1004
4, FEBRUARY 15, 2016
Performance of Si-Doped WO3 Thin Films for
Acetone Sensing Prepared by Glancing
Angle DC Magnetron Sputtering
Artur Rydosz, Aleksandra Szkudlarek, Magdalena Ziabka, Krzysztof Domanski,
Wojciech Maziarz, and Tadeusz Pisarkiewicz
Abstract— This paper presents the acetone sensing
characteristics of Si-doped (1 at.%) tungsten oxide thin
films prepared by glancing angle dc magnetron sputtering. The
performance of Si-doped WO3 sensors in the concentration range
of 0.04–3.8 ppm at operating temperatures of 150 °C–425 °C
has been investigated. Doping of the tungsten oxide film
with Si significantly decreases the limit of detection of
acetone compared with the pure WO3 sensors reported
in the literature. The gas sensor’s response (S) to acetone
was defined as the resistance ratio S = Rair /Rgas , where
Rair and Rgas are the electrical resistances for the sensor in air
and in gas, respectively. The maximum response measured in
this experiment was S = 40.5. Such response was measured in
the presence of 3.8 ppm of acetone at an operating temperature
of 425 °C using a Si-doped (1 at.%) WO3 thin film deposited
at 300 °C and annealed at 300 °C for 4 h in air. The films
phase composition, microstructure, and surface topography
have been assessed by X-ray diffraction, scanning electron
microscope, atomic force microscope, and energy dispersive
X-ray spectroscopy methods.
Index Terms— Gas sensor applications, WO3 films, magnetron
sputtering, acetone sensing.
I. I NTRODUCTION
E XHALED acetone is considered as a biomarker for
non-invasive diagnosis of type-1 diabetes [1]–[5]. The
exhaled acetone is usually in the range of 0.3 - 1.1 ppm
for healthy people, and above 2 ppm for people with
diabetes [6]. In order to measure such low biomarker
concentrations, laboratory systems such as: PTR-MS [7],
SIFT-MS [8], [9], amongst other examples, can be applied.
Manuscript received June 21, 2015; revised October 23, 2015; accepted
October 26, 2015. Date of publication November 5, 2015; date of current
version January 21, 2016. This work was supported by the National Science
Centre Poland under Grant DEC-2013/09/N/ST7/01232. The associate editor
coordinating the review of this paper and approving it for publication was
Prof. Boris Stoeber. (Corresponding author: Artur Rydosz.)
A. Rydosz, W. Maziarz, and T. Pisarkiewicz are with the
Department of Electronics, AGH University of Science and Tech-
nology, Kraków 30-059, Poland (e-mail: artur.rydosz@agh.edu.pl;
maziarz@agh.edu.pl; pisar@agh.edu.pl).
A. Szkudlarek is with the Academic Centre for Materials and
Nanotechnology, AGH University of Science and Technology, Kraków 30-059,
Poland (e-mail: aleszkud@agh.edu.pl).
M. Ziabka is with the Department of Ceramics and Refractories,
AGH University of Science and Technology, Kraków 30-059, Poland (e-mail:
ziabka@agh.edu.pl).
K. Domanski is with the Institute of Electron Technology, Piaseczno 05-500,
Poland (e-mail: kdoman@ite.waw.pl).
Digital Object Identifier 10.1109/JSEN.2015.2496212
1558-1748 © 2015 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.
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IEEE SENSORS JOURNAL, VOL. 16, NO.
However, the breath analysis as a supplementary tool for
diagnosing and monitoring diabetes makes sense only in case
of utilization of portable analyzers. This need has created
a market for gas sensors. However, commercially available
acetone gas sensors have detection limit at level of several
tens part per million (ppm). Therefore, many researchers have
focused on investigation of semiconductive oxides with higher
sensitivity to the acetone, i.e. SnO2 [10], ZnO [11], TiO2 [12].
One of the promising materials for acetone sensors is tungsten
oxide (WO3 ). It is a n-type semiconductor with a band
gap from 2.6 eV (highly crystalline) to 3.3 eV (amorphous)
and monoclinic crystal structure. WO3 is a very attractive
material, because it shows a high catalytic behaviour both in
oxidation and reduction reactions on its surface [13]. Recently,
various chemical or physical methods have been developed
successfully to synthesize nanostructured tungsten oxides,
i.e. sol-gel technique [14], electrodeposition [15], mag-
netron sputtering [16], solution drop coating [17], electron
beam evaporation [18], hot-wire CVD technique [19], laser-
ablation technique [20], hydrothermal technique [21], etc.
Gao et al. [22] have reported acetone gas sensors based on
porous WO3 -Cr2 O3 thin films prepared by a sol-gel method.
The obtained gas response (S) defined as: S = Rair /Rgas ,
where Rair is the film resistance in air and Rgas is the
resistance at a given concentration of analyte was around 2, 4,
and 8.91 for 5 ppm, 10 ppm, and 20 ppm acetone concentra-
tions, respectively. The relative humidity (RH) and operating
temperature (OT) were set to: 20% and 320 °C, respectively.
Recently, Righettoni et al. [23], [24] have reported acetone
vapour sensing properties of 10 mol% Si-doped WO3 as an
alternative to doping with potentially toxic Cr. The obtained
results are very promising: the sensitivity (S = Rair /Rgas − 1)
is around 1.54 for 0.5 ppm acetone (dry gas at 350 °C),
and around 0.11 for 80 ppb acetone concentration (90% RH
at 350 °C). Wang et al. [25] have reported flower-like WO3
architectures synthesized via a microwave-assisted method
with sensitivity (S = Rair /Rgas − 1) around 7 for 100 ppm
acetone concentration at 300 °C operating temperature and
fast response for acetone (∼1 s under 100 ppm exposure).
Chávez et al. [26] have reported the palladium-functionalized
WO3 nanowires obtained by a drop-coating method. The
reported sensitivity for 1000 ppm acetone concentration is
around 1.35 and OT has been set to 300 °C. Luo et al. [27]
 RYDOSZ et al.: PERFORMANCE OF Si-DOPED WO3 THIN FILMS FOR ACETONE SENSING
Fig. 1. Schematic view of the WO3 nanorods array fabrication by glancing-
angle dc magnetron sputtering deposition.
have reported gas sensing behaviour of La2 O3 -added
WO3 nanoparticles prepared by a sol-gel method. The
maximum gas response (WO3 +1 mol%-La2O3 ) was obtained
at 265 °C and it was around 20 for 50 ppm acetone.
Chen et al. [28] have reported acetone-sensing properties
of tungsten trioxide nanocrystals. The sensitivity (S = Rair /
Rgas − 1) results for 2 ppm, 5 ppm, 10 ppm and 1000 ppm
were 4, 5.5, 8, 43, respectively.
During the current study the glancing angle
deposition (GLAD) methodology was applied to obtain
WO3 thin films with high surface to volume ratios. The
GLAD technique provides the possibility for fabrication of
well-ordered and sophisticated nanostructures, e.g. nanorods,
nanocolumns, etc. [29]–[31] by manipulating the deposition
angle, α, and substrate rotation angle, ϕ. Fig.1. shows a
schematic view of GLAD configuration. The sensitivity of
chemiresistive gas sensors is highly dependent on the surface
to volume ratio of the films [13]. To improve the sensitivity
the post-deposition annealing treatments were performed.
The gas sensing films were deposited on silicon gas sensors
substrates with Au interdigitated electrodes. The sensor
performance was investigated for a wide range of operating
temperatures and gas concentrations.
II. E XPERIMENT
A. Preparation of Films
It is believed that the sensor response can be improved
both by doping and the increase of sensitive surface areas
of the materials. Therefore, the preparation method for the
sensing materials plays an important role. After standard
cleaning process, Si-doped WO3 thin films were deposited
onto glass and silicon gas sensor’s substrates by glancing angle
DC magnetron sputtering. The interdigitated Au electrodes
(interdigital spacing 1-2 μm) on silicon substrates were used
to reduce the resistance of highly resistive tungsten oxide
material.
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1005
The vacuum chamber was initially evacuated to a base
pressure of 5.0 · 10−6 mbar. A tungsten metal target
of 4 diameter (99.95% purity) was employed for reactive
sputtering. The silicon dopant particles (purity of 99.95%)
have been placed on the tungsten target. A home-made
GLAD manipulator equipped with a DC motor maintained
the azimuthal sample rotation at a speed of 20 rpm during
each deposition. The substrate tilt angle was manually set to
α = 80° before each run. The W target was placed at a dis-
tance of 80 mm from centerline of the substrate. A sputtering
power of 100 W was initially applied to the target while intro-
ducing Ar into the chamber to ignite the plasma. The target
was presputtered in Ar for 10 min prior to film deposition.
The WO3 films were deposited with constant 90%Ar/10%O2
ratio. The flows of argon and oxygen were controlled by
MFC (mass flow controllers). The sputtering power was set
to 150 W for reactive deposition. The deposition pressure
was kept constant at 3.0 · 10−2 mbar and the duration of
deposition was set to 30 min to achieve 400 nm film thickness.
The samples were deposited at various temperatures: room
temperature (RT), 200 °C, and 300 °C. The substrates were
heated by resistive heating (Thermocoax Sas, France) and
the deposition temperature was controlled by Eurotherm 2408
PID controller. Films were characterized immediately after
deposition and also after post-deposition annealing treatments
at 300 °C, 400 °C, and 500 °C in air for 4 h.
B. Films Characterization
The crystallographic structure of films was determined
with X-ray diffraction, X’Pert PRO MPD PANalytical sys-
tem (Cu Kα1 ). Fig.2 shows the X-ray Diffraction (XRD)
experiment results. The measurements have been performed
after the deposition process and additionally after annealing.
The XRD patterns reveal reflection from the WO3 monoclinic
phase described with the space group P21/n (JCPDS database
01-083-0950, parameters: a = 7.3008 Å, b = 7.5389 Å,
c = 7.6896 Å, α = γ = 90°, β = 90.89°). It can
be observed that the crystallinity increases with increasing
annealing temperature. Thin films deposited at temperatures
higher than 200 °C are partially crystallized.
The surface topography of the films was determined using
Atomic Force Microscope (AFM) technique. The images have
been gathered out by NTMDR Ntegra Aura in semicontact
mode with Si top of 8 nm nominal diameter. Fig. 3, Fig.4
and Fig. 5 show AFM images of WO3 thin films deposited
and annealed at various temperatures. Each AFM image was
obtained using an area of 3 μm×3 μm. The root mean square
surface roughness of the deposited films ranged from 23 nm to
140 nm. It can be seen that the film surface for films deposited
and annealed at 300 °C and 500 °C, respectively, shows a large
quantity of cracks comprised of large islands with different
diameters dispersed over the whole scanned area.
The morphology and film thickness of the WO3 thin
films and nanorods were examined by Scanning Electron
Microscopy FEI Versa 3D DualBeam. Fig. 6 shows cross-
sectional view Scanning Electron Microscope (SEM) images
of Si:WO3 deposited on glass substrate and annealed at var-
ious temperatures. The films deposited at lower temperatures
 1006
Fig. 2. XRD diffractograms of WO3 thin films deposited at different
temperatures: (a) RT, (b) 200 °C, and (c) 300 °C and annealed at 300 °C,
400 °C and 500 °C.
demonstrated cauliflower morphology (Fig.6a, Fig.6b, Fig.6d,
and Fig.6e) due to kinetic roughening process. When deposi-
tion temperature increases the nanorods morphology becomes
readily apparent (Fig.6g, Fig.6h, Fig.6i). Brossmann et al. [32]
have stated that existence of a possible threshold temperature
in metal oxides can be ascribed to slower surface diffusivity
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IEEE SENSORS JOURNAL, VOL. 16, NO. 4, FEBRUARY 15, 2016
Fig. 3. AFM micrographs of WO3 thin films deposited at room temperature
and annealed at: (a) 300 °C, (b) 400 °C and (c) 500 °C.
of oxygen anions compared with cations, which suggest the
oxygen surface diffusion rates might be the limiting factor in
surface morphology evolution [32]. The columnar nature of the
nanorods comes from atomic shadowing effect. The roughness
fluctuations on the substrate surface make some region receive
more material flux than others due to shadowing. Annealing of
 RYDOSZ et al.: PERFORMANCE OF Si-DOPED WO3 THIN FILMS FOR ACETONE SENSING
Fig. 4. AFM micrographs of WO3 thin films deposited at 200 °C and
annealed at: (a) 300 °C, (b) 400 °C and (c) 500 °C.
films deposited at lower temperatures (Fig.6c, Fig.6f) yielded
crystallization to the monoclinic/triclinic WO3 phase accom-
panied by a morphological deviation into nanorods networks,
however, without significant boundary between nanorods.
In order to verify the composition and particularly the
doping content of obtained samples, energy dispersive
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1007
Fig. 5. AFM micrographs of WO3 thin films deposited at 300 °C and
annealed at: (a) 300 °C, (b) 400 °C and (c) 500 °C.
x-ray spectroscopy (EDX) was carried out. Fig.7 shows the
EDX spectra of Si-doped WO3 after deposition at different
temperatures and annealing at 300 °C/400 °C/500 °C for
4h in air. The spectra indicate the characteristic x-ray peaks
 1008 IEEE SENSORS JOURNAL, VOL. 16, NO. 4, FEBRUARY 15, 2016

Fig. 6. SEM images of (a) 300 °C-annealed, (b) 400 °C-annealed, (c) 500 °C-annealed Si:WO3 thin films deposited at room temperature, (d) 300 °C-annealed,
(e) 400 °C-annealed, (f) 500 °C-annealed Si:WO3 thin films deposited at 200 °C, (g) 300 °C-annealed, (h) 400 °C-annealed, and (i) 500 °C-annealed Si:WO3
thin films deposited at 300 °C.

corresponding to O, W and Si atoms present in the sample.
From the EDX analysis, the amount of Si was found to be
varied from 0.5 at.% for sample deposited at room temperature
and annealed at 300 °C to 2.0 at.% for sample deposited
at 300 °C and annealed at 500 °C. However, it has to be
underlined that it is not easy to evidence Si at low concen-
trations when the W is present at high concentration, because
all energies of the SiK and WM are very close. The values of
the characteristic energies of the SiK are 1.740 keV for SiKα
and 1.829 keV for SiKβ. For WM are 1.776 keV for WMα,
1.835 keV for WMβ, 2.035 for WMγ and 1.379 keV
for WMz2 [33]. The absence of any other peaks except
those due to O, W and Si indicates that we have obtained
high purity Si-doped WO3 samples without any elemental
impurities incorporated during the deposition and annealing
processes.
C. Gas Sensing Test System
The gas sensing characteristics were measured in a gas
sensing system presented in Fig.8. The electrical resistance
of the sensors was acquired and continuously monitored using
a digital electrometer (Keithley 6517) controlled by a PC with
homemade LabView based software. The sampling interval
was set to 1 s. The resistance was measured at operating
temperatures ranging from 150°C to 425°C as a function
of acetone concentration in a range between 0.04 ppm and
3.8 ppm. The successive sensors’ temperatures were calcu-
lated with the use of the measured resistance of Pt sensor
heaters and their TCR values. In order to reduce the impact
of the temperature difference related to the flowing gas, a
PID system stabilizing the sensor working temperature is
necessary.
In this study, the authors used a quartz tube-shaped measure-
ment chamber having a volume of approximately 45 cm3 and
the gas flux was set to 50 sccm. The gas sensor’s response (S)
was defined as S = Rair /Rgas , where Rgas is the sensors
resistance in a sample gas, in this case acetone and Rair is the
sensors resistivity in the air with 50% relative humidity. The
response/recovery times are determined in 10-90 percentile
range for a single gas/air impulse and depend directly on the

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 RYDOSZ et al.: PERFORMANCE OF Si-DOPED WO3 THIN FILMS FOR ACETONE SENSING
Fig. 7. EDX spectra of Si-doped WO3 deposited at different temperatures
and annealed at 300 °C/400 °C/500 °C for 4 h in air.
Fig. 8. The measurement system of sensors’ characteristics and gas
installation.
chemical composition and physical properties of the deposited
films.
III. R ESULTS AND D ISCUSSION
A. Gas Sensing Characteristics of Si-Doped WO3
It is well known that the operating temperature is the most
important factor that influences the performance of semicon-
ductor gas sensors. The electron concentration of WO3 materi-
als is determined mainly by the concentration of stoichiometric
defects such as oxygen vacancies. The resistance decreases
with increase of the temperature. The gas sensing properties of
the Si-doped WO3 sensors towards acetone gas were analyzed
for working temperatures between 150°C and 425°C in dry as
well as in humidified air. The main goal was to obtain sensor
that can respond to low acetone concentrations. Such sensors
are still required for many applications, including exhaled
breath analysis. The commercially available acetone sensors
have limit of detection at level of 50 ppm (Figaro TGS822,
TGS823, Scimarec AF63) which is too high for exhaled breath
applications. A main interfering compound always present in
the exhaled breath is humidity (80-90%). Due to this fact, the
sensors were measured at various RH concentrations (Fig.13).
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1009
Fig. 9. Response of Si-doped WO3 sensors to 0.32 ppm acetone measured
at different temperatures and for 50% RH.
Fig. 10. Multi-test of Si-doped WO3 sensors to acetone gas (0.32 ppm) at
operating temperature of 425 °C.
As it can be seen, the sensor response is higher when RH is
lower, which is a ‘classic’ issue for semiconductor gas sensors.
The authors did some measurements for other interfering gases
that may be present in exhaled breath, i.e. ethyl alcohol.
In both cases a significant response was observed.
Fig.9 shows the response of Si-doped WO3 sensors to
0.32 ppm acetone (RH 50%) measured at different tempera-
tures. The 0.32 ppm acetone concentration is the lowest value
of acetone detected for healthy people. Therefore, it is crucial
to develop sensors with such a limit of detection. To ensure
the reliability of the testing data, each sensor sample was
tested at least five times at every operating temperature. The
obtained results showed no difference in sensor responses. The
highest response to acetone (RH 50%) was observed for
the sensor deposited and annealed at 300°C (Si - 1.0 at.%).
The sensor response reached approx. 15.8 towards 0.32 ppm
acetone (Fig.10), and the response/recovery time was about
60 s and 150 s, respectively. The recovery time increased as
the concentration increased.
 1010 IEEE SENSORS JOURNAL, VOL. 16, NO. 4, FEBRUARY 15, 2016

Fig. 11. Response of the Si-doped WO3 sensor deposited and annealed Fig. 13. Response of the Si-doped WO3 sensor (deposited and annealed
at 300 °C to 0.32 ppm acetone measured at different relative humidity. at 300 °C) to various concentration of acetone measured at 425 °C.

TABLE I
S UMMARY OF S ENSITIVITY TO VARIOUS A CETONE C ONCENTRATIONS
OF WO 3 S ENSORS (O BTAINED W ITH D IFFERENT M ETHODS )
R EPORTED IN L ITERATURE

Fig. 12. Resistance changes of the Si-doped WO3 sensor (deposited and
annealed at 300 °C) to different concentration of acetone, measured at 425 °C.

Fig. 11 shows the gas sensor’s responses for different

acetone concentration at various relative humidity concentra-
tions. The response S of Si-doped WO3 is approximately 10
even at the relative humidity of 80%, which indicates that
it is relatively stable at humid atmosphere. The presented
sensor will be placed in the sensor chamber as a part of
microsystem [37] for exhaled breath analysis in conjunction
with micropreconcentrator, which provide excellent selectivity
by adsorbing selected compounds in exhaled breath. Recently,
the authors have reported investigation results with utilization
of micropreconcentrators [38], [39] for acetone detection as
well as for analysis of diabetes biomarkers [40]–[42].
Fig.12. shows the responses of the Si-doped WO3 sensor
(deposited and annealed at 300 °C) to different acetone con-
centration from 0.16 ppm to 0.64 ppm measured at 425 °C. Therefore, it is crucial to detect acetone in a wide range of
The sensor response gradually increases with the increase concentration (Fig.13).
of the concentration of acetone. As already mentioned, The sensitivity to various acetone concentrations of
the acetone concentration is usually below 1 ppm for WO3 sensors reported in the literature, obtained with different
healthy people, and above 2 ppm for people with diabetes. methods are summarized in Table 1. It can be noticed that

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 RYDOSZ et al.: PERFORMANCE OF Si-DOPED WO3 THIN FILMS FOR ACETONE SENSING
almost all of the works reported in literature are based on the
nanostructures, i.e. nanoplates, nanoparticles, etc.
IV. C ONCLUSION
The gas sensing characteristics of Si-doped WO3 films
deposited and annealed at various temperatures in the presence
of acetone at various concentrations and for sensor operat-
ing temperatures of 150 – 425 °C were investigated. The
addition of 1.0 at.% Si significantly increased the sensor’s
response compared with the results obtained for the pure
WO3 films reported in the literature. However, doping with
Si slightly increased the response/recovery time, which was
60 s and 150 s, respectively. This issue has to be improved
for commercial applications of portable breath acetone sen-
sors. The sensors demonstrated high sensitivity to acetone
at low concentration (healthy region) as well as at higher
concentration (diabetes region), both in ideal (dry air) and
realistic conditions (80% RH). Further work is necessary to
develop portable acetone sensors for real-time breath analyses
that meet strict requirements regarding precision, accuracy
and robustness and can be used as a supplementary tool for
diabetes monitoring [43].
ACKNOWLEDGMENT
The authors acknowledge Jaroslaw Kanak and
Wieslaw Powroznik from Structural Testing Laboratory
SPM-XRD at Department of Electronics AGH for XRD,
AFM measurements.
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