrared band markers of TX-100 at
1600, 1460, 1351, 1298, 1246, 1184, 1124 and 953 cm–1.
The infrared markers at 1246 cm–1 of PANI are retained
in PANI-TX-100 with the sharp intensity. It means TX-
100 is doped inside the polymeric network of PANI and
may enhance the properties of resulting polymer. The
doping of TX-100 may also be proved by the breading of
infrared absorption at 1124 cm–1 (corresponding to ether
linkage in TX-100 PANI-TX-100. The small shift in the
peak position and intensity might be due to the level of
doping and nature of dopant in the resulting polymeric
network of PANI. The shift in the peaks position of
PANI towards the lower wavenumber by introducing the
TX-100 is may due to the weak interaction forces (hy-
drogen bonding and vander Waal forces etc.) between
TX-100 and PANI matrices. TX-100 supports the poly-
meric network of PANI this is proving by the shift in the
absorption bands at 884 and 816 cm–1 towards the higher
wave number.
300 400 500 600 700 800 900
Wavelength (nm)
8001000 1200 1400 1600 1800 2000 2200 2400
T (%)
Wavenumber (cm-1)
(A) (B)
Figure 1. (A) UV-vis spectra electrochemically polymerized thin film of (a) PANI-HCl/ITO (b) PANI-TX100/ITO (0.05M)
and (c) PANI-TX100/ITO (0.1M) and (B) FTIR spectra electrochemically polymerized thin film of (a) PANI-HCl/ITO (b)
PANI-TX100/ITO (0.05M) and (c) PANI-TX100/ITO (0.1M).
Copyright © 2011 SciRes. ACES
3.2. Atomic Force Microscopy
The surface morphology of electrochemically deposited
thin film is shown in Figure 2(a) PANI (b) PANI-
TX-100 (0.05M) and (c) PANI-TX-100 (0.1M) investi-
gated using AFM. The AFM micro images shows that
TX-100 are uniformly dispersed as hexagonal closed
packing into the PANI matrices and TX-100 phase and
PANI phase are found to be strictly interconnected with
no major macroscopic phase separation. This proves that
incorporation of TX-100 change the surface morphology
of PANI i.e., plane morphology changes into the rough
surface. This changed morphology of PANI with em-
badation of TX-100 in PANI matrices may use in sensing
3.3. Scanning Electron Microscopy
The surface morphologies of (a) PANI/ITO, (b)
PANI-TX100/ITO (0.05M) electrode and (c) PANI-
TX100/ITO (0.1M) electrodes have been investigated
using Scanning Electron Microscopy (SEM) respectively.
SEM of PANI film shows porous non-uniform sponge
like, rough structure (Figure 3(a)) wherein, a new regu-
lar cage like network appears after the introduction of
TX-100 in PANI backbone (Figures 3(b) and (c)) sug-
gesting that TX-100 is uniformly distributed in PANI
matrix. After the increase of TX-100, cage like mor-
phology of PANI-TX-100 has been changes into another
regular uniform porosity form resulting due to coverage
of available active cites on PANI film surface by TX-100.
It may be noted that the affinity of TX-100 is very strong
with PANI and its incorporation in PANI. The porous
surface morphology has suitable advantage for enzymes
and antibodies immobilizations are expected to adsorb
strongly on the surface of PANI-TX-100.
3.4. Electrical Conductivity Measurements
The results of electrical conductivity electrochemically
polymerized PANI thin film prepared in the presence of
nonionic surfactants TX-100 are summarized in Table 1.
An increase in the electrical conductivity of PANI is ob-
served on further increasing the concentration of TX-100
during the polymerization of aniline. It’s suggested the
electrochemical process for PANI is based on radical
cation intermediate coupling and the surfactant mole-
cules provide a hydrophobic effect preventing the poly-
mer degradation, and thus improving the degree of
structural order of PANI film [38]. The TX-100 may
neutralize or stabilized the polymer chain that may en-
hance the polarons transfer, which leads to increase in
conductivity. Thus the increase in the electrical conduc-
tivity of PANI –TX-100 is due to the doping of TX-100
in the polymeric network of PANI that may support the
delocalization of electron within the PANI metrices. This
change in the electrical conductivity with concentration
of dopant proves that TX-100 doped PANI may be used
as a sensing material.
Figure 2. Atomic force microscopic images of (a) PANI-HCl/ITO (b) PANI-TX100/ITO (0.05M) and (c) PANI-TX100/ITO
Figure 3. Scanning electron microscopy images of (a) PANI-HCl/ITO (b) PANI-TX100/ITO (0.05M) and (c) PANI-
TX100/ITO (0.1M).
Copyright © 2011 SciRes. ACES
Table 1. Electrical conductivity of PANI and PANI-TX-100 thin film on to indium-tin-oxide probe.
S. No. Matrix Added (TX-100) Temperature
(˚C) Electrical conductivity
1 PANI-HCl No TX-100 30˚C 2.36 × 10–3 S/cm
2 PANI-TX-100 0.05 M 30˚C 1.06 × 10–2 S/cm
3 PANI-TX-100 0.1 M 30˚C 1.38 × 10–2 S/cm
4 PANI-TX-100 0.2 M 30˚C 2.59 × 10–2 S/cm
5 PANI-TX-100 0.4 M 30˚C 4.95 × 10–2 S/cm
3.5. Cyclic Voltammogram Analysis
In the Figure 4 shows CV of PANI and PANI-TX-100
matrix at PBS (50mM, pH 7.0, containing 0.9% NaCl) at
constant 30 mVs–1 scan rate. The PANI layer was seen to
be redox active in the potential region –200 to +900 mV
was studied, exhibiting three sets of redox peaks. Ini-
tially, the oxidation of aniline occurred at approximately
+800 mV resulting due to nucleation of PANI. During
subsequent scans the oxidation of aniline occurred at
lower potentials due to the catalytic effect of PANI,
which resulted in deposition of polymer on the electrode
surface. Redox couples peaks were attributed to intrinsic
redox processes of the polymer itself. The redox couple
peak occurred at approximately +200 mV and is attrib-
uted to the transformation of PANI from the reduced
leucoemeraldine (LE) state to the partially oxidized em-
eraldine state (EM). The redox couple peak at approxi-
mately +800 mV corresponds to transition of the PANI
from LE to pernigraniline (PE) state, and is accompanied
by the oxidation of aniline monomer [39]. The redox
couple peak at approximately +500 mV, which is ge-
neally attributed to the redox reaction of p-benzoquinone
-2000200 400 600 800
Potential (mV)
-2000200 400 600 800
Potential (mV)
Figure 4. Cyclic Voltammogram of (a) PANI-HCl/ITO (b)
PANI-TX100/ITO (0.05M) and (c) PANI-TX100/ITO (0.1M)
using as supporting electrolyte PBS (50mM, pH 7.0, con-
taining 0.9% NaCl).
[40], is less intense. The cathodic and anodic peak posi-
tions of PANI-TX-100 thin film shifted and increase the
charge transfer appreciably corresponding to PANI-HCl
are shown in the curve (b). This increase in current was
due to fast redox process at PANI-TX-100 matrix surface.
Difference between cathodic (Epc) and anodic peak (Epa)
shift (Ep = Epa - Epc) was use to determine the kinetics
of electron transfer in these matrixes. This may be due to
electrostatic interactions between the head group of
TX-100 and charged aniline at the hydrophilic interface
of the micelles.
4. Conclusions
Electrochemical polymerization process was used for
stable thin film deposition of TX-100 with PANI. TX-
100 molecules in PANI had enhanced charge transfer
and current voltage characteristics at electrode interface.
Increases in oxidation peak current and enhanced broad-
ening were observed due to fast redox process in PANI-
TX-100 matrix. UV-vis and FTIR spectroscopy confirms
the interaction of TX-100 in PANI matrices. The electri-
cal conductivity of PANI-TX-100 thin film increases on
further increasing the concentration of TX-100 during
the polymerization of aniline. AFM and SEM studies
show the incorporation of TX-100 in PANI matrices that
changes the surface morphology of PANI. The change in
surface morphology and electrical conductivity of PANI-
TX-100 with the concentration of TX-100 shows the
potential for sensing application. The electrical conduc-
tivity of PANI-TX-100 increases from 1.06 × 10–2 S/cm–1
to 4.95 × 10–2 S/cm–1 as the amount of TX-100 increases
during the polymerization. The electrochemically syn-
thesized PANI-TX-100 thin film enhances the electrical
conductivity of PANI film and make suitable for sensing
5. Acknowledgements
Raju Khan is thankful to the Department of Science and
Technology (DST), Government of India for financial
support received under the awarded Fast Track Young
scientist project No. SR/FTP/CS-77/2007.
Copyright © 2011 SciRes. ACES
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