Sensors and Actuators B 115 (2006) 198–204

Composite of TiO2 nanowires and Nafion as humidity sensor material

Ren-Jang Wu a,∗ , Yi-Lu Sun b , Chu-Chieh Lin b,∗∗ , Hui-Wen Chen c , Murthy Chavali c
a Department of Applied Chemistry, Providence University, 200 Chungchi Road, Shalu, Taichung, Hsien 433, Taiwan, ROC
b Department of Chemistry, National Chung-Hsing University, Taichung 402, Taiwan, ROC
c Center for Measurement Standards, Industrial Technology Research Institute, Hsinchu 300, Taiwan, ROC

Received 21 January 2005; received in revised form 6 September 2005; accepted 6 September 2005
Available online 10 October 2005

Abstract
Homogeneous TiO2 nanowires were fabricated by hydrothermal method. SEM pictures proved the yield of nanowires to be more than 90%.
Composite humidity sensing films were made by using TiO2 nanowires, TEOS and Nafion. FTIR absorption spectroscopy was used as a semi-
quantitative method to get information about the protonation. The sensing films were prepared by a dip-coating method. The composite films coated
on a pair of gold electrodes were tested for humidity sensors of resistance type. The measurement was carried out at five fixed humidity points
in the range of 12–97% relative humidity, which were controlled by employing five different salt solutions. Resistance changes were about three
orders of magnitude. The nanowires-based humidity sensors showed moderate sensitivity, short response and recovery time (<2 min) at relative
humidity less than 76%, and good long-term stability.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Nanowires; Nafion; Humidity; Impedance

1. Introduction Ceramic humidity sensors usually show better chemical resis-

Needs for humidity sensors are growing in industrial and
agricultural applications for monitoring and controlling the
surroundings is growing. Different measuring techniques, like
impedance [1,2], capacity [3–5], field effect transistors (FET)
[6], surface-acoustic wave (SAW) [7], quartz crystal microbal-
ance (QCM) [8–11], fiber optic [12–15] and microwave sensors
[16], have been explored for humidity detection. In recent years,
nanorod and nanowire films were fabricated and their humid-
ity sensitive characteristics have been investigated [17–19], and
these nanomaterial films were found to be efficient humid-
ity sensors. In consideration of quality and cost, impedance
type humidity sensors are becoming more prevalent. Humidity-
sensitive materials used in various fields are classified into three
groups: electrolytes, organic polymers and porous ceramics
[20].
∗
Corresponding author. Tel.: +886 4 26328001x15212; fax: +886 4 26327554.
∗∗
Corresponding author. Tel.: +886 4 22840411x718.
E-mail addresses: rjwu@pu.edu.tw (R.-J. Wu), cchlin@mail.nchu.edu.tw
(C.-C. Lin).
tance and mechanical strength than polymer sensors. TiO2 sens-
ing materials are commonly used in research for the reason
of easy fabrication. Gusmano and co-workers [21,22] used the
TiO2 modified with 1–10% K+ and Li+ through a sol–gel method
as a sensing material. The electrical resistance of the material
showed a variation of seven orders of magnitude with the change
in relative humidity (RH) from 4 to 90%. A humidity sensing
material ZrO2 –TiO2 increased the sensitivity by doping with
Li+ in the research of Jain et al. [23]. Nitsch et al. [24] used an
active thick film layer based on ZnO–TiO2 –Cr2 O3 as a sens-
ing material. Traversa and co-workers [25] used the technology
of electrochemical impedance spectroscopy to investigate the
humidity-sensing electrical conduction mechanism of the films
of TiO2 doped with 1–10% K+ and Li+ in the RH range of 4–87%
RH.
TiO2 nanowires are a kind of nano-scale material and have
been successfully synthesized by some research groups through
hydrothermal treatment, chemical vapor deposition or other
methods [26–28]. The TiO2 nanowires are very intriguing as a
humidity-sensing material. In the present study, therefore, com-
posite films of TiO2 nanowires and Nafion were made, since such
composites of fine ceramic particles and polymers are often used
as humidity sensors [1,2,31].

0925-4005/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2005.09.001
 R.-J. Wu et al. / Sensors and Actuators B 115 (2006) 198–204
2. Experiment
2.1. Fabrication of TiO2 nanowires
TiO2 nanowires were prepared by using hydrothermal
method in our laboratory. One gram of anatase TiO2 powder
(Sigma–Aldrich Co., Inc., USA) was placed into a Teflon-lined
autoclave, and 40 ml of 10 M aqueous NaOH solution was added.
Heating was maintained at 200 ◦ C for 24 h without stirring. After
the autoclave was cooled to room temperature naturally, the
obtained sample was washed sequentially with a dilute aqueous
HCl solution, distilled deionized water and ethanol sequentially
several times. A fibrous white crystalline product was obtained
after drying the sample at 70 ◦ C for 6 h.
2.2. Sensing material fabrication
Humidity sensing materials were fabricated by mixing the
TiO2 material (powder or nanowires), a Nafion solution and a
tetraethyl orthosilicate (TEOS) solution by the weight ratio of
1:500:500, but at various ratios for subsequent studies, including
0% for each component. The purity of the anatase TiO2 pow-
der was >99% (Sigma–Aldrich Co., Inc., USA). The Nafion®
solution was obtained from Aldrich (USA) and the concen-
tration was 5 wt.% in a mixture of lower aliphatic alcohols
and water. The TEOS (98%) as a binding material was pur-
chased from ACROS Organic Co., Inc., USA and was dissolved
into a mixed solution of methanol and water at a volume ratio
of TEOS:C2 H5 OH:H2 O = 5:16:2. The sensing films were dip
coated on an alumina substrate of 10 mm × 5 mm on which pair
of comb-like gold electrodes had been made (see Fig. 1), fol-
lowed by drying at 120–150 ◦ C for 1 h.
2.3. Measurement systems setup
An LCZ meter (DU-6022, made from Delta United Instru-
ment Co., Ltd.) was used in measuring the impedance signals of
the humidity sensors.
The standard humidity measurement system is shown
in Fig. 2. Actually, five systems with different humidity’s
were setup. The humidity in each setup was controlled by
employing five different saturated salt solutions, and was
calibrated with a standard fixed-point calibration with a
standard hygrometer (Rotronic M-131, UK) to the humid-
Fig. 2. Humidity measurement system.
199
Fig. 1. Structure of a humidity sensor element.
ity standard of National Measurement Laboratory, Taiwan,
ROC. The five humidity-controlling salt solutions of LiCl,
MgCl2 , NaBr, NaCl and K2 SO4 were kept at a constant tem-
perature 25 ± 2 ◦ C and the resulting humidity values were
12.0 ± 0.2, 33.2 ± 0.4, 50.0 ± 0.4, 75.8 ± 0.2 and 96.9 ± 0.6%
RH, respectively. Each humidity system has a dimension of
150 mm × 120 mm × 100 mm. Before first measurement of a
sensor, aging of each sensor was performed for 2 weeks in a 97%
K2 SO4 salt solution system. Long-term stability of the sensors
was tested in the humidity measurement systems for about 8
months.
Data on the temperature effect were obtained from experi-
ments carried out under the divided flow humidity system [8].
The divided flow humidity generator contained a dry-air flow
and a saturated humidity-air flow. The saturated humidity-air
and dry air were mixed together and then fed into a bottle-like
test chamber with a volume of 10 l to generate air of the required
humidity at a total flow rate of 10 l min−1 .
The apparatus for the divided flow system was Protec PC-540
from Sierra Instruments Inc., which was equipped with two mass
flow controllers and flow display power-supply. The humidity
sensors prepared were tested and calibrated in the test chamber.
The relative humidity, RH, of the test chamber was approxi-
mately given by
Msat
% RH = f × 100%
Msat + Mdry
200 R.-J. Wu et al. / Sensors and Actuators B 115 (2006) 198–204
where Msat and Mdry were the flow rates of saturated air and
dry air, and ‘f’ was the coefficient of this system which was
dependent on temperature and flow rate. The homemade sim-
ple apparatus has been developed for producing air of a known
relative humidity at temperatures ranging from 15 to 35 ◦ C.
2.4. FTIR experimental
The composite materials of TiO2 –TEOS–Nafion were sub-
jected to FTIR analysis using a Horiba Fourier transform infrared
spectrometer [FT-720, Japan] equipped with a DTGS detec-
tor. A NaCl crystal of 25 mm × 4 mm size (Spectral Systems
Inc., #955-3616, USA) was used to obtain the spectra. Each
spectrum was collected at room temperature under atmospheric
pressure, at an average of 64 scans with a 2 cm−1 resolution in
a transmission mode from 400 to 5000 cm−1 . In all experiments
background spectra were measured.
3. Results and discussion
3.1. SEM observations of TiO2 nanowires
SEM pictures revealed that TiO2 nanowires were successfully
fabricated by a hydrothermal method in our laboratory. Fig. 3a
and b and other SEM pictures revealed a high yield of nanowires
Fig. 3. SEM photographs of TiO2 nanowires: (a) magnification of ×40,000; (b)
magnification of ×10,000.
Fig. 4. Humidity characteristic curves of various TiO2 materials: (
) TiO2
nanowires/Nafion, () TiO2 powder/Nafion, (䊉) Nafion, () TiO2 nanowires,
() TiO2 powder.
over 90%. The average length of the wires was about 5–10 ␮m,
and the average diameter was 40–50 nm.
3.2. Response due to addition of TiO2 and Nafion
The original response calibration curve was defined by using
the materials of TiO2 powder and nanowires combined with
TEOS in Fig. 4. Impedance (Z/Ω) was the parameter of the
humidity measurement. A good sensitive characteristic curve
was not observed with the sensing materials of TiO2 powder and
nanowires combined with TEOS in the humidity ranging from
10 to 75%. The figure also reveals that mixing the inorganic TiO2
and organic hydrophilic Nafion changes the sensing curve. The
addition of Nafion was found to result in a remarkable increase
in sensitivity and a decrease in the impedance of the humidity
sensor. Nafion has been reported to enhance the water adsorption
at the sites of hydrophilic ionic group, –SO3 H−/+ [29].
The composite of TiO2 nanowires/Nafion exhibited the
higher sensitivity 2–3-folds than those of the composite TiO2
powder/Nafion or Nafion film alone. The impedance change
from the humidity range of 12–97% was more than three orders
of magnitude. Especially in the humidity range of 10–40%, the
TiO2 nanowires/Nafion revealed a better sensitivity curve. Some
nanomaterials like carbon nanotubes (CNTs) had been used in
our laboratory process to promote the adsorption of water [30]. It
has been reported that the SiO2 /Nafion composite can add to the
stability and good linearity of the sensor [31]. A SEM picture of
the composite TiO2 nanowires/Nafion sensing film is shown in
Fig. 5. Most of the TiO2 nanowires kept their original shape. A
part of nanowires penetrated into the surface of Nafion and some
remained on the surface. Nanowires have unusual electrical,
optical, magnetic, mechanical, thermal and biological proper-
ties due to their dimensions and high aspect ratios [length to
width ratio]. Thus TiO2 nanowires with homogeneous morphol-
ogy and high specific surface area can adsorb moisture easily and
 R.-J. Wu et al. / Sensors and Actuators B 115 (2006) 198–204
Fig. 5. SEM photograph of TiO2 nanowires/Nafion.
uniformly. The high sensitivity of the TiO2 nanowires/Nafion is
therefore attributed to the enhanced water adsorption on the TiO2
nanowires.
3.3. FTIR experimental data
A typical infrared (IR) spectrum of the composite material
was recorded on a NaCl crystal. Several bands were identified
from the obtained FTIR spectrum typical to the components
of the composite material (see Fig. 6). Most of the obtained
vibrational bands were similar to those of the published data.
TiO2 -anatase form nanowires having characteristic peaks at 638,
513 and 397 cm−1 were observed in the FTIR spectrum. The
peak at 397 cm−1 is not completely evident in the spectrum due
to the usage of NaCl crystal that has a cutoff nearly equal to
400 cm−1 . Nevertheless, an initiation of the prominent peak,
that is specifically characteristic to TiO2 -anatase, is obviously
visible from 404 cm−1 .
Fig. 6. FTIR spectrum of a TiO2 [anatase] nanowires–TEOS–Nafion composite.
201
A broad peak between 800 and 465 cm−1 is assigned to the
Ti–O–Ti stretching vibrations [13–15] with a valley centered
at 517 cm−1 . The peak at 638 cm−1 is superimposed with that
of a strong IR absorption peak of Si (640 cm−1 ) from TEOS
in the combined composite material spectrum. The peaks at
800 and 969 cm−1 are due to Si–O–Si and Si–OH, respectively,
also from TEOS. In addition there were also less significant
IR peaks at 509, 611, 755 and 805 cm−1 and a prominent
peak at 669 cm−1 . The band Ti–OH observed below 3500 cm−1
indicates the existence of hydrogen bonding. This interaction
between the organic and inorganic phase is favorable for the
improvement of the thermal stability and optical transparency
of the composite films. The IR spectrum of the hydrated titanium
dioxide [h-TiO2 ] shows a large broad band between 3250 and
3490 cm−1 and narrow bands at 1641 and 1454 cm−1 . The broad
band at 3250–3490 cm−1 is assigned to the stretching mode of
hydroxyl, δOH , while those at 1641 and 1454 cm−1 are assigned
to bending modes of hydroxyl δOH , respectively [32–34]. Com-
pared with the intensity of the characteristic absorption bands
of Ti–OH below 3500 cm−1 , an increase in peak area ratio sug-
gests increase in humidity sensing is due to the anatase TiO2
nanowires.
Humidity sensing of Nafion is usually observed at 1300 and
1056 cm−1 , which are anti-symmetric stretching and symmet-
ric stretching vibrations of the –SO3 − , respectively. However,
the anti-symmetric stretching vibrations of the –SO3 are unfortu-
nately shrouded by the strong C–F stretching bands exactly over
1300 cm−1 . Nevertheless humidity sensing can be evidenced
with the transfer of proton and the shift in peak centered at
1057 cm−1 . The presence of –SO3 − also accounts indirectly
for the proton transfer, supported by the increase in relative
peak area ratio at 1300 cm−1 , thus resulting in the disappear-
ance of asymmetric bands of the SO3 H− group at 1410 and
910 cm−1 and the changes in relative peak area ratios at 1057
and 1300 cm−1 .
202 R.-J. Wu et al. / Sensors and Actuators B 115 (2006) 198–204

Fig. 7. Humidity response curve of TiO2 nanowires/Nafion.

Fig. 9. Temperature effect of TiO2 nanowires/Nafion film: (
) 35 ◦ C, () 25 ◦ C,
() 17 ◦ C.
3.4. Response signal and hysteresis

A response curve of the TiO2 nanowires/Nafion film is shown

in Fig. 7. The response and recovery time T90 (T90 is defined as
the time required to reach the 90% of the final equilibrium signal)
was less than 1.5 min at the humidity range, of 12–75%. The
response time at the humidity of 97% was much longer than those
for the humidity ranging from 12 to 76%. This phenomenon was
also observed with the Nafion film.
Fig. 8 reveals the hysteresis data of the TiO2 nanowires/
Nafion film. Hysteresis was calculated as: [log10 (impedance
descending) log10 (impedance ascending)/log10 (impedance
descending at fixed point RH)]. The hysteresis of the sensing
film was small (calculated <2%).

3.5. Temperature effect and long time stability test

Temperature has some interference on the resistance sig-

nal of the TiO2 nanowires/Nafion film as shown in Fig. 9.
R = R0 exp(−Ea /RT) was used to calculate the activation energy Fig. 10. Long time stability test of TiO2 nanowires/Nafion film: () 12% RH,
(Ea ) of water adsorption on the sensing film. R represents the
(䊉) 33% RH, (
) 50% RH, () 76% RH, () 97% RH.

resistance of the humidity sensor, R is the gas constant and T

the absolute temperature. Ea of 12.9 kcal mol−1 was calculated
from the slope of the plot of ln(R) with ln(1/T) in 60% humidity
with a temperature interval of nearly 10 ◦ C.
The test data of long-term stability is shown in Fig. 10. The
impedance values of the sensor at five different testing points of
12, 33, 50, 76 and 97% RH did not show obvious deviation for
250 days.

4. Conclusion

In this research, humidity sensing was investigated by using

the TiO2 nanowires/Nafion material. For humidity range of
12–97% the change in resistance of the TiO2 nanowires/Nafion
Fig. 8. Hysteresis effect of TiO2 nanowires/Nafion film: () descending humid- sensing film was observed to be more than 1000. The nanowires
ity, () ascending humidity. humidity sensor showed moderate sensitivity, short response and
 R.-J. Wu et al. / Sensors and Actuators B 115 (2006) 198–204
recovery time (<2 min) for smaller than 76% humidity and a
good long-term stability for up to 250 days.
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Biographies
Ren-Jang Wu is an assistant professor in Department of Applied Chemistry
at Providence University. He received a BS in Chemistry from National Tsing
Hua University in 1986, an MS in Chemistry from National Taiwan University
in 1988 and a PhD in Chemistry from National Tsing Hua University in 1995.
His main areas of interest are chemical sensors, catalysis, nanoscience and
chemical standard technology.
Yi-Lu Sun received a BS degree in Chemistry from Soochow University in
1995, and an MS degree in Chemistry from National Chung-Hsing University
in 1997. He entered the PhD course of Chemistry at National Chung-Hsing
University in 2003. His main areas of interest are inorganic chemistry and
chemical sensor technology.
Chu-Chieh Lin is a professor of Department of Chemistry at National
Chung-Hsing University. He received a BS degree in Chemistry from Soo-
chow University in 1981, an MS degree in Nuclear Science from National
Tsing-Hua University in 1983 and a PhD degree in Chemistry from Texas
Tech University in 1992. His research interests are in inorganic chemistry
and chemical sensor technology.
Hui-Wen Chen received a BS in Chemistry from Chung Yuan Christian
University in 1998, and an MS in Chemistry from National Chung-Hsing
University in 2000. Her main areas of interest are electroanalytical chemistry
and chemical sensor technology.
Murthy Chavali received MSc (Tech.) in Chemistry from Jawaharlal Nehru
Technological University, India in 1994 and PhD Tech in 2000 from Technis-
che Universität Wien, Austria in Analytical Chemistry. He was a postdoctoral
204 R.-J. Wu et al. / Sensors and Actuators B 115 (2006) 198–204

scientist at Center for Instrumental Analysis, Kobe University, Japan, on
Japanese National Fellowship (JSPS) worked for NIR combustion sensors.
He served as Researcher at NSC-Taiwan for a short period. After that he
joined as a Researcher with sensors and standards group at CMS/ITRI-
Taiwan. His research interests are optical waveguide technology, IR sensors,
LIF, chip based chemical and biochemical sensors (␮ & n), development
and application of spectroscopic techniques for the study of nanomaterials.
His present work focuses on synthesis and fabrication of various organic and
inorganic nanostructures, nanocomposite materials, broadly nanotechnology
applications for gas and liquid sensors.