Sensors and Actuators B 68 Ž2000.

189–196
www.elsevier.nlrlocatersensorb

TiO 2 thin films by a novel sol–gel processing for gas sensor applications
C. Garzella a,) , E. Comini a , E. Tempesti a , C. Frigeri b, G. Sberveglieri a
a
Department of Chemistry and Physics for Engineering and Materials and I.N.F.M., UniÕersity of Brescia, 25100 Brescia, Italy
b
Instituto CNR-MASPEC Parco Area Delle Scienze 37 r A, 43100 Parma, Italy

Abstract

Novel thin films of titanium dioxide dispersed in a polymeric matrix have been prepared by a chemically modified sol–gel technique.
Nanostructured films of pure TiO 2 in the anatase form are obtained after annealing at 5008C. SEM, TEM and TGrDTA are used for the
structure characterisation of TiO 2 films. The role of the polymer in controlling the microstructure is confirmed. The first application of
this technique in gas sensor field is presented in this work. Ethanol and methanol sensing properties are tested and reported. TiO 2 sensors
can detect very well concentration required for breath analysers. q 2000 Elsevier Science S.A. All rights reserved.

Keywords: TiO 2 ; Sol–gel deposition; Thin film; Alcohol sensing

1. Introduction air. By using this method, the TiO 2 deposition has the
same microstructure and crystallographic orientation as
There is widespread interest in TiO 2 thin films for
TiO 2 powders.
applications such as ultraviolet filters for optics and pack-
A further improvement has been recently found by
aging material, antireflection coatings for photovoltaic cells
using a chemically modified alkoxide method, which yields
and passive solar collectors w1x, photocatalysts for purifica-
a characteristic microstructure w5x Ža so-called nanostruc-
tion and treatment of water and air w2x and thin ceramic
ture. of nanosized crystallites and nanosized spaces be-
films or membrane with controlled porosity w3, Chap 14x.
tween the crystallites with excellent photocatalytic activity
Thin, transparent TiO 2 films have been made previously
for the decomposition of aqueous acetic acid w6x.
by various vapour-phase methods including chemical
We would like to report now a novel application of the
vapour deposition, reactive evaporation, electron beam
so-called Achemically modified sol–gel techniqueB in the
evaporation and sputtering w1x. Films made by these pro-
gas sensor field. The possibility to control the porosity of
cesses tend to be crystalline and nonporous.
films is of particular interest for gas sensor application
Alternatively, TiO 2 films derived from alkoxides using
since the number of gas molecules that interact with the
sol–gel process require considerably less equipment, re-
semiconductor surface increases with films surface area.
sulting in generally lower processing costs. A major advan-
The peculiarity of this technique to maintain good surface
tage of sol–gel processes over the vapour-phase methods
properties at high temperatures is also important since the
is the ability to control the microstructure of the deposited
response towards gases usually implies working tempera-
film, i.e. the pore size, pore volume and surface area w3,
tures higher than 4008C.
Chap. 8x. In this regard, an innovative sol–gel processing
The films made by the procedure described in the
has been described for the preparation of ceramic thin
present paper have the following advantages: Ž1. a wide
films as novel materials for integrated humidity sensors
w4x. The prototype sensors were prepared by depositing choice of substrate is available since the films are made in
the absence of any acid or base catalyst Žimpurities., which
metal alkoxide solutions onto Al 2 O 3 substrates with
may be corrosive; Ž2. the film properties do not change
comb-type Au electrodes, by dip-coating and heating in
with time as the TiO 2 precursor is fully hydrolysed and
condensed prior to film formation; Ž3. crack-free films are
)
Corresponding author. Tel.: q39-30-3715769; fax: q39-30-3715788. produced in relative easy terms; and Ž4. film properties can
E-mail address: garzella@bsing.ing.unibs.it ŽC. Garzella.. be controlled by varying the TiO 2rpolymer weight ratio.

0925-4005r00r$ - see front matter q 2000 Elsevier Science S.A. All rights reserved.
PII: S 0 9 2 5 - 4 0 0 5 Ž 0 0 . 0 0 4 2 8 - 7
190 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196
2. Experiments
2.1. Film preparation and coating
2.1.1. Materials
Tetraethyl orto-titanate ŽTEOT. was obtained from
Chempur. Anhydrous ethanol was received from Aldrich.
Hydroxypropylcellulose ŽHPC. was used with an average
molecular weight of 80 kgrmole.
The films were deposited onto 3 = 3 mm2 Ž250 mm
thick. or 10 = 10 mm2 Al 2 O 3 Ž500 mm thick. substrates
for electrical or structural characterisation, respectively.
Silicon substrates were used in order to prepare samples
for TEM analyses. The films dedicated to electrical charac-
terisation were grown onto substrates equipped with a Pt
meander heater on the backside and Pt interdigitated con-
tacts sputtered on the thin-film side. The platinum heater,
acting also as temperature sensor, is necessary to reach the
working temperature of the sensor, which is in general
between 2008C and 6008C for this kind of semiconductor
materials.
2.1.2. Synthesis of TiO2 particles
TiO 2 sol preparation was made using the chemically
modified sol–gel procedure proposed by Nagpal et al. w7x,
which implies hydrolysis and condensation of TEOT in the
presence of HPC dissolved in ethanol. The TEOT and
water concentrations were 0.02 and 2.3 M, respectively;
the addition of HPC led to a final TiO 2rHPC ratio of
48%r52%; under this condition, a full conversion of
TEOT is obtained. The effect of water concentration on the
particle growth has been investigated by Nagpal et al. w8x.
Equal volumes of TEOT in anhydrous ethanol were mixed
with solutions of HPC in ethanol and water. The TEOT
solution was prepared by dripping TEOT in ethanol under
nitrogen. The mixture of the two solutions was stirred for
24 h at ambient temperature and concentrated at 708C.
Another sol was prepared via the classical sol–gel
technique with the same procedure, but without adding
Fig. 1. MicroRaman spectra of the TiO 2 film after annealing at 5008C.
HPC, in order to compare the characteristics of the films
obtained with the two technologies.
2.1.3. Coating
For film formation we used the dip-coating technique.
Alumina supports were dipped and immersed into the
TiO 2 –HPC sol Žor into the TiO 2 sol obtained via the
classical sol–gel technique.. After a few minutes, the
samples were withdrawn upward and vertically relative to
the surface solution with a speed of 0.26 cmrs. The
annealing treatment was optimised as follows. The films
were dried at 1608C for 1 h, heated at a rate of 308rh up to
5008C and held at this temperature for 5 h in air. The final
samples were obtained by repeating film deposition and
heating treatment four times.
2.2. Characterisation
2.2.1. Microstructure
The TiO 2 thin film structural characterisation has been
performed by TEM ŽJEOL 2000FX operated at 200 keV.
and microRaman ŽDilor Labram spectrograph.. SEM ob-
servations have been carried out with a Cambridge 360
microscope with beam energies in the 10–25 keV range
for thin films samples as grown and after annealing. The
removal of the polymeric matrix has been checked by
TGArDTA analysis ŽSeiko Instrument Thermogravimetric
Analyser.. The gas sensors properties of novel films have
been checked by the electrical characterisation reported
below.
2.2.2. Electrical properties
We have tested the gas sensing properties of this mate-
rial towards reducing gases like ethanol and methanol and
oxidising gases like nitrogen dioxide and carbon monox-
ide. The technique used was the flow-trough technique that
was just reported by Sberveglieri et al. w9x elsewhere. A
constant flux of synthetic air of 0.3 lrm was used as gas
carrier and the desired concentrations of pollutants were
 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196 191

obtained by mixing the gas from certified bottles with the electrical properties due to variations of the atmosphere
synthetic air. All the measures were made under controlled have been registered with the Volt Amperometric tech-
humidity ŽRH 30%. and the temperature of the chamber nique, applying a constant potential of 3 V to the sensing
containing the sensors was set at 208C. The changes in the layer and registering with a picoammeter the conductance

Fig. 2. SEM micrographs of films obtained via sol–gel chemically modified Ža. TiO 2 –HPC film as grown and Žb. TiO 2 film annealed at 5008C Žbar: 500
nm..
192 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196

variation as a function of time. Either the gas flow or the
electrical parameters were controlled by a PC, which also
registered the conductance change of the sensors.
3. Results and discussion
3.1. Microstructure
3.1.1. Structural characterisation
The microstructure and the crystal phase of the an-
nealed samples have been investigated by TEM analyses,
selected area diffraction ŽSAD. and microdiffraction pat-
terns of single crystallites. The deposited layer appears
nanostructured with particle sizes between 3 and 30 nm.
The crystal phase has been identified as TiO 2 anatase, as
confirmed by microRaman analysis. The TEM micrograph
with more details have been reported by the authors else-
where w10x.
A complete scanning of the films surface was per-
formed by microRaman analysis. The microRaman spec-
trum ŽFig. 1. was obtained by subtraction of alumina
absorption and presents an intense band at 144 cmy1 and
three less intense bands at 400, 515 and 640 cmy1 , which
are characteristic of the anatase form w11x.
3.1.2. SEM analysis
Fig. 2a and b reports two scanning secondary electrons
images of TiO 2 –HPC films as grown and after annealing
at 5008C, respectively. The polymer-oxide composite ap-

Fig. 3. SEM micrographs of TiO 2 thin film obtained by classical sol–gel technique and annealed at 5008C Žbars: Ža. 5 mm and Žb. 500 nm..
 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196
pears uniform and nanostructured; the presence of poly-
meric matrix intertwined between oxide particles is evi-
dent. It is interesting to observe that during the annealing,
the particles do not coalesce, maintaining the nanostructure
until 5008C. Polymer is absent after annealing as con-
firmed by TGArDTA analysis as reported hereafter.
Fig. 3 shows two scanning electron micrographs of the
films prepared with the classical sol–gel technique Žwithout
polymer. and annealed at 5008C. The surface presents
large particles and macroscopic cracks.
We can conclude that the polymer plays an essential
role during the thin films growth: it acts as in situ steric
stabiliser preventing particle sintering and film cracking
during the annealing treatment.
3.1.3. Thermal analysis
The necessary amount of TiO 2 –HPC composite was
prepared depositing the sol on a large Petri dish; after the
solvent evaporation, 20 g of fine powder are obtained upon
removing the film from the glass.
The decomposition of organic matrix has been checked
using the differential thermal analysis ŽDTA. and thermo-
gravimetry ŽTG. ŽFig. 4.. After the solvent loss, the poly-
mer quantitatively decomposes between 3008C and 5008C,
over which the stability of the oxide is confirmed. The
calculated weight ratio TiO 2rHPC Ž48.8%r51.1%. agrees
with the theoretical ratio Ž48%r52%..
3.2. Electrical measurements
Gas measurements were made under constant tempera-
ture conditions and the gas concentrations were varied for
ethanol and methanol in the range 100–600 ppm at 30%
RH. Other possible interfering gases were examined to
complete these gas measurements, such as nitrogen dioxide
and carbon monoxide. The working temperature was var-
ied in the range between 4008C and 5008C since during
Fig. 4. TGArDTA analyses of TiO 2 thin film as grown obtained with
chemically modified sol–gel technique.
193
Fig. 5. Dynamic variation of the current flowing through the TiO 2 thin
film when 100 ppm of ethanol are introduced in the test chamber at two
different working temperatures Ži.e. 4008C and 5008C. at 30% RH.
preliminary measurements no appreciable response was
registered below 3508C.
3.2.1. Gas response to ethanol and methanol
Fig. 5 shows the kinetic variation of the current flowing
through the TiO 2 thin film when 100 ppm of ethanol is
introduced in the test chamber at two different working
temperatures Ži.e. 4008C and 5008C. at 30% RH. The
relative change in the conductance when ethanol is intro-
duced in the chamber is very high in both tests, even more
than 2000% Ž2110%, 3666%.. As the temperature in-
creases, the current in the film increases as well as the
signal to noise ratio. The measurements highlight that
these thin films are stable and that the recovery of the
signal is complete when the air flux is restored after the
gas test.
Fig. 6 reports the dynamic response as methanol is
introduced at 4008C and 5008C. The responses are about
700% and 1700%, respectively.
The cited values are considerably high for both alcohols
compared to those found for TiO 2 obtained by classical
Fig. 6. Dynamic variation of the current flowing through the TiO 2 thin
film when 100 ppm of methanol are introduced in the test chamber at two
different working temperatures Ži.e. 4008C and 5008C. at 30% RH.
194 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196
sol–gel method and doped with Nb and Pt w12x. Consider-
ing e.g. the responses in the presence of 500 ppm of
ethanol at 4008C, the values obtained for the TiO 2 films
prepared with the sol–gel chemically modified technique
ŽFig. 7. are six times higher than the values obtained with
doped TiO 2 film Ž140 vs. 22.3.. The more pronounced
sensing properties can be related to the morphological
characteristics of the films. Doped TiO 2 is characterised
by a reduced grain size relative to the pure oxide w12x, but
using the new sol–gel technique, the nanostructure is finer
and even smaller Žparticles size 3–30 vs. 25–50 nm.. This
implies higher surface area to volume ratio and, as a
consequence, a greater surface activity results. The re-
sponses toward ethanol and methanol are also better than
those found for the SnO 2 films reported in the literature
w13x.
3.2.2. Response time
The dynamic of these sensors is very fast as it can be
noticed. The response and recovery times are defined as
the times the conductance takes to reach 90% of Ž R f –R 0 .
when the gas is introduced and to recover 30% of Ž R f –R 0 .
when the flux of air is restored. The response and recovery
times for ethanol are about 2 and 1 min, respectively, for
all the temperatures tested. For methanol, the response
time is half a minute and the recovery time is less than 1
min. The sensor response and recovery times are short
enough for possible gas sensing application like control
food analyses, wine identifications, electronic noses and
breath analysers. The kinetic behaviour of the response is
quite the same for both alcohols; for methanol, the rise
time is shorter simply because the change in the conduc-
tance is lower.
3.2.3. Modelling
Considerations on the sensitivity of this thin film to-
wards ethanol and methanol can be made by plotting the
Fig. 7. Response as a function of ethanol and methanol concentration of
the TiO 2 sensors at two different working temperatures.
Table 1
A and B coefficients for the sensors for the two kind of alcohols, resulted
from the fits with a power low Ž DGr Gs Awgasx B , where concentration
of gas is expressed in ppm.
Gas T Ž8C. A B
Ethanol 400 0.12 1.14
500 1.74 0.66
Methanol 400 0.05 1.12
500 0.84 0.67
response, defined as relative change in the conductance, as
a function of the concentration, as in Fig. 7. For the target
gases the results obtained at two working temperatures are
reported in the plot. This dependence follows the well-
known power behaviour DGrG s Awgasx B for the two kind
of alcohols. Four different fits, with this kind of power
expression, were made and the values for the fitting pa-
rameters are reported in Table 1. The slope of the lines in
the logarithmic scale is the same for both ethanol and
methanol, but there are differences regarding the two
working temperatures. As the temperature is increased, the
dependence of the response with the concentrations be-
comes less pronounced. A higher value of the exponent B
allows an easier distinction between two concentrations of
gas, while a lower value rises the lower detectable concen-
tration. In this case, if we are interested in the determina-
tion of the concentrations value in the range of 500 ppm,
we could work at 4008C, since the slope is higher. Other-
wise, if we are interested in lower concentrations, we can
work at 5008C since in this case the detection limit is
lower than 1 ppm. As we have already noticed, the re-
sponse to ethanol is higher than methanol.
3.2.4. Detection limit
A breath analyser must detect at least 200 ppm ethanol
that corresponds approximately to 0.6 g alcoholrl in the
blood. Our sensors can detect very well lower levels Žwith
a response toward 100 ppm more than 2000%.. The detec-
tion limit that could be reached with these sensors for
ethanol are 3 and 0.1 ppm at 4008C and 5008C, respec-
tively, if a relative variation in the conductance of 40% is
considered respectable. For methanol, the detection limits
are higher, 6 and 0.3 ppm for the two working tempera-
tures.
3.2.5. Comparison with TiO2 deposited with standard
sol–gel technique
Finally, in order to complete this study of the gas
sensing properties of TiO 2 grown with this sol–gel modi-
fied technique, we have compared the TiO 2 deposited
performances with those of standard sol–gel procedures.
The enhancement in the response, indicated with the
ratio Ž Q s SrS w . of the response of the sensor deposited
with the new technique Ž S . relative to the standard sol–gel
Ž S w ., is always higher than 1000%. The differences be-
 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196
Fig. 8. Ratio Ž Qs SrS w . of the response of the sensor deposited with
the new technique and the standard sol–gel as a function of the concen-
tration of ethanol and methanol at a working temperature of 4008C and
5008C, and 30% RH.
tween the two layers become more pronounced as the
temperature increases; at the working temperature of 5008C
the ratio Q rises, increasing the alcohol concentration. The
highest value is reached for 600 ppm of ethanol at 5008C,
as reported in Fig. 8.
It has been highlighted that the morphological charac-
teristics of the TiO 2 can be related to the more pronounced
sensing properties.
3.2.6. Cross sensitiÕity
The influence on the response amplitude of relative
humidity of the environment atmosphere has been tested
for the target gases. Fig. 9 plots the different responses to
300 ppm of ethanol at 5008C and at two different values of
RH Ž30% and 50%.. The response in the two ambient
varies about 15%, which is less than 100 times the varia-
tion due to the presence of 100 ppm of ethanol.
In Fig. 10, the response Ž DGrG for reducing gases and
D RrR for oxidising gases. is reported for two other kind
Fig. 9. Kinetic variation of the current flowing through the TiO 2 thin film
when 300 ppm of ethanol are introduced in the test chamber at two
different values of RH at 5008C.
195
Fig. 10. Response as a function of CO and NO 2 concentration of the
TiO 2 sensors at 4008C.
of gases as the NO 2 and CO in the concentrations ranges
from 0.5–4 to 100–300 ppm, respectively, at a working
temperature of 4008C. The response to these possible
interfering gases, in high concentration with respect to the
alarm level for indoor and outdoor conditions, is more than
one order of magnitude lower than the response to the
alcohols. This sol–gel deposited material is well suited for
the alcohol presence detection.
4. Conclusions
Thin composite films of TiO 2 and polymer HPC have
been made via the chemically modified sol–gel technique
by dip-coating onto alumina substrates. Sintering the sam-
ples at 5008C in air results in the complete burnout of the
HPC and the formation of an anatase film. The deposited
layers are uniform and present a characteristic nanostruc-
ture with particles size between 3 and 30 nm. Films made
in the same condition via the classical sol–gel procedure
imply a cracked surface and larger particle size.
The new role of polymer in the sol–gel process for
TiO 2 thin film growth has been confirmed: it acts as in situ
steric stabiliser preventing particle sintering and film
cracking during the annealing treatment.
The temperature stable nanostructured TiO 2 films pre-
sent interesting surface properties for gas sensors applica-
tions. The TiO 2 thin films deposited via the chemically
modified sol–gel technique show a response towards alco-
hols that is always enhanced Žfrom 10 to 60 times. relative
to the film grown via the classical sol–gel technique.
The TiO 2 layers show a better surface interaction with
gas molecules; this behaviour can be tentatively ratio-
nalised assuming that nanosized particles imply higher
surface areas and porosity. The response and recovery
times for ethanol are particularly interesting for possible
applications such as control food analyses, wine identifica-
tions, electronic noses and medical devices. As noticed, the
response is very high at concentrations well below the
limit imposed for breath analysers and the responses to-
196 C. Garzella et al.r Sensors and Actuators B 68 (2000) 189–196
ward possible interfering gases are always two order of
magnitude lower than the responses of alcohols.
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Biographies
Carlotta Garzella was born on June 14, 1972. She received a graduate
degree in chemistry at the University of Milan in 1997. She is now a PhD
student in Materials Science at the University of Brescia and is working
on chemical sensors with particular interest on the sol–gel technology for
oxide thin film deposition and the chemico–physical characterisation of
the oxide surfaces.
Elisabetta Comini was born in 1972. She received a graduate degree in
physics at the University of Pisa in 1996. She is presently working on
chemical sensors with particular reference to deposition of thin films by
PVD technique and electrical characterisation of MOS thin films. She is
now finishing the PhD in material science at the University of Brescia.
Ezio Tempesti was born on the 26th of October 1943. He obtained his
degree in 1968 at the Pavia University. At the Politecnico di Milano, he
was an assistant from 1968 to 1969 then he became Assistant Professor
until 1982 and Associated Professor from 1982 to 1986. Full Professor at
the University of L’Aquila until 1990, he left for the University of
Brescia where he is now the Director of the Department of Chemistry and
Physics for Engineering and Materials. He has been involved in several
research projects, e.g. with S.N.I.A., Montedison, SNAM Progetti, I.C.I.,
Euratom, Elf Atochem, etc. He has been project leader of the Italian
Ministry of Scientific Research, C.N.R., E.N.E.A. and European Commu-
nity. He is a member of Assne. Italiana di Ingegneria Chimica, Fedn.
Europeenne du Genie Chimique, N.Y. Academy of Sciences.
Cesare Frigeri has obtained his degree in solid state physics at the
University of Bologna. For 8 years he was a Research Scientist in Agip
Nucleare where he performed researches in the field of sintering of
ceramic materials and the relationship between mechanical properties and
crystalline textures in metal alloys. In 1982 he joined the CNR-MASPEC
Institute in Parma where he is a Senior Scientist. Since then, his activity
has dealt with the study of extended defects by electron microscopy, their
interaction with point defects and their correlation with growth parame-
ters in both bulk and epitaxial III–V compound semiconductors, as well
as with the development of SEM and TEM methods for defect analysis in
such compounds. He is the author of 85 publications in international
journals and proceedings with international refereeing committee. He has
given six invited talks in international conferences and is member of the
scientific or steering committee of two international conferences.
Giorgio SberÕeglieri was born on July 17, 1947 and received his degree
in physics from the University of Parma in 1971 with his research
activities on the preparation of semiconducting thin film solar cells. He
has been appointed Associate Professor at the University of Brescia in
1987. In the following year, he established the Thin Film Laboratory,
afterwards called Gas Sensor Lab., mainly devoted to the preparation and
characterisation of thin film chemical sensors; he has been the Director of
the GSL since 1988. In 1994, he was appointed Full Professor in Physics,
formerly at the Faculty of Engineering of the University of Ferrara and
then in 1996 at the Faculty of Engineering of the University of Brescia.
He is referee of the journals AThin Solid FilmsB, ASensors and ActuatorsB
ASensors and MaterialsB and other journals and member of Scientific
Committee of Conferences on Sensor and Materials Science. During his
25 years of scientific activities, Giorgio Sberveglieri published more than
140 papers on international reviews; he presented more than 50 oral
communications to international congresses and numerous oral communi-
cations to national congresses.