Sensors and Actuators B 147 (2010) 488–494

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Sensors and Actuators B: Chemical

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

Room temperature liquefied petroleum gas (LPG) sensor

D.S. Dhawale, D.P. Dubal, A.M. More, T.P. Gujar, C.D. Lokhande ∗
Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (M.S.), India

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

Article history: The p-polyaniline/n-ZnO thin film heterojunction sensor for room temperature LPG detection was fabri-
Received 12 November 2009 cated by electrodepositing polyaniline on chemical bath deposited ZnO film. The heterojunction showed
Received in revised form 21 February 2010 rectifying behavior indicating the formation of a diode with ideality factor 1.10. The formation of diffusion
Accepted 26 February 2010
free interface of heterojunction was confirmed from cross-sectional FESEM. The heterojunction sensor
Available online 10 March 2010
has quick and high response towards LPG as compared to N2 and CO2 and exhibited maximum response
of 81% upon exposure of 1040 ppm of LPG. The LPG sensing mechanism for heterojunction is modeled
Keywords:
through change in height of barrier potential.
Heterojunction
Thin films © 2010 Elsevier B.V. All rights reserved.
LPG sensor
Selectivity
LPG sensor model
Stability

1. Introduction intrinsically safe performance in potentially hazardous situations.

LPG is a flammable gas which presents many hazards to both the
humans and an environment. Due to its highly flammable char-
acteristics, even low level concentration (ppm) poses a serious
threat. With the global population boom, more and more human
lives are being endangered by the effect of LPG exposure. LPG is
used as an automotive fuel or as a propellant for aerosols, in addi-
tion to other specialist applications. The widespread use of LPG for
cooking and as fuel for automobile vehicles requires fast and selec-
tive detection of LPG to precisely measure the leakage of gas for
preventing the occurrence of accidental explosions. In spite of con-
siderable efforts, good sensor for LPG has not been found hitherto,
the problem being of vital significance to industry as well as general
public. To meet this demand, considerable research for new sen-
sors is underway, including efforts to enhance the performance of
traditional devices, such as resistive metal oxide sensors, through
nano-engineering. Metal oxide LPG sensors allows for the detec-
tion of lower level LPG presence, but suffer from low selectivity
to specific target gases and high operation temperature and lower
sensitivity [1–3]. Thus increase power consumption, reduce sensor
life, limit the portability, etc. Though metal oxides have been exten-
sively used for gas sensor, a new approach is needed to increase this
selectivity and sensitivity at room temperature (300 K). The room
temperature operation is also an important criterion to achieve
∗ Corresponding author. Tel.: +91 231 2609229; fax: +91 231 2692333.
E-mail addresses: l chandrakant@yahoo.com, dattatraydhawale@gmail.com
(C.D. Lokhande).
It has been pointed out that such sensors exhibit a fast, reversible
response at room temperature [4–6]. In recent years, heterojunc-
tion between p- and n-type semiconductors have been developed
for detecting various gases [7–10]. The heterojunction type sen-
sors work on the principle of barrier mechanism [11,12], which
needs no adsorption and desorption of oxygen for the detection of
gas. The ZnO found potential applications in optoelectronic devices
[13,14], gas sensor [15], dye sensitized solar cells (DSSC) [16], etc.
However, these are effective at only temperatures above 473 K,
resulting in high power consumption and complexities in inte-
gration. To meet the requirements for analyzing LPG and other
poisoning species, to improve the stability and selectivity and to
lower fabrication costs, conducting polymers in the form of thin
films, blends, or heterojunctions have been developed and have
shown great potential to enhance its sensitive characteristics. A
considerable interest in the fabrication of ZnO/organic hybrid struc-
ture has also been developed for solar cell, photodiode, photovoltaic
and photoelectrochemical applications [17–20]. Polyaniline (PANI)
is potential p-type semiconducting material for use in junction
devices [21,22]. It exhibits high electrical conductivity on doping
and can be used in rechargeable batteries, electrochromic displays,
electronic switches, gas sensors and photovoltaic devices. There
are reports on the luminescence from nanosized ZnO/polyaniline
structures [23] and UV photodetection by ZnO/PANI films [24,25].
Salomsom fabricated HCl doped p-polyaniline/n-ZnO junction by
chemical bath deposition method which sensitive to UV photons
[24]. The ZnO together with PANI, an inorganic/organic hybrid
structure shows a promising application in the UV photodetection.
The fabrication of p-polyaniline/n-ZnO heterojunction based diode

0925-4005/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2010.02.063
 D.S. Dhawale et al. / Sensors and Actuators B 147 (2010) 488–494 489

Fig. 1. (a) Schematic and (b) actual experimental set up for the deposition of ZnO thin films.

structure and its application for room temperature gas sensor is not
reported.
Thus, the goal for this research is to produce a reliable, highly
selective and sensitive LPG room temperature sensor, for a hand
held application. Therefore, in this work, we have fabricated p-
polyaniline/n-ZnO heterojunction using an (electro) chemical route
and studied its room temperature LPG sensor mechanism.
2. Experimental details
2.1. Deposition of ZnO thin film
by CBD method from alkaline bath of zinc salt containing the sub-
strates immersed in it. All chemicals used were A.R. grade (supplied
by S.D. Fine Chem. Ltd., Mumbai). An aqueous solution of 0.1 M
Zn(NO3 )2 was prepared and in this solution aqueous NH3 solution
(25%) was added under constant stirring. A white precipitate was
initially observed, which subsequently dissolved back into solution
upon the further addition of the NH3 solution. Pre-cleaned stainless
steel substrates were immersed and placed vertically in the solu-
tion. The solution was maintained at a pH of 9 and a temperature of
333 K for 2 h, resulting in the direct growth of ZnO nanorods on the
substrate. The substrate was then removed from the bath, washed
with deionized water, dried and annealed in air at 673 K for 4 h.

The schematic of an experimental set up employed for the depo-

sition of ZnO thin films using chemical bath deposition (CBD) is
shown in Fig. 1(a). It consists of container, usually a glass beaker
fixed in a water bath. The water bath is kept on the magnetic stirrer-
heater set up in order to maintain the desired temperature. The
substrates were fitted in the bakelite holder having the slots for
substrate and the holder is fixed in beaker containing the precursor
solution. The actual setup of CBD method used for the deposition of
ZnO films is shown in Fig. 1(b). ZnO thin films have been deposited
2.2. Fabrication of p-polyaniline/n-ZnO heterojunction
Fig. 2(a) shows the experimental setup for the deposition of
polyaniline on to ZnO thin films. It consists of conventional three-
electrode system, i.e. working electrode (ZnO), counter electrode
(cathode) and reference electrode. These three electrodes are fit-
ted in the bakelite holder having the slots for each electrode and
the holder is fixed in cylindrical cell containing electrolyte. The

Fig. 2. (a) Schematic and (b) actual electrodeposition set up for the deposition of polyaniline thin films.
490 D.S. Dhawale et al. / Sensors and Actuators B 147 (2010) 488–494

cylindrical cell used is made up of glass, which serves two pur-

poses of chemically inertness and visibility inside the bath. All the
depositions were carried out using a scanning Potentiostat EG &G
Princeton Applied Research Model 263A. The actual setup and elec-
trochemical cell used for deposition of polyaniline films is shown
in Fig. 2(b). For the fabrication of p-polyaniline/n-ZnO heterojunc-
tion, polyaniline film was deposited onto a previously deposited
ZnO film using galvanostatic electrodeposition method [26] with
a constant current 4 mA/cm2 . For this a solution containing 0.5 M
H2 SO4 + 0.45 M aniline (C6 H5 NH2 ) was used.

2.3. Characterization techniques

The thicknesses of the ZnO and Polyaniline films were calculated

using fully computerized AMBIOS Make XP-1 surface profiler with
1 Å vertical resolution. For that sharp step is performed by applying
cello tape prior to deposition. After the junction fabrication for each
thickness of ZnO as well as polyaniline, the current density–voltage
(J–V) characteristics were recorded. From the J–V characteristics,
the junction with low ideality factor having high rectification
ratio were calculated and optimized the film thickness. The opti-
mized thicknesses of ZnO and polyaniline films were 0.5092 and
0.9012 ␮m, respectively. The J–V characteristics of the junction
were examined by making front aluminium foil press contact and
back stainless steel contact to a heterojunction sample having area
1 cm × 1 cm. The schematic diagram of the p-polyaniline/n-ZnO
heterojunction is depicted in inset (a) of Fig. 3. Onto stainless steel
substrate ZnO and polyaniline films were subsequently deposited
using CBD and electrodeposition methods, respectively. The surface
morphological study of the ZnO, polyaniline and cross-sectional
interface of a p-polyaniline/n-ZnO heterojunction was studied with
field-emission scanning electron microscopy (FESEM, Model: JSM-
6160).
2.4. LPG sensing properties p-polyaniline/n-ZnO heterojunction
2.4.1. Experimental setup for gas sensor study
In order to test the gas sensing ability of heterojunction, the gas
sensor unit was specially designed. The gas sensor unit consists
of small dome shaped glass vacuum chamber. The special mount-
ing for sample with precise contacts was permanently installed
inside the vacuum chamber. Fig. 4(a) shows the schematic of
the gas sensor unit. Through the external connections, junction
current–voltage (I–V) characteristic were recorded using Potentio-
stat (EG&G Princeton Applied Research Model 262-A). The forward
biased I–V characteristics of the junction before and after exposure
Fig. 3. The current density (J)–voltage (V) plot of p-polyaniline/n-ZnO heterojunc-
tion. Inset: schematic representation of p-polyaniline/n-ZnO heterojunction.
of gases were recorded for different concentrations. From I–V char-
acteristics, a fixed potential at which the maximum current change
occurred, was noted. The electrical currents of heterojunction in
air (Ia ) and in the presence of gas (Ig ) were measured and using
following relation the gas response was calculated.
Ia − Ig I
S(%) = × 100 = × 100 (1)
Ia Ia
The response and recovery time periods of the junction towards
gas were determined at fixed forward biased potential (+1.8 V).
2.4.2. Gas volume measurement
In the present work, we have developed a simple gas volume
measurement unit as shown in Fig. 4(b). It consists of glass bottle
containing double distilled water which is saturated with gas to be
measured, in order to avoid the possibility of dissolution of inserted
gas. Above this bottle, the measuring tube (pipette) is connected by
vacuum seal. The cock I is connected to gas cylinder and cock II is
connected to inlet of gas chamber. When the cock I is opened, the
gas from the cylinder is filled in the glass bottle and the equivalent
amount of water is displaced in the measurement pipette. When the
cock II is opened, the desired amount of gas volume is injected in the
gas chamber which is prefilled with air. Fig. 5(a) and (b) shows the
photograph of actual set up of gas sensor assembly and gas volume
measurement unit.

Fig. 4. Schematic diagram of the (a) gas sensor unit and (b) the gas volume measurement unit.
 D.S. Dhawale et al. / Sensors and Actuators B 147 (2010) 488–494 491

Fig. 5. (a) Actual set up of gas sensor unit [inset: photograph of sample mounting and contacts] and (b) gas volume measurement unit.

3. Results and discussion
3.1. Surface morphological studies
The typical J–V characteristic of p-polyaniline/n-ZnO hetero-
junction for optimized film thicknesses is shown in Fig. 3. The
J–V characteristic shows rectifying behavior having rectification
ratio 8.8 × 103 with ideality factor 1.10 indicating the forma-
tion of good quality diode. Fig. 6(a) and (b) shows the typical
FESEM images of ZnO and polyaniline films at ×100K magnifi-
cations, respectively. It is clearly seen that ZnO films consist of
nanorods which are well-defined and grown almost perpendicular

Fig. 6. The FESEM images of (a) annealed ZnO at 673 K, (b) polyaniline and (c) cross-sectional FESEM of p-polyaniline/n-ZnO heterojunction.
492 D.S. Dhawale et al. / Sensors and Actuators B 147 (2010) 488–494

exposed to LPG, contrast to hydrogen gas sensors based on Pd/TiO2

Fig. 7. Forward biased I–V characteristics of p-polyaniline/n-ZnO heterojunction in
the voltage range of 0 to +1.8 V and at a concentration of 520 ppm for various gases
(a) without, (b) N2 , (c) CO2 , and (d) LPG. (Inset: selectivity bar diagram for different
gases at 520 ppm gas concentration.)
and parallel to the substrate. The FESEM image of the polyaniline
film (Fig. 6(b)) exhibits a fibrous structure with many pores and
gaps among the fibers. Fig. 6(c) shows the cross-sectional FESEM
image of p-polyaniline/n-ZnO heterojunction interface. The inter-
face cross-sectional FESEM image shows the formation of diffusion
free junction. The FESEM also revealed that the polyaniline is highly
porous with interconnectivity of fibers and grains and the rough
layer of ZnO. Due to the rough layer, a non-uniform interface is
formed.
3.2. Gas sensing studies
3.2.1. Selectivity studies
Fig. 7 shows the forward biased I–V characteristics of p-
polyaniline/n-ZnO heterojunction for different gases at room
temperature in voltage range of 0 to +1.8 V. Fig. 7(a) is the I–V char-
acteristic before exposure to the gas and those from (b), (c) and
(d) are the plots when exposed N2 , CO2 and LPG at 520 ppm con-
centration. From the Fig. 7 it is seen that, the maximum change in
current is observed for LPG as compared to N2 and CO2 gases. Inset
of Fig. 7 shows the heterojunction gas response towards N2 (1.74%),
CO2 (15.46%) and LPG (28.48%). The heterojunction showed more
selectivity for LPG over N2 compared to CO2 (SLPG /SN2 = 16.36 and
SLPG /SCO2 = 1.86). It revealed that LPG is most selective against N2
and poor selective against CO2 .
[27]. The change in current may be due to the chemical reaction
between interface of heterojunction and adsorbed gas molecules.
Tucci et al. [28] have reported that the change in the conductivity
is due to the interaction of adsorbed gas molecules onto inter-
face of heterojunction. The LPG response of the heterojunction
at an applied potential +1.8 V is depicted as inset of Fig. 8. The
sensitivity increased from 15.46% to 81% with increase in concen-
tration of LPG from 260 to 1040 ppm. The maximum LPG sensitivity
of 81% was recorded under the exposure of 1040 ppm, i.e. 4% of
lower explosive level (LEL) of LPG. At 1300 ppm LPG, sensitivity
was decreased to 69.76%. At lower gas concentrations (<1040 ppm
LPG), the unimolecular layer of gas molecules would be expected
to form on the interface, which would interact with the interface
more actively giving larger response. There would be multilayers of
LPG molecules on the interface of junction at the higher gas concen-
trations (>1040 ppm LPG) resulting into decrease in the sensitivity.
3.2.3. LPG sensing model
The most commonly accepted model for the operation of het-
erojunction gas sensors is the potential barrier dependent. Fig. 9(a)
and (b) shows the schematic representation of the model for
p-polyaniline/n-ZnO heterojunction for LPG detection at room
temperature (300 K) with corresponding its physical model in
Fig. 9(a’) and (b’), respectively before and after the exposure of
LPG. Heterojunction diode is a rather simple device and can be
employed to detect gas analytes. Instead of using the mechanism of
adsorption–desorption of oxygen for the detection of LPG, the prin-
ciple of formation of heterojunction barrier in air ambient and their
disruption on exposure to LPG is employed. The effective barrier
height, ‘B ’ can be modulated by analyte, through changing dop-
ing level of conducting polymer. The molecules of reducing gases
(LPG), changes the potential barrier height and consequently the
current across the junction. From Fig. 9(b’), it is seen that, when LPG
molecules entered through the polyaniline, reach at the interface
of p-polyaniline/n-ZnO heterojunction, increases the barrier height
of heterojunction (Fig. 9(b’)). This leads to the interaction of LPG
molecules at the interface of p-polyaniline/n-ZnO heterojunction
(Fig. 9(b’)) resulting the decreases in the carrier concentration near
the interface of heterojunction. This decrease in carrier concen-
tration increases the potential barrier of heterojunction interface
(Fig. 9(b’)).

3.2.2. LPG sensing studies

Fig. 8 represents the typical forward biased I–V characteristic
plots of p-polyaniline/n-ZnO heterojunction in the absence and
presence of different concentrations of LPG at room temperature.
Fig. 8(a) shows the I–V characteristics without LPG and those from
(b) to (f) are with LPG for the concentration ranging from 260 to
1300 ppm. A shift is occurred in the I–V characteristics after expo-
sure of LPG. As the heterojunction is exposed to LPG, the forward
current drastically decreased with increase in concentration of LPG
up to 1040 ppm. The decrease in forward current with increased
concentration of LPG has been attributed to the decrease in charge
carrier concentration as LPG molecules reach at the interface of the
heterojunction through polyaniline.
Such decrease in current has been attributed due to the change
in work function of the polyaniline and resistance of the polyani-
line increase. Thus the carrier concentration of the heterojunction
Fig. 8. Forward biased I–V characteristics of p-polyaniline/n-ZnO heterojunction at
decreases and current across the junction decreases and con- various concentrations of LPG in (a) without, (b) 260 ppm, (c) 520 ppm, (d) 780 ppm
sequently barrier height of the heterojunction increases when (e) 1040 ppm, and (f) 1300 ppm. (Inset: the gas response (%) vs. LPG concentration.)
 D.S. Dhawale et al. / Sensors and Actuators B 147 (2010) 488–494
Fig. 9. The LPG sensing model of p-polyaniline/n-ZnO heterojunction before (a) and after (b) exposure of LPG and their corresponding physical models (a’) and (b’).
3.2.4. Dynamic response and stability studies
The dynamic variation of gas response with time at the fix
concentration of 1040 ppm LPG is shown in Fig. 10. For the mea-
surement of response and recovery time periods, we have taken
I–V characteristics in forward biased region for different LPG con-
centrations and we found as the LPG concentration increases from
260 to 1040 ppm, response time decreases from 200 to 100 s. Also,
the corresponding recovery time periods increase from 110 to 150 s.
The heterojunction attained the maximum sensitivity in short time
upon exposure of 1040 ppm LPG and dropped rapidly when the gas
was removed from testing atmosphere indicating that the sensor
has the good response (100 s) and recovery time (150 s).
For the stability studies of the p-polyaniline/n-ZnO heterojunc-
tion sensor element, the forward biased I–V characteristics were
performed at room temperature upon exposure of fixed concentra-
Fig. 10. The gas response (%) vs. time(s) plot of the p-polyaniline/n-ZnO heterojunc-
tion at voltage of +1.8 V and at a concentration of 1040 ppm LPG. (Inset: stability
studies.)
493
tion of 1040 ppm LPG for 30 days with 5 days interval after the first
measurement. The gas response with time is illustrated in inset of
Fig. 10. The LPG performance remained almost the same after initial
decrease (10%) from which it is concluded that p-polyaniline/n-
ZnO heterojunction can stand as a reliable sensor element for room
temperature LPG sensor application.
4. Conclusions
In summary, the present work has been addressed LPG sens-
ing performance of p-polyaniline/n-ZnO heterojunction, which
appeared as a promising material for such an application due to
its room temperature operation. The results highlighted that this
material can be applied in gas sensing field to develop LPG sensors
with performances suitable for practical application. The present
heterojunction is stable, robust, compact, easy to fabricate and
diffusion free and compatible with integrated circuit fabrication
technology.
Acknowledgement
Authors are grateful to the Department of Science and Tech-
nology, New Delhi for financial support through the scheme no.
SR/S2/CMP-82/2006.
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Biographies
D.S. Dhawale received his B.Sc. degree (2005) in general physics, M.Sc. degree (2007)
in materials science and Ph.D. (2009) in liquefied petroleum gas sensor performance
of polyaniline based heterojunctions from the Shivaji University, Kolhapur, India
(M.S.). His present research interest includes synthesis of polyaniline based hetero-
junctions, metal oxides for solar cells, dye sensitized solar cells, room temperature
(300 K) gas sensors and supercapacitors.
D.P. Dubal received his B.Sc. degree (2006) in general physics, M.Sc. degree (2008)
in solid state physics and presently doing Ph.D. in preparation and characterization
of electrodeposited Fe doped MnO2 thin films for supercapacitor application, from
the Shivaji University, Kolhapur, India (M.S.). His present research interest includes
synthesis of oxide thin films and their applications.
A.M. More received his B.Sc. (2003) in general physics from Shivaji University, Kol-
hapur (India), M.Sc. (2005) in general physics from Pune University, Pune, and Ph.D.
(2009) in synthesis of nanocrystalline TiO2 thin films by chemical methods and their
applications in dye sensitized solar cells. He is presently working as a post doc. fellow
at Hanyang University, South Korea. His research interests are in the field of syn-
thesis of thin films of metal oxide by chemical, electrochemical methods and their
applications in solar cells, dye sensitized solar cells, gas sensors and supercapacitors.
T.P. Gujar received his B.Sc. (2001) in general physics, M.Sc. (2003) in materials sci-
ence and Ph.D. (2006) in oxide film preparation and application in supercapacitors,
from Shivaji University, Kolhapur (India). He is presently working as a post doc. fel-
low at KIST, Republic of Korea. His research interests are in the field of synthesis of
thin films of metal oxide by vacuum, chemical, electrochemical methods, and their
applications in supercapacitors and gas sensors.
C.D. Lokhande received his Ph.D. in 1984. He was a Humboldtian (Hahn-Meitner
Institute, Berlin, Germany). He is fellow of Institute of Physics. He is currently a
professor in the Department of Physics, Shivaji University, Kolhapur, India (M.S.).
He has been continuously engaged in the research field more than last 30 years. His
research interest includes the synthesis of thin films of metal chalcogenides, metal
oxides, conducting polymers and ferrites by chemical, electrochemical methods and
their applications in dye sensitized solar cells, gas sensors, energy storage devices,
etc.