Vacuum deposited WO

3
thin lms based sub-ppm H
2
S sensor
Niyanta Datta
a
, Niranjan Ramgir
a,
*
, Manmeet Kaur
a
, Mainak Roy
b
, Ranu Bhatt
a
, S. Kailasaganapathi
a
,
A.K. Debnath
a
, D.K. Aswal
a
, S.K. Gupta
a
a
Thin Films Devices Section, Technical Physics Division, Bhabha Atomic Research Center, Trombay, Mumbai 400 085, India
b
Solid State Chemistry Section, Chemistry Division, Bhabha Atomic Research Center, Trombay, Mumbai 400 085, India
a r t i c l e i n f o
Article history:
Received 28 July 2011
Received in revised form
13 February 2012
Accepted 8 March 2012
Keywords:
Thin lms
Vacuum deposition
Defects
Surface properties
a b s t r a c t
A simple method of vacuum deposition using W foils has been utilized to fabricate Au-incorporated WO
3
thin lm sensors. Incorporation of Au has been demonstrated to improve both the sensitivity and the
selectivity of the sensor lms towards H
2
S. The effect of operating temperature, Au loading and gas
concentrations have been investigated and correlated with the observed sensitivity values to determine
the optimum conditions for realizing H
2
S sensor with better sensing properties. The sensor lm con-
taining 2.32 at.% Au detected H
2
S selectively with an enhanced sensitivity of S 16 (1 ppm) at an
operating temperature of 250

C. The enhanced response kinetics has been conrmed further using
Raman and work function measurements.
2012 Elsevier B.V. All rights reserved.
1. Introduction
WO
3
, an n-type wide band gap material, has demonstrated its
potential for realizing highly sensitive and selective sensors
towards different gases [1,2]. Similar to other semiconducting
oxides like SnO
2
and ZnO, its surface is characterized by the pres-
ence of oxygen vacancies. These oxygen vacancies act as donor
levels and contribute in the governing sensing mechanism [3].
Various sensors including C
2
H
5
OH, O
3
, NH
3
, NO
x
, H
2
S, have been
attempted and realized using WO
3
in conventional thin lms as
well as nanoforms [4e7]. Thin lm based sensors have been
commonly deposited using techniques like micromachining, sput-
tering, thermal evaporation and solegel [8]. To improve sensitivity
and selectivity, the host matrix is generally modied with various
sensitizers including Pd, Pt, Ag, Au, and often a bimetallic sensitizer
is also considered [9e12]. In particular, Au incorporation resulted in
improved sensing characteristics like faster response time and
increased sensitivity values and accordingly, has been found to be
a promising sensitizer [13]. Modulation of sensing properties based
on Au has been mainly ascribed to the electronic sensitization
mechanism. Use of Au has been demonstrated to improve the
sensing performance towards different gases like NO
2
, NO
x
H
2
S, H
2
,
and NH
3
[14e18]. Of these hydrogen sulde (H
2
S) is one of the
highly toxic and ammable gases that is being employed exten-
sively in various industrial applications. In particular, its exposure
affects humans nervous system and could cause loss of
consciousness at a very lowconcentration. Its threshold limit value
has been set to 10 ppm and hence detection at low or sub-ppm
concentrations has become the focus of research. Besides, as the
catalytic decomposition of H
2
S is known to occur between 300 and
400

C [19], the H
2
S sensors must be operated below 300

C. Ion-
escu et al. have reported the sub-ppm detection of H
2
S upto 20 ppb
with a sensitivity value of w1.1 (S 1.25 towards 50 ppb) at an
operating temperature of 250

C. Although the sensors responses
were good, nanoparticles formation via advanced gas deposition
unit is tedious [2]. Tao et al. have investigated the effect of different
doping element on H
2
S sensing properties of WO
3
lms deposited
by RF plasma sputtering [10]. There report lacks the systematic
investigation of doping element and its concentration in the host
matrix to realize a better sensing material. Hence to know and
understand under what conditions sensitizers imparts sensitivity
towards a particular gas demands a detailed investigation.
In the present work we report a systematic investigation of the
gas sensing properties of pure and Au-incorporated WO
3
sensor
thin lms towards H
2
S. The sensor lms have been realized using
a simple method of vacuum deposition. We have investigated the
effect of sensor operating temperature, Au loading, and gas
concentration on sensing properties to determine the optimum
conditions for the detection of H
2
S gas. Additionally, Raman and
work function measurements both with and without the test gases
* Corresponding author. Tel.: 91 22 25595839; fax: 91 22 25505296.
E-mail address: niranjanpr@yahoo.com (N. Ramgir).
Contents lists available at SciVerse ScienceDirect
Materials Chemistry and Physics
j ournal homepage: www. el sevi er. com/ l ocat e/ mat chemphys
0254-0584/$ e see front matter 2012 Elsevier B.V. All rights reserved.
doi:10.1016/j.matchemphys.2012.03.080
Materials Chemistry and Physics 134 (2012) 851e857
have been performed to elucidate the nature of interaction with the
sensor lm. Our studies indicates that Au-incorporated WO
3
sensor
lms could detect sub-ppm (50 ppb, S 2.7) H
2
S selectively at an
operating temperature of 250

C.
2. Experimental section
2.1. Sensor fabrication
The steps involved in the fabrication of sensor lms are illus-
trated schematically in Fig. 1. In brief, Al
2
O
3
substrates were rst
cleaned by ultrasonicating in solvents namely trilene, acetone and
methanol. Contact electrodes were then predened on these
substrates using Pt-wire and a high temperature drying Au paste
followed by curing at 850

C for 10 min. The predened electrodes
were protected by masking with molybdenum foils. W lms
(w600 nm thick) were then vacuum deposited using W-foil
(purity: 99.99%, dimensions 1 4 cm) under application of a very
high current (w80 A) in a base vacuumof 2 10
4
mbar. In order to
prepare Au-incorporated WO
3
lms a sandwich layer of
W(300 nm)/Au (t nm)/W(300 nm) (t taking values 1.86, 3.3, 7.4 and
13.3 nm corresponding to 0.55, 1.23, 2.32 and 3.95 at.%, as
measured using energy dispersive X-ray analysis (EDAX)) were
deposited onto alumina substrates. The resulting lms were then
subjected to post deposition annealing at 600

C for 1 h in quartz
tubular furnace under constant oxygen (O
2
) ow of 100 sccm. In
order to make electrical contacts 120 nm thick Au layer was
deposited using a mask having 400 mm spacing.
2.2. Instruments and analysis
Surface morphology of the as-grown lms was investigated
using scanning electron microscopy, SEM, (TESCAN, model: TS
5130MM) equipped with EDAX unit. X-ray diffraction measure-
ments were performed using Rigaku expert machine with CuK
a
radiation having 1.5406 wavelength. Raman spectra were recor-
ded on a Labaram-I spectrometer in a backscattering geometry at
room temperature. Prior to measurements sensor samples were
exposed to H
2
S at an elevated temperature of w100

C. The change
in signal was better observed for higher dose of exposure
(100 ppm) and hence was chosen for the experiments. Kelvin probe
contact potential difference (CPD) measurements were carried out
using SKP Kelvin Probe 4.5 from KP Technology Ltd. UK. All the
measurements were performed at room temperature and ambient
conditions using Au electrode having tip diameter of 2 mm. For
better average value of the work function the electrode tip was
scanned across the sample surface (Raster scan) and the relative
variation in the CPD was measured. Sensor samples were exposed
to 100 ppm of H
2
S at an elevated temperature of w100

C before
measuring the work function [20]. Sensing measurements were
performed in a static system as described elsewhere [21]. In brief,
sensor lms were mounted in a stainless steel test-chamber
(volume: 250 cm
3
) equipped with a temperature control unit. The
desired temperature was achieved using a Pt-wire based heater
attached to the backside of the sensor lm. The desired concen-
tration of the test gas was achieved by injecting the measured
quantity of commercial gas inside the chamber. Commercial grade
gases having 1000 ppmconcentration of desired gas in N
2
, obtained
in half liter cylinders were used to control the nal concentration.
The resistance of the lmwas monitored and acquired as a function
of time using a personal computer equipped with Labview soft-
ware. Recovery of the sensors was achieved by opening the housing
to the atmosphere.
Sensor response or sensitivity (S) was calculated using the
relation:
S
R
a
R
g
(1)
for reducing gases namely H
2
S, CH
4
and NH
3
, and
S
R
g
R
a
(2)
for oxidizing gases namely Cl
2
, NO
2
and NO, where R
a
and R
g
are
resistances in air and test gases, respectively. Response and
Fig. 1. Steps involved in the fabrication of (a) pure WO
3
and (b) Au-incorporated WO
3
sensor devices.
N. Datta et al. / Materials Chemistry and Physics 134 (2012) 851e857 852
recovery times were dened as the time needed for 90% of total
change on exposure to test gas and fresh air, respectively.
3. Results and discussion
3.1. Structural and morphological characteristics
The resultant W lms after vacuum depositions are black in
color, which when oxidized at an elevated temperature of 600

C in
O
2
environment gets transformed into greenish yellow color.
Fig. 2(a)e(e) shows the SEM images of pure and Au-incorporated
WO
3
thin lms. It is seen that pure lm consists of large number of
microparticles having an average grain size of w5.4 mm containing
microcracks and even cavities. Additionally, these particles are
seemed to consist of large number of nanosized grains with size
<100 nm. The sensor lms color changes from greenish yellow to
violet purple upon incorporation of Au. Besides it also causes
elimination of microcracks. Additionally, grain size decreases
(Fig. 2(f)) and porosity increases with Au incorporation. Fig. 3
shows the XRD prole of Au-incorporated (2.32 at.%) WO
3
thin
lm. The pattern matches with the monoclinic crystal structure of
WO
3
[22] having lattice parameters of a 7.309, b 7.545 and
c 7.689 , respectively.
3.2. Gas sensing properties of pure and Au-incorporated WO
3
sensor lms
Fig. 4 shows the sensing response curves recorded for pure WO
3
towards 1 ppm of H
2
S at an operating temperature of 250 and
225

C, respectively. The sensitivity of sensor lm towards H
2
S is
not affected much with the operating temperature however
a strong variation in sensor lms recovery time is seen. Recovery
time is observed to decrease with increase in operating tempera-
ture. From Fig. 4(c) it is clear that the sensor responded with fairly
good sensitivity and a reasonable recovery time at an operating
temperature of 250

C and hence was chosen for all the further
experiments.
To determine the optimum Au concentration in the host matrix
a systematic investigation of Au loading and its effect on sensitivity
towards H
2
S have been carried out. A typical bell shaped curve (S
vs. Au concentration) as shown in Fig. 5(a) with maxima for WO
3
thin lms containing 2.32 at.% Au was observed. The low Au
concentration has a discontinuous distribution causing insufcient
catalytic activity leading to smaller sensitivity, while higher
concentration gives continuous distribution leading to lower initial
resistance and thence lower sensitivity value [23]. An overall trend
of decrease in the air resistance (measured at xed temperature of
250

C) with Au incorporation is seen (Fig. 5(a)) that further
corroborates the ndings. Fig. 5(b) shows the selectivity histogram
of pure and Au-incorporated (2.32 at.%) sensor lm at an operating
temperature of 250

C towards 1 ppm of different gases. Interest-
ingly, both pure and Au-incorporated samples exhibited
a maximum sensitivity towards H
2
S. However, upon Au incorpo-
ration the sensor became highly sensitive and thereby selective
towards H
2
S. A negligible response towards all the other interfering
gases namely NH
3
, Cl
2
, CO, CH
4
, CO
2
and NO
2
was observed. Our
initial ndings suggested that pure WO
3
responded with maximum
sensitivity towards H
2
S in comparison to that of Au modied lms
Fig. 2. SEM images of (a) pure and Au-incorporated WO
3
thin lms containing (b) 0.55, (c) 1.23, (d) 2.32 and (e) 3.95 at.% Au, and (f) a plot of average grain size vs. Au content in
WO
3
thin lm.
Fig. 3. XRD prole of Au (2.32 at.%) incorporated WO
3
sensor thin lm.
N. Datta et al. / Materials Chemistry and Physics 134 (2012) 851e857 853
[24]. One of the reasons for the difference in the sensitivity values
in the two cases could be the gas sensing measurement units that
were used in both the cases. In particular, earlier measurements
were performed in a static system 250 cm
3
(cylindrical) with one
end enclosed/rested on a heater (w5 cm diameter). In the present
work the sensing measurements were preformed with Pt-wire
(R 2e3 U) heater attached at the backside of the sensor thereby
providing a localized heating. In former case at high temperatures
the whole set-up was heating up and is probably responsible for the
difference in measurements.
A systematic investigation of the effect of gas concentration was
then performed at an operating temperature of 250

C. Fig. 6 shows
the response curves of pure and Au-incorporated WO
3
sensor lms
recorded with the increasing concentration of test gas. As is evident
from the gure sensitivity is found to increase with gas concen-
tration. Au-incorporated WO
3
lms exhibited a better sensing
performance in comparison with that of pure WO
3
sensor lms. For
example, towards 0.7 ppm of H
2
S, pure WO
3
lms showed a sensi-
tivity of 2.9 with a response and recovery time of 106 s and 32 min,
while Au-incorporated sample (2.32 at.%) exhibited an increase in
the sensitivity to 12 with a response and recovery times of 88 s and
18 min, respectively. Moreover, Au-incorporated thin lms were
able to detect as lowas 50 ppb of H
2
S with a sensitivity value of 2.7.
For practical applications, the reproducibility and the stability of
sensing-device are also important. In the present case, the sensors
developed under identical conditions (same and different batches)
exhibited similar response towards H
2
S. Moreover, the stability
measurements performed over a period of 15 days indicate themto
be quite stable. For example, the sensor sample with 2.32 at.% Au
exhibited a variation of about 8% in its initial resistance value for
this period. A detailed investigation of the long termstability of the
sensor lms is underway.
3.3. Raman and work function measurements
Raman investigations of the sensor lm before and after expo-
sure to H
2
S have also been performed as it is known to give the
ngerprint of the material. Fig. 7(a) shows the Raman spectra
(recorded at room temperature) of a bare WO
3
lms before and
after exposure to H
2
S. Both the spectra invariably exhibit a series of
sharp peaks at wavenumbers lower than 250 cm
1
attributed to
vibrational modes of the WO
3
lattice i.e. the translational and
rotational motion of WO
6
octahedra in the same unit cell. They also
exhibit peaks at intermediate frequency region (200e400 cm
1
)
assigned to the bending modes of OeWeO bridging bonds and at
high frequency region (600e900 cm
1
) attributed to the stretching
modes of WeO bonds [25,26]. The Raman peaks observed at
approximately 60, 73, 136, 274, 328, 718 and 809 cm
1
and
a shoulder at w96 cm
1
are characteristic of crystalline monoclinic
g-phase of WO
3
. The monoclinic g-phase is the most stable room
temperature phase of WO
3
and has been reported for both WO
3
powder and nanoforms [27,28]. The ngerprint Raman peak at
approximately 33 cm
1
could not be detected for the samples due
to experimental limitations [notch cut off]. Additionally, the
absence of the 950 cm
1
Raman peak in both the samples is
indicative of their high crystalline nature [29]. Apart from the
Raman peaks of the g-phase, an additional peak at w40 cm
1
attributed to the orthorhombic b-phase is observed. The low
frequency Raman modes involve tilted motion of the oxygen cages
around the Watoms and/translational motion of WO
6
octahedra in
the same unit cell. Strong polarizability modulation of these lattice
vibrational modes during the evolution of a new phase makes
Raman spectroscopy a more sensitive technique than XRD for
studying phase transition in WO
3
. Reversible transition from g to
b phase has been reported at w300

C for microcrystalline WO
3
Fig. 4. Sensors response curves at (a) 250, (b) 225

C and (c) the variation in sensitivity and recovery times as a function of an operating temperature for pure WO
3
thin lms
measured upon exposure to 1 ppm of H
2
S.
N. Datta et al. / Materials Chemistry and Physics 134 (2012) 851e857 854
powder [25] and for nanowires above 227

C [26]. However, room
temperature observation of the b-phase for the vapor deposited
thin lm samples is an interesting and notable exception. Upon
exposure to H
2
S, intensity of the Raman peaks due to the g-phase
relative to that of the peak at 40 cm
1
(considered to be the
ngerprint of the b-phase) reduced signicantly, but their peak
positions remained almost unaltered. The two peaks at w60 and
73 cm
1
almost merged to form a single broad band. Since, inter-
action of WO
3
with H
2
S is likely to occur at the lm surface, the
observation indicates a further stabilization of the b-phase on the
lm surface at the expense of the g-phase. Additionally a decrease
in the intensity of the peaks corresponding to the stretching modes
was also observed.
Raman spectra, before and after exposure to H
2
S, of Au-incor-
porated WO
3
are depicted in Fig. 7(b). Although the spectrumof the
unexposed sample is qualitatively similar to that of bare WO
3
,
intensity of the peak at w40 cm
1
is much higher than that at
60 cm
1
. Moreover, the broad hump at w96 cm
1
in the spectrum
of bare WO
3
appears as a distinct peak for AueWO
3
. These clearly
indicate the relative enhancement of the orthorhombic b-phase.
Upon exposure to H
2
S, intensity of the lattice and stretching modes
reduced marginally, whereas no signicant change in the intensity
Fig. 5. Response curves of (a) pure and (c) Au-incorporated (2.32 wt.%) WO
3
thin lms towards sub-ppm concentration of H
2
S at an operating temperature of 250

C and cor-
responding variation in sensitivity with gas concentration (c) and (d).
Fig. 6. (a) Effect of Au loading on sensitivity towards 1 ppm H
2
S, and on the air resistance at an operating temperature of 250

C. (b) Selectivity histogram pure WO
3
and Au-
incorporated WO
3
thin lm sensors towards different gases at an operating temperature of 250

C.
N. Datta et al. / Materials Chemistry and Physics 134 (2012) 851e857 855
of the bending modes of WO
3
was observed. Interestingly, in
contrast to the bare WO
3
, intensity of the peak at w40 cm
1
relative
to that at 60 cm
1
got reduced after exposure to H
2
S. Augmentation
of Raman signals due to the surface enhanced resonance Raman
effects of the embedded Au may contribute towards the anomalous
intensity variation for AueWO
3
sensor lms.
Fig. 8 shows the work function area scan recorded for 3.3 mm
2
of sensor samples before and after exposure to 100 ppm of H
2
S.
Upon exposure to H
2
S, the CPD over the measured area is observed
to vary. The color variation indicates the localized variation in the
CPD. Table 1 illustrates the nal work function values of the sensor
samples calculated taking the average of the relative variation in
the CPD. As is clearly evident the incorporation of Au in the WO
3
resulted in work function decrease by 0.25 eV. Besides exposure to
H
2
S causes changes in the work function of pure and Au-incorpo-
rated WO
3
samples by 30 and 11 meV, respectively. The small
variation in the work function of Au-incorporated sample is
attributed to the faster reaction kinetics (recovery time). This result
is in accordance with and corroborates further the ndings of
Raman investigations.
3.4. Gas sensing mechanism
It is established that interaction of H
2
S with WO
3
leads to the
generation of large number of oxygen vacancies [10]. The inter-
action leads to the introduction of new energy levels in the mid
gap states of WO
3
. Besides, incorporation of doping elements in
particular Au has been known to impart the sensitivity in the
host material mainly via electronic sensitization mechanism [26].
In this the additives enhance the rate of reaction by providing
the additional active sites. The interaction with the test gas
mainly occurs on the Au surface and the corresponding changes
Fig. 7. Raman spectra recorded for (a) pure WO
3
and (b) Au-incorporated WO
3
sensor lms before and after exposure to H
2
S gas at room temperature.
Fig. 8. 2-D work function map of pure WO
3
sensor lms (a) before and (b) after exposure to H
2
S and Au-incorporated WO
3
(c) before and (d) after exposure to H
2
S.
N. Datta et al. / Materials Chemistry and Physics 134 (2012) 851e857 856
are transferred immediately to the host matrix reected as a fast
drop in the resistance of the sample. This is expected to
contribute for improving both the response and the recovery
times of the sensor lms. Further, the oxygen vacancies can
easily be reoxidized upon exposure to fresh air thereby assuring
complete recovery.
4. Conclusions
In summary, we have deposited pure and Au-incorporated WO
3
sensor thin lms using a simple technique of vacuum deposition.
Effect of operating temperature, gas concentration, and Au loading
has been explored and correlated with the observed sensitivity
values to determine the optimum condition for improved sensing
performance towards H
2
S. The sensor lm containing 2.32 at.% of
Au detected H
2
S selectively and sensitively (S w16) at an oper-
ating temperature of 250

C. The enhanced reaction kinetics is
mainly attributed to Au and has been conrmed using both the
Raman and the work function measurements. Our results clearly
indicate that the WO
3
thin lms can be made selective and sensitive
towards sub-ppm H
2
S by a proper control over the process
parameters namely operating temperature, doping element (Au)
and its concentration in the host matrix.
Acknowledgments
This work is partly supported by DAE-SRC Outstanding
Research Investigator Award (2008/21/05-BRNS) and Prospective
Research Funds (2008/38/02-BRNS) granted to D.K.A. Authors also
thank Dr. A.K. Chauhan and Mr. Arvind Kumar for their help with X-
ray diffraction and work function measurements, respectively.
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Table 1
Work function values recorded for sensor samples before and after exposure to H
2
S.
Sample name F, before exposure (eV) F, after exposure (eV)
Pure WO
3
5.221 5.191
Au-incorporated WO
3
4.973 4.962
N. Datta et al. / Materials Chemistry and Physics 134 (2012) 851e857 857