Sensors and Actuators B 126 (2007) 181–186

High throughput screening of the propylene and ethanol sensing

properties of rare-earth orthoferrites and orthochromites
Maike Siemons, Ulrich Simon ∗
Institute of Inorganic Chemistry, RWTH Aachen University, Landoltweg 1, 52056 Aachen, Germany
Available online 18 December 2006

Abstract
Perovskite-type LnMO3 (Ln = La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu; M = Cr, Fe) oxides were prepared by the polyol mediated
synthesis. Thick films of the prepared materials were electrically characterised using high throughput impedance spectroscopy (HT-IS). All samples
showed p-type semiconductivity. Ethanol and propylene were used to test the gas sensing behaviour in a temperature range from 200 to 500 ◦ C. A
correlation between the (Ln–O) binding energy and the sensing properties is observed.
© 2006 Elsevier B.V. All rights reserved.

Keywords: LnFeO3 ; LnCrO3 ; Polyol method; High throughput impedance spectroscopy; Gas sensor

1. Introduction evolutionary optimising of selected material properties. Most

Gas monitoring represents a growing demand resulting from
strategies for intelligent process management, environmental
protection and medical diagnostics as well as from the domestic
and automobile sector. The four key parameters identifying a
good sensor are sensitivity, selectivity, stability and response
time [1]. However, the majority of the research activities on
the development of fast responding, sensitive and especially
highly selective gas sensor materials is often restricted to
modification and improvement of known systems and only
rarely being directed towards the search for alternative sensor
materials. Therefore, nowadays commercial gas sensors are
either based on few n-type conducting semiconductor materials,
like, e.g. SnO2 , ZnO, WO3 , Fe2 O3 or TiO2 , or, for more
demanding applications, are based on sensor arrays of these
materials enhancing selectivity with appropriate complex signal
analysis.
The use of high throughput experimentation (HTE) tech-
niques accelerates material synthesis and characterisation,
enabling to investigate a multiplicity of materials compared to
‘one at a time’ strategy [2,3]. Besides, HTE allows the appli-
cation of combinatorial strategies, which typically are based on
∗ Corresponding author. Tel.: +49 241 80 94644; fax: +49 241 80 99003.
E-mail address: ulrich.simon@ac.rwth-aachen.de (U. Simon).
recently we have reported on the development of a high through-
put impedance spectroscopy (HT-IS) setup for the analysis of
the gas sensing properties of metal oxides together with a broad
variety of different surface doping elements [4,5]. By means of
selected examples we have demonstrated how materials with
desired properties can be found in a huge variety of different
combinations of metal oxides and surface doping.
In this work we report on the gas sensing properties of 25
nanoscaled p-type semiconducting LnMO3 metal oxides with
(Ln = La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu;
M = Cr, Fe) using an HTE methodology. The rare-earth per-
ovskites (LnMO3 ) containing transition metal ions (M) show
a wide range of electrical properties. They show good thermal
stability and have been tested, for example, as catalysts [6,7],
photocatalysts [8], electrodes of fuel cells [9,10] and magneto-
optics [11,12]. Some of them have been proposed as gas sensing
materials for CO [13], NO2 [14,15] and hydrocarbons [16–20].
We report about measurements on the sensitivity and
response times in a temperature range from 200 to 500 ◦ C
towards ethanol and propylene. In continuation of our earlier
studies [21] on LnMO3 we took into account the sensitivity
towards ethanol, which is a test gas of high interest in differ-
ent field of application. In order to verify the model proposed
for structure–property-relations we analysed the dependence
between the (M–O) binding energy and the sensitivity of the
materials towards ethanol.

0925-4005/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2006.11.022
182 M. Siemons, U. Simon / Sensors and Actuators B 126 (2007) 181–186

Table 1
Summary of materials prepared (DS stands for Debye–Scherrer)
Ln-precursor Compound DS (nm) SEM (nm)a Compound DS (nm) SEM (nm)a

La(NO3 )3 ·6H2 O; 99% Fluka LaFeO3 74 30–80 LaCrO3 84 70–90

Pr(NO3 )3 ·6H2 O; 99.9% Aldrich PrFeO3 42 40–100 PrCrO3 87 80–100
Nd(CH3 COO)3 ·nH2 O; 99% Alfa Aeser NdFeO3 55 50–70 – – –
Sm(NO3 )3 ·6H2 O; 99.9% Acros SmFeO3 55 30–60 SmCrO3 131 Highly agglomerated
Eu2 (CO3 )3 ·nH2 O; 99.9% Alfa Aeser EuFeO3 62 50–80 EuCrO3 108 60–100
Gd(CH3 COO)3 ·nH2 O; 99.9% Alfa Aeser GdFeO3 55 50–80 GdCrO3 101 60–80
Tb(NO3 )3 ·6H2 O; 99.9% Acros TbFeO3 70 40–80 TbCrO3 148 80–100
Dy(NO3 )3 ·5H2 O; 99.9% Alfa Aeser DyFeO3 71 30–70 DyCrO3 94 50–100
Ho(NO3 )3 ·5H2 O; 99.9% Alfa Aeser HoFeO3 56 Highly agglomerated HoCrO3 132 Highly agglomerated
Er2 (CO3 )3 ·nH2 O; 99.9% Alfa Aeser ErFeO3 57 Highly agglomerated ErCrO3 82 70–90
Tm(CH3 COO)3 ·nH2 O; 99.9% Alfa Aeser TmFeO3 91 40–100 TmCrO3 109 50–70
Yb(NO3 )3 ·5H2 O; 99.9% Strem YbFeO3 56 30–60 YbCrO3 77 60–80
Lu(CH3 COO)3 ·nH2 O; 99.9% Alfa Aeser LuFeO3 120 Highly agglomerated LuCrO3 114 Highly agglomerated
a Size of visible spherical primary particles.

2. Experimental needed to be optimised with respect to particle size, yield and

2.1. Material preparation and characterisation
For the preparation of the perovskite compounds, which is
described in detail elsewhere [21], stoichiometric amounts of
Fe(NO3 )3 ·9H2 O (Merck, p.a.) or Cr(NO3 )3 ·9H2 O (Alfa Aeser,
96%) and a suitable lanthanoid precursor (see Table 1) were dis-
persed in diethylene glycol (DEG, Merck, 99.99%). The mixture
was heated up to T1 (80–140 ◦ C) under vigorous stirring until
a clear solution was obtained. If necessary, a sufficient surplus
of hydrolysis agent was added. The emerging suspension was
heated for 5 h up to T2 (160–190 ◦ C) and then cooled to room
temperature. The preparation resulted in a stable suspension
with a standard concentration in all experiments of typically
1 wt% (solid to DEG). For further characterisation the solid
material was separated from the suspension via centrifugation
and washing with acetone. These “as synthesised” samples were
dried at 60 ◦ C. To obtain crystalline materials the suspensions
were dried at 400 ◦ C (1 h) and then annealed at T3 (700–900 ◦ C)
for 2–12 h. For each individual synthesis, reaction parameters
purity.
The initial characterisation of the products was carried out
by powder XRD measurements (Cu K␣, λ = 1.54059 Å) on thin
films with a Huber Image Plate in transmission. Powder diffrac-
tion patterns were analysed using Stoe WinXPow 1.06 Software
(Stoe & CIE GmbH). Powder morphology was examined by
SEM analysis using a Zeiss DSM 982 Gemini and a LEO Supra
35 VP. For that purpose, all samples were sputtered with car-
bon. Table 1 summarises the composition as well as the mean
particle size (diameter) obtained from SEM measurements and
the mean crystallite size obtained from XRD measurements
(Debye–Scherrer equation [22]).
2.2. Thick film preparation and high throughput setup
The prepared materials are well suited for thick layer prepa-
ration on interdigital electrode structures. These electrode sub-
strates consist of an Al2 O3 -plate (side length of 105 mm) with
64 interdigital capacitors (IDC) made of platinum. The platinum
IDC has a structure width of 110 ␮m and each well has a diame-

Fig. 1. Left: Scheme of the HT-IS setup. For reasons of clearness only two measuring lines are displayed. Right: Layout of the multielectrode array with photograph
of an already deposited sample plate (adapted from Ref. [23]).
 M. Siemons, U. Simon / Sensors and Actuators B 126 (2007) 181–186
ter of 5 mm (as shown in Fig. 1 on the right hand side) [4,23]. The
array allows automated pipetting robot assisted sample prepa-
ration and coating, respectively. Time consuming process steps
like thermal annealing or sample conditioning can be proceeded
in parallel. For the thick film deposition on these electrodes,
the powder materials were dispersed by mixing in a mortar with
an aqueous polyethylene imine (0.5 wt%) solution. The resulting
suspensions had a concentration of 0.08 mol/L. The suspensions
were deposited into wells formed by a Teflon mask on top of
the microelectrode substrates by use of an Eppendorf pipette or
a laboratory roboting system (Lissy, Zinsser Analytic GmbH).
Each well had an O-ring for sealing against the substrate. The
substrate was first dried for 48 h at room temperature in air. After
that it was held for 6 h at 700 ◦ C in air to remove the organic
residues. To compensate possible gradients in gas concentration
and temperature as well as single failures due to contact defects
over the substrate two to three statistically selected positions
were equipped with the same material composition. Sample
plates (coated arrays) were inserted into the measuring head.
Fig. 1 (left) shows the scheme of the HT-IS setup. The leads to
each IDC are electrically connected via Al2 O3 covered platinum
wires in the measuring head. Constant contact pressure is assured
using spring loaded contact tips which connect the IDCs via high
frequency capable relay matrices (multiplexers) to the measur-
ing instruments. A set of gas flow controllers is used to compose
the different test gases. In addition, the test gases can be humidi-
fied by bubbling the carrier gas through a water reservoir at room
temperature. The test gases are led to a quartz glass bell covering
all sample positions on a plate. For further technical details see
Ref. [5].
2.3. Electrical characterisation
Electrical measurements were performed using an impedance
analyser (Agilent 4192 A) in a frequency range from 10 to
106 Hz (15 measuring points per frequency decade) and an
amplitude of 100 mV (rms). The measurements were taken out
in a temperature range between 500 and 200 ◦ C in 25◦ -steps.
Reference measurements were performed in humid synthetic
air (air), which was also used as carrier gas for ethanol and
propylene. For the gas sensing experiments, the test gases were
mixed with synthetic air to reach a consistent volume flow of
each 100 sccm. Conditioning of the materials was carried out
at 500 ◦ C for 240 min under air and at the following temper-
atures for 90 min. The measuring sequence was air, ethanol
(40 ppm), air, propylene (25 ppm), air. The intermediate mea-
surements in air insure the recovery of the resistance, before
the next test gas is applied. Relative humidity of the gases was
45% at room temperature in order to perform the measure-
ments in a typical humidity range representative for ambient
conditions. For sample conditioning a preliminary gas flow was
applied over 30 min to reach equilibrium. All data achieved are
stored in a database, which has been developed for data mining
and for comparison with complementary measuring methods
[24].
In order to measure the response time of the individual
samples, measurements at fixed frequency (100 Hz) were
183
performed. One hundred Hertz have been chosen to stay in any
case in the quasi-dc plateau, i.e. the frequency independent part
at low frequencies of the impedance spectra. While each mea-
surement took 1.5 s, the time interval between the measurements
was 4 s.
3. Results and discussion
3.1. Characterisation of the gas sensing properties of
LnMO3
Fig. 2 shows the plot of real part of the complex impedance
versus the imaginary part (Argand plot) representative for
TbFeO3 in synthetic air, propylene and ethanol at 300 ◦ C. Auto-
mated data fitting allows describing the impedance spectra with
the impedance function of a circuit equivalent, consisting of a
resistor and a capacitor in parallel (see Fig. 2). Further informa-
tion is given in Ref. [25]. The use of fit functions reduces the
complex impedance function describing the electrical properties
of each material to one value for the resistance R and the capac-
itance C, respectively. While the capacitance can be assigned to
the geometric capacitance of the IDC, the resistance values under
the respective measuring conditions are taken for the determi-
nation of the material sensitivity. The absolute sensitivity S of a
material to a test gas is defined by:
⎧ 
⎪ Rgas 
⎪
⎪
⎨ Rair R >R
S=  gas air
⎪
⎪ R 
⎩ R 
air
⎪
gas Rair >Rgas
where Rgas is the resistance obtained from the fit under test gas,
while Rair is the reference resistance value for a measurement
under synthetic air.
Fig. 2. Argand plot and circuit equivalent exemplarily for TbFeO3 (T = 300 ◦ C).
p-Type semiconductors show an increase of resistance compared to synthetic
air, when reducing gases are applied.
184 M. Siemons, U. Simon / Sensors and Actuators B 126 (2007) 181–186

Fig. 3. Temperature dependence of the sensitivity of LnFeO3 .

We describe the response of a material to a test gas by the est sensitivity towards the used hydrocarbons. Measurements for
relative sensitivity S , which is defined as YbFeO3 could only be evaluated above 300 ◦ C. At lower tem-
⎧  perature the resistance of the material exceeds the measurement
⎪ Rgas − Rair 
⎪
⎪− 
limits (R > 20 M). The highest overall sensitivities for all tem-
⎨ Rgas R >R peratures below 450 ◦ C can be found for SmFeO3 , TmFeO3 and
S =  gas air
⎪
⎪ R − R  LuFeO3 .
⎪
⎩+
air gas 
R  Fig. 4 shows the temperature dependence of the sensitivity
air Rair >Rgas
for the LnCrO3 materials. In comparison to LnFeO3 , LnCrO3 in
where values for S range from 1 to −1. Decrease of resistance general shows smaller sensitivities towards hydrocarbons. The
while applying a test gas gives values between 0 and 1, rise of temperature of maximum sensitivity is shifted to lower values.
resistance results correspondingly in values between −1 and 0. LaCrO3 shows the smallest sensitivity towards the applied gases,
Using S instead of the commonly used absolute sensitivity S whereas DyCrO3 appears to be the material with the highest
including algebraic signs turned out to be beneficial for the data sensitivities towards both test gases.
mining process in our high throughput workflow [24]. Further- In both material groups the sensitivity towards ethanol is
more, it allows an immediate differentiation between oxidising much more pronounced than towards propylene. This is presum-
and reducing test gases, respectively. ably caused by the functional OH-group of ethanol, as expected
Fig. 3 shows the temperature behaviour of the sensitivity of from Ref. [26].
the different LnFeO3 materials indicating that the operating tem- For further evaluation we took into account the strength of the
perature affects the properties of all materials. LaFeO3 , which is M–O bond in the metal oxide. The bond strength of the oxygen
the material with the largest lanthanoid radius, shows the small- at the surface near sites is an important factor for the sensing

Fig. 4. Temperature dependence of the sensitivity of LnCrO3 .

 M. Siemons, U. Simon / Sensors and Actuators B 126 (2007) 181–186 185

Fig. 5. Sensitivity S vs. binding energy Ln–O according to Ref. [27] at 300 ◦ C
(without LuFeO3 ). Solid lines are no fit data; they should only serve as a guide
for the eye.

Fig. 7. Response behaviour of TmFeO3 towards ethanol (40 ppm). T = 325 ◦ C,

properties which has already been proposed by Arakawa et al.
for methanol sensing activity of different rare-earth perovskites
[27]. Therefore, we show in Fig. 5 a correlation between the
binding energy of oxygen and lanthanoid ion versus the sensi-
tivity towards propylene and ethanol, respectively. The binding
energy H(M–O) is calculated by:
1  n 
H(M–O) = Hf − H s m − D O
CNm 2 values of ethanol sensitivities of LnFeO3 and LnCrO3 oxides at
where Hf is the formation energy of one mole of oxide Mm On , Hs
the sublimation energy of the metal, DO the dissociation energy
of O2 and CN is the coordination number of metal ions. As a
f = 100 Hz, t = 30 min.
result we can show that also in the case of ethanol the sensitiv-
ity is correlated to the binding energy. The higher the absolute
value of the binding energy, the smaller the sensitivity towards
the gases. Only LuFeO3 shows higher sensitivities than it was
expected from this model. In addition, Fig. 6 shows the absolute
the temperature of highest sensitivity versus the (Ln–O) binding
energy. For LnCrO3 the correlation between the (Ln–O) binding
energy and the sensitivity is obvious. However, the sensitivity
of the orthoferrites is in all cases higher than of the LnCrO3
oxides. This difference in sensitivities presumably results from
the difference in the binding energy H(Cr–O) and H(Fe–O)
[21].

3.2. Response times of LnFeO3

In this section we exemplarily show the response and recov-

ery time of TmFeO3 . The response and recovery times are
important parameters for tailoring sensors for desired applica-
tions. The response time upon 40 ppm ethanol is about 20 s at
325 ◦ C (see Fig. 7). The recovery time is slightly bigger, i.e. 44 s.
On and off cycles under ethanol could be repeated several times
without observing major changes in the response. The response
times of all LnFeO3 materials are given in Table 2 for T = 350 ◦ C
and 60 ppm ethanol.

Table 2
Response times (τ 50 /s) of LnFeO3 towards 60 ppm of ethanol at 350 ◦ C
Ln
Fig. 6. Ethanol sensitivity of LnFeO3 (300 ◦ C = TSMax ) and LnCrO3 La Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
(225 ◦ C = TSMax ) vs. binding energy Ln–O according to Ref. [27]. Solid lines 17 <15 <15 24 26 20 25 19 <15 <15 <15 <15 <15
are no fit data; they should only serve as a guide for the eye.
186 M. Siemons, U. Simon / Sensors and Actuators B 126 (2007) 181–186
4. Conclusions
Nanoparticles of LnMO3 (Ln = La, Pr, Nd, Sm, Eu, Gd,
Tb, Dy, Ho, Er, Tm, Yb, Lu; M = Cr, Fe) have been pre-
pared via polyol-mediated synthesis. All materials are sensitive
towards propylene and ethanol, while the absolute sensitivity
towards ethanol is much higher than towards propylene. The
orthochromites showed lower sensitivity than the LnFeO3 per-
ovskites. LaFeO3 and LaCrO3 presented the smallest sensitivity
of their group towards ethanol, while DyCrO3 was the best sens-
ing material in the LnCrO3 group. The sensitivity of the materials
could be correlated to the Ln–O binding energy and it was shown
that the higher the absolute value of the binding energy, the
smaller the sensitivity towards various gases. The binding energy
of (Cr–O) is higher than that of (Fe–O) which might explain that
the change of the M ion from Fe to Cr depresses the sensitivity
of LnMO3 .
Acknowledgements
This work was financially supported by BMBF under con-
tract No. 03 C 0305 A. M.S. gratefully acknowledges generous
support by the Studienstiftung des Deutschen Volkes. We thank
T.J. Koplin and Dr. D. Sanders for helpful discussions.
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Biographies
Maike Siemons received her degree in chemistry at the RWTH Aachen Uni-
versity in 2003. She is currently a PhD student at the Institute of Inorganic
Chemistry. Her research interests are focussed on the preparation and charac-
terization of nanocrystalline metal oxides which are suitable as chemical sensor
materials.
Ulrich Simon holds the Chair of Inorganic Chemistry and Electrochemistry
at the RWTH Aachen University since May 2000. The main interest of his
current research includes the synthesis and the electrical properties of metal
and semiconducting nanoparticles and of nanoporous materials, as well as their
application in molecular electronics and chemical sensing.