Sensors and Actuators B 160 (2011) 1020–1025

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Sensors and Actuators B: Chemical

journal homepage: www.elsevier.com/locate/snb

Polyaniline–chitosan nanocomposite: High performance hydrogen sensor from

new principle
Wei Li, Dong Mi Jang, Sea Yong An, Dojin Kim ∗ , Soon-Ku Hong, Hyojin Kim
Department of Materials Science and Engineering, Chungnam National University, Daejeon, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history: A high selectivity and response towards hydrogen gas is realized with a composite of polyaniline
Received 2 March 2011 nanofibers embedded in chitosan matrix. The enhanced response originated from the new sensing mech-
Received in revised form 22 August 2011 anism related with the composite nature of chitosan and polyaniline. Based on the high gas sensing
Accepted 6 September 2011
performance through nanostructured resistive polyaniline nanofibers, the swelling of chitosan as the
Available online 12 September 2011
matrix distributing among the resistor network controls the hopping conduction between the nanofibers.
This gate control of chitosan on the polyaniline conduction claims a new type of sensor mechanism result-
Keywords:
ing in a reverse polarity in conductivity change with respect to the conductivity change of polyaniline.
Polyaniline
Nanofiber
The response-reversal can enhance the sensing response. Furthermore, the highly enhanced selectivity
Chitosan for hydrogen was also achieved through filtration action of chitosan for large size and polar molecules.
Sensor We thus demonstrate a new material and structural design of solid state sensor for improvement in
Hydrogen selectivity and response.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction intrachain gaps. Nevertheless, CP sensors can be categorized under

Based on semiconducting oxides, solid state gas sensors have
been widely studied because of their small size, low cost, and
compatibility with microelectronic processing, among others. The
simplest and most important sensor type is based on the change
of resistance due to the interaction of adsorbing gas molecules
with defects in oxide material. The accompanying charge exchange
between gas molecules and oxides causes a conductance change in
the material, to be recorded as sensing signal. Reaction for sens-
ing and transducing of signals in the sensor structure occurs in the
same material, as schematically drawn in Fig. 1(a). The device usu-
ally requires high operation temperatures (above ∼200 ◦ C) for fast
and reversible redox reactions on the material surfaces [1,2].
On the other hand, conducting polymers (CPs) such as polyani-
line (PANI) have attracted considerable attention as a resistive type
sensor, particularly due to the advantage of room temperature
operation. Conductivity change in CPs can occur through various
response mechanisms, such as changes in PANI conductivity by NH3
adsorption via deprotonation, chloroform adsorption via swelling,
and methanol adsorption via uncoiling [3,4]. Response mechanisms
originate from the polymer structure of long molecular chains with
abundant functional groups and relatively spacious interchain and
Fig. 1(a).
A new resistive type sensor structure of PANI nanofibers embed-
ded in chitosan (CHIT) is proposed, as schematically drawn in
Fig. 1(b), where the semiconducting PANI nanofibers network
provides the default transducing path. However, current flow is
controlled by a gating action of surrounding CHIT that interacts
with analyte gas. Specifically, hydrogen molecules react with envi-
ronmental oxygen to form water molecules, which in turn causes
CHIT to swell, hence interrupting the conducting path between
PANI nanofibers and raising resistance of the PANI nanofiber net-
work, as schematically shown in Fig. 1(c). This type of indirect
conduction control in sensors is preferred because of the resulting
higher response signal and significantly improved gas selectivity.
Poor gas selectivity or cross sensitivity of materials has long
been the limitation of resistive type sensor materials [3–7]. A soft-
ware dubbed “electronic nose” has been proposed to solve the poor
selectivity issue of sensor materials in general [8,9]. Meanwhile,
the concept of filter was proposed to improve device selectivity
[1]. The CHIT layer in the composite structure is shown to reveal an
excellent filtering action for gases other than hydrogen.
2. Experiment

2.1. Preparation of PANI nanofibers

∗ Corresponding author. Tel.: +82 42 821 6639, fax: +82 42 823 7648. Aniline and ammonium persulfate were used, as received from
E-mail address: dojin@cnu.ac.kr (D. Kim). Sigma–Aldrich Co. PANI nanofibers were prepared using rapid

0925-4005/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2011.09.020
 W. Li et al. / Sensors and Actuators B 160 (2011) 1020–1025
Fig. 1. (a) The conventional resistive type sensor like PANI which adsorb hydrogen
to lower its resistance. (b) The newly proposed resistive type sensor made of series
connection of conducting PANI and insulating CHIT. (c) Hydrogen can react with both
PANI and CHIT, however in this case, the swelling of CHIT layer plays the major role to
increase the resistance of the PANI conducting channel. The right-hand side of each
panel shows the corresponding equivalent circuit. The standby resistance of PANI
(RoPANI ) changes to RgPANI with gas adsorption. For the CHIT/PANI composite structure,
the resistance changes from RoPANI + RoCHIT to RgPANI + RgCHIT with gas adsorption.
mixed reaction [10]. An ammonium persulfate acidic solution
(50 ml, 1 M HCl) was quickly poured into aniline acidic solution
(50 ml, 1 M HCl) at room temperature, followed immediately by
magnetic stirring for 2 h. The solution was then left undisturbed for
12 h. Green precipitates were filtrated with filter paper and washed
with a large amount of deionized water. According to previous stud-
ies [11], these PANI nanofibers are in highly doped emeraldine salt
forms.
Fig. 3. SEM images of PANI/CHIT composites made of different CHIT solution: (a) zero wt.%, (b) 0.07 wt.%, (c) 0.33 wt.%, and (d) 1.67 wt.%. Inset of (a) shows the high
magnification of PANI nanofibers.
1021
Fig. 2. Schematic diagram of PANI/CHIT composite structure.
2.2. Preparation of PANI/CHIT composite film
A solution of 0.07 ∼ 1.67 wt.% CHIT (75 ∼ 85% deacetylated, low
molecular weight, produced by Aldrich, 30 ml) is prepared by dis-
solving 0.02–0.5 g CHIT in acetic acid solution (5%) with magnetic
stirring. A PANI nanofiber (0.05 g) was added into this solution and
dispersed by sonication, after which the green dispersion was spin
coated (∼800 rpm) on the glass substrate using a pipette to apply
a desired amount of solution onto the substrates. Film thickness
was ∼5 ␮m according to the cross section point of SEM view. The
PANI and CHIT may form a strong hydrogen bonding through the
abundant polar group (–OH, –NH2 , etc.) in PANI and CHIT (Fig. 2)
[12].
1022 W. Li et al. / Sensors and Actuators B 160 (2011) 1020–1025

2.3. Material characterization

Surface morphology of the synthesized PANI nanofibers

and PANI/CHIT composite was examined via scanning elec-
tron microscopy (SEM, JEOL-7000) at an accelerating voltage of
15 kV.

2.4. Sensor measurement

Gas-sensing properties were measured in a stainless steel cham-

ber equipped with a temperature-controlled chuck, as performed
in previous experiments [13]. Pt electrodes were patterned on
the glass substrate via sputter deposition of platinum through
an interdigitated metal shadow mask. The comb-type electrodes
consisted of four pairs of fingers. Each finger had a length of
4000 ␮m and width of 200 ␮m. The gap between each finger was
100 ␮m.
Dry air was used as both carrier and dilution gas. H2 , NH3 , and
NO gases were diluted with dry air via a controlled flow through
a mass flow controller. Because the volatile organic compounds
(VOC) are in liquid form at room temperature, a bubbler evapo-
ration system was used to deliver fixed concentration of volatile
analytes into the detection chamber. All measurements were per-
formed at room temperature. Current measurements on the sensor
were obtained using a source meter (Keithley Model 2400) at a fixed
voltage as a function of time. Resistance change is expressed by the
following:
R Rg − Ro
(%) = 100 × (1)
Ro Ro
where Ro is the resistance in dry air, and Rg is the resistance upon
exposure to gas molecules.

3. Results and discussion

SEM image of a pure PANI nanofiber sensor is shown in Fig. 3(a),
which reveals nanofibers with a diameter range of 40–70 nm and
hundreds of nanometers in length, forming a network. PANI/CHIT
composites, or PANI nanofibers coated by various thicknessess of
CHIT layers, are shown in Fig. 3(b–d). Sensing property measure-
ments were mainly conducted with the structure of Fig. 3(d) unless
specified. The PANI is not exposed to out from CHIT matrix indi-
cating that PANI is fully soaked in CHIT. Therefore, PANI fibers are
distributed in the CHIT matrix as schematically depicted in Fig. 1(b).
The other composite structures of Fig. 3(b) and (c) with thinner CHIT
layers coating were tested only for comparison.
Resistance of the PANI thin film [Fig. 3(a)] was approximately
∼103 . Film resistance was observed to increase in the composites
due to intervention of insulating CHIT between the PANI nanofibers
at their contacts. Resistance rise was drastic, up to ∼105 , with
the highest content of CHIT [Fig. 3(d)]. Resistance of composite
structure may be simplified to a series connection of a PANI and
comp
CHIT resistor, Ro = RoPANI + RoCHIT , although the PANI network is
three-dimensional (Fig. 1). Resistance is directly proportional to
CHIT concentration due to an increase in RoCHIT , as seen in a thick
CHIT coating.
Fig. 4 compares (a) the CHIT/PANI composite and (b) pure PANI
structures in response to 4% H2 gas diluted in air at room temper-
ature. The difference between the two are as follows: (i) resistance
increased with the composite while it decreased with the PANI
upon exposure; (ii) response with the composite film was higher
(at ∼130%) than with the PANI at ∼28%; (iii) recovery did not
completely occur with the composite; (iv) absolute resistance
increased with repetition of exposure-and-recovery cycles; and
(v) recovery level increased with repetition of the exposure-and-
recovery cycles, and so on.
Fig. 4. The response of (a) PANI/CHIT(1.67 wt.%) composite and (b) pure PANI
nanofiber to 4% H2 in dry air at room temperature.
A sign reversal of the response between composite
and PANI structures can be expressed by the following:
comp comp
Rcomp = Rg − Ro > 0 while RPANI = RgPANI − RoPANI < 0.
This indicates that R CHIT = RgCHIT − RoCHIT > −RPANI > 0 since
R comp = R PANI + R CHIT . In short, upon exposure to H2 , resis-
tance increase due to CHIT is far greater than resistance decrease
in PANI.
To determine how exposure of CHIT to H2 in the compos-
ite results in resistance increases, we need to reinvestigate the
interaction between H2 and PANI, as well as between H2 and
CHIT. Emeraldine salt, a form of polyaniline, is a p-type conduc-
tor that exhibits conductivity enhancement via interaction with
hydrogen molecules. In addition, this is the origin of the negative
RPANI . However, the explanation is not universally true; basically,
two interpretations have been proposed in literature. MacDiarmid
[14,15] proposed that hydrogen molecules adsorb on the polymer
and dissociate into H atoms to bind on the backbone of the poly-
mer chain and supply charge carriers. Conn et al. [16], for their part,
proposed that hydrogen molecules convert to water molecules via
catalytic oxidation, and their adsorption on the polymer increases
its conductivity. Therefore, adsorbing species on PANI for conduc-
tion change is not definite between atomic hydrogen and water
molecule, and it is important to figure out the species for the fol-
lowing discussion on the interaction between H2 gas and CHIT.
To investigate the interaction of hydrogen with PANI, a structure
[Fig. 3(a)] was mounted in a test chamber with ambient air until sta-
bilization of the resistance is obtained. The examination focused on
responses to H2 and water molecules. First, response to N2 , dry
 W. Li et al. / Sensors and Actuators B 160 (2011) 1020–1025 1023

Fig. 5. (a) The response of PANI in various environments (a: N2 ; b: vacuum; c: N2 ; d: vacuum; e: dry air; f: vacuum; g: wet air; h: vacuum; i: N2 ; j: wet air; and k: dry air);
(b) the intrinsic response of PANI to 4% H2 diluted in N2 and dry air; (c) the response of PANI/CHIT (1.67 wt%) composite to 4% H2 diluted in dry air and wet air; and (d) the
response of PANI/CHIT composite of different CHIT contents to 4% H2 . All the experiments are carried out at room temperature.

air, vacuum, and wet air were examined, as shown in Fig. 5(a).
Note that responses are all extremely slow processes. Exposure to
water vapor exhibited enhanced conductivity in PANI (Regime g).
Adsorbed water molecules were desorbed out of PANI by flushing
gases such as nitrogen or air (Regime i and k), but not by evacuation
(Regime h). Resistance increase with flowing of N2 or air (Regime
a, c, and e) can then be understood as a similar process. The same
goes with gases that flush preadsorbed moisture out of the PANI, if
nitrogen does not interact with PANI [16,17]. Response in regime
a revealed a long and slow upward drift as similarly reported by
Conn et al. [16], who explained the behavior as a continuous des-
orption of moisture out of PANI. Therefore, recovery with pumping
(Regime b, d, and f) occurred by re-adsorption of water molecules
from the environment such as the chamber wall.
Examinations that follow include the sensing of PANI to H2 in
various recovery environments of vacuum, N2 , and air. Comparison
of results between N2 and air environments is depicted in Fig. 5(b).
While response was small in N2 (and vacuum), it was relatively
large in ambient air. If hydrogen molecules directly adsorb and dis-
sociate in PANI as per the MacDiarmid model, the response should
not depend on ambient gas. This comparison suggests a role of oxy-
gen in conductivity change of PANI along with H2 introduction,
which supports Conn’s model. According to Barsukov et al. [18,19],
oxygen molecules can chemisorb in PANI and participate in reduc-
tion reaction to form water molecules. Therefore, one conclusion is
that reaction between H2 and O2 to form H2 O molecules may occur
catalytically with PANI at room temperature.
Behavior of H2 in the CHIT/PANI composite structures is then
examined, where diffusion of hydrogen (and oxygen) molecules
through CHIT is required to interact catalytically with PANI.
Response of the CHIT/PANI composite to H2 (as well as to H2 O
for comparison purposes) is shown in Fig. 5(c). The following
are observed: (i) response polarity reversal with composite was
observed not only for H2 , but for H2 O molecules as well, and (ii)
response-and-recovery kinetics was considerably slower with H2 O
than with H2 . While response polarity reversal for both H2 and
H2 O in the composite again strongly supports that the origin of
H2 sensing is same as that of H2 O sensing, polarity changes defi-
nitely attribute to CHIT, which is known to swell by absorbing water
molecules [12,20]. Spin-coating of a mixture of PANI nanofibers in
viscous CHIT solution produces a structure [Fig. 1(b)], and stack-
ing of CHIT-covered PANI nanofibers results in a thin CHIT layer
jammed at PANI fiber-to-fiber contacts. When the jammed CHIT
swells and separates fiber-to-fiber contacts [Fig. 1(c)], transport of
carriers from fiber-to-fiber is interrupted to yield a positive RCHIT .
Although adsorption of H2 O into PANI reduces PANI resistance (or
negative RPANI ), the considerably larger positive RCHIT increases
overall resistance of the composite, Rcomp . The thicker jammed
CHIT layer will produce greater swelling, and in turn, larger sep-
aration of fiber-to-fiber gap to produce larger RCHIT . Comparison
between composites with different thicknessess of jammed CHIT
layers [Fig. 3(b)–(d)] is depicted in Fig. 5(d). As expected, relative
contribution of RCHIT over RPANI is larger with a thicker CHIT
sample.
The second observation that regards the difference in the
response-and-recovery kinetics between H2 and H2 O [Fig. 5(c)]
may be discussed as follows. The relatively much slower response
for H2 O may be explained by the polar nature of water molecules,
whose diffusion can be immensely obstructed by strong hydrogen
bonding with significant amounts of amine and hydroxyl groups
1024 W. Li et al. / Sensors and Actuators B 160 (2011) 1020–1025
Fig. 6. The concentration dependence of response of the PANI/CHIT (1.67 wt.%) com-
posite sensor.
of CHIT. On the contrary, the considerably smaller kinetic diameter
of H2 and O2 molecules in comparison with the inter- and intra-
chain distance of CHIT [21,22], along with their nonpolar nature,
may allow faster diffusion in CHIT at the response stage.
However, if the real species operating at the PANI–CHIT interface
is H2 O for both H2 and H2 O analytes, different recovery behaviors
between H2 and H2 O in Fig. 5(c) cannot be distinguished. One may
expect similarly slow recoveries in the hydrophilic CHIT for both
cases because recovery kinetics is related with diffusion out of the
same water molecules. In the recovery cycle for H2 , one observes
two clearly distinguished kinetic regions: initial fast recovery (sev-
eral minutes), followed by an extremely slow recovery (more than
hundreds of minutes). The latter process was manifested by an
offset in the recovery resistance level, which accumulated in the
following repeated cycles [Fig. 4(a)]; this suggested that either two
different molecular species or two different binding energies of a
species are involved in the recovery stage. The first case can be pos-
sible if, in addition to binding with the catalytically produced H2 O,
H2 directly interacts as well with amino/hydroxyl functional groups
at the interface. For the latter case, one may imagine the different
binding energy of H2 O at the PANI–CHIT interface from that in the
CHIT bulk since PANI–CHIT interface offers more variable functional
groups for the binding of H2 O compared to pure CHIT. In any case,
the Raman and FTIR analyses did not reveal any remarkable indi-
cation that H2 or H2 O molecules are bound in the composite. Thus,
further detailed microscopic examination is necessary to figure out
the sensing mechanism.
The sensor response to the H2 gas concentration ranging from
0.3 to 4% was quite linear, as shown in Fig. 6. Another remark-
able feature of the composite structure exists in its high selectivity
towards hydrogen. Sensing properties of the composite to other
oxidizing, reducing, and organic vapor gases are summarized in
Fig. 7. NO gas is known to oxidize the emeraldine salt PANI to
increase its resistance [7], and the PANI nanofiber sensor showed
approximately 25% response to 40 ppm NO while the composite
sensor showed practically no response. Therefore, null response
with the composite indicates that NO gas could neither reach the
PANI nanofibers nor contribute to volume change of CHIT. Evi-
dently, NO gas could not penetrate the CHIT layer, possibly due to
its capture by the functional groups of CHIT through H-abstraction
reaction [23,24]. The composite did not show any response to a
reducing gas, or 60 ppm NH3 , again indicating total blockage of NH3
by CHIT. High polarity of molecules can induce strong dipole–dipole
interactions with the functional groups.
The filtering action of CHIT was observed as well with cer-
tain important volatile organic compounds of chloroform (CHCl3 ),
Fig. 7. The response of PANI and PANI/CHIT (1.67 wt.%) composite to NH3 , NO, CCl3 ,
CH3 OH, C6 H6 , CH3 COCH3 , CH3 COOH, C6 H14 , and H2 at room temperature. All the
gases and vapors are diluted in dry air.
methanol (CH3 OH), benzene (C6 H6 ), acetone (CH3 COCH3 ), acetic
acid (CH3 COOH), and hexane (C6 H14 ). A number of neutral volatile
organic compounds are known to change conductivity of PANI via
the swelling effect [3,25], but CHIT almost blocked the six com-
mon organic vapors used in laboratory or industry. High selectivity
of the composite structure relies on CHIT, which filters out large
and polar molecules while admitting small and nonpolar ones [20].
Upon filtration, hydroxyl and amino functional groups of CHIT
catch polar gas molecules through strong dipole–dipole interaction
and/or hydrogen bonding.
4. Conclusions
In conclusion, nanocomposite structures of the PANI nanofibers
network, coated with controlled thicknesses of CHIT, are fabricated.
The composite structure sensor showed higher response towards
hydrogen gas than the pure PANI nanofiber sensor, but with rever-
sal in response polarity. The result was explained by modeling the
composite structure as a network of conducting PANI nanofibers,
which are coated with insulating CHIT film. When exposed to H2
diluted in air, H2 catalytically react with O2 to form H2 O on PANI,
whose adsorption enhances PANI conductivity. However, H2 O like-
wise causes swelling of CHIT at contact and physically separates the
distance between conducting PANI nanofibers, hence interrupting
current flow between PANIs. The latter effect overrides the former
so that the overall conductivity in the composite decreases. In other
words, CHIT exhibits a gating action on current flow from PANI to
PANI, similar to the depletion-mode junction field-effect transis-
tor; this unique conduction control mechanism in the PANI–CHIT
composite induced the apparent conductivity-type reversal.
Another observed important function of CHIT is the physico-
chemical filter: finite inter- and intra-chain space and numerous
functional groups of CHIT can block large size and/or polar
molecules. The most dramatic effect is observed with selective
sensing of the smallest and nonpolar molecule of H2 . Therefore,
a new operating principle is discovered for hydrogen sensors with
high sensitivity and high selectivity, given that they operate at room
temperature.
Acknowledgements
This study was supported by the National Research Laboratory
and R32-20026 programs of the Ministry of Education, Science, and
 W. Li et al. / Sensors and Actuators B 160 (2011) 1020–1025
Technology, Korea. We also acknowledge the financial support from
the Grant No. 2010-0004327 and 205-2005-1-D00078.
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Biographies
Wei Li received the degree of Master of Science in Materials Science at Shenyang Uni-
versity of Chemical Technology, China in 2005. He is now in Ph.D. course in Materials
Science and Engineering, Chungnam Nat. Univ., Korea. His current research inter-
ests are fabrication of nanostructure conducting polymers and their applications to
electronic devices, gas sensors, etc.
Dong Mi Jang received her BS in Materials Science and Engineering at Chungnam
National University, Korea, in 2009. She is now in Master course in Materials Sci-
ence and Engineering, Chungnam National University, Korea. Her current interest is
synthesis of metal oxide nanostructures.
Sea Yong An received his BS in Materials Science and Engineering at Chungnam
National University, Korea, in 2009. He is now in Master course in Materials Sci-
ence and Engineering, Chungnam National University, Korea. His current interest is
synthesis of metal oxide nanostructures.
Dojin Kim received his Ph.D. in Materials Science and Engineering from the Uni-
versity of Southern California, USA, in 1989. He is a professor at the School of
Nanotechnology and the Department of Materials Science and Engineering in
Chungnam National University, Korea. His current research interests are synthesis
of carbon nanotube and metal oxides and applications to electronic devices of field
emitters, solar cells, gas sensors, and so on. He is also interested in semiconductor
nanostructures growth and applications.
Soon-Ku Hong received his Ph.D. in Applied Physics from Tohoku University, Japan,
in 2001. He is an associate professor at the School of Nanotechnology and the Depart-
ment of Materials Science and Engineering in Chungnam National University, Korea.
His current research interests are growth and applications of oxide and nitride
semiconductors for light emitting diodes, sensors, and solar cells. Major fabrication
techniques for his researches are molecular-beam epitaxy, chemical vapor deposi-
tion, hydrothermal growth, and sol–gel. He is also interested in defect and interface
engineering in hetero-epitaxial films and characterization of structural defects by
transmission electron microscopy.
Hyojin Kim received his Ph.D. in Materials Science and Engineering from Korea
Advanced Institute of Science and Technology, Korea, in 1993. He is a professor at the
Department of Materials Science and Engineering in Chungnam National University,
Korea. He is currently interested in synthesis and applications of ZnO-based oxide
materials, including ZnO-based gas sensors and diluted magnetic semiconductors.