Nano Communication Networks 1 (2010) 283–288

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Nano Communication Networks

journal homepage: www.elsevier.com/locate/nanocomnet

High sensitivity of a ZnO nanowire-based ammonia gas sensor with Pt

nano-particles
Shoou Jinn Chang a , Wen Yin Weng a , Cheng Liang Hsu b , Ting Jen Hsueh a,∗
a
Institute of Microelectronics and Department of Electrical Engineering, Advanced Optoelectronic Technology Center, Center for Micro/Nano Science and
Technology, National Cheng Kung University, Tainan 70101, Taiwan
b
Department of Electronic Engineering, National University of Tainan, Tainan 700, Taiwan

article info abstract

Article history: We report the growth of high-density single crystalline ZnO nanowires on a patterned
Received 16 February 2010 ZnO:Ga/SiO2 /Si template, the adsorption of Pt nano-particles on the nanowire surface,
Received in revised form 17 July 2010 and the fabrication of a ZnO nanowire-based NH3 gas sensor. It was found that the sensor
Accepted 23 September 2010
responses were 22.5% and 36% for the nanowires without and with Pt adsorption when the
Available online 29 September 2010
chamber was injected with 1000 ppm of NH3 gas at 300 °C. With Pt adsorption, it was found
that the measured sensitivities were around 16%, 22%, 26% and 36% when the concentration
Keywords:
ZnO
of the injected NH3 gas was 100, 200, 500 and 1000 ppm, respectively.
Nanowires © 2010 Elsevier Ltd. All rights reserved.
Pt adsorption
Ammonia sensor

1. Introduction semi-conducting metal oxide materials generally involves

Ammonia (NH3 ) is a colorless gas with a distinctive
odor. Traditionally, the detection of gaseous NH3 was
performed either by potentiometric electrodes [15] or
by infrared devices [13]. However, these devices are
expensive and bulky. Recently, it was found that semi-
conducting metal oxide materials such as SnO2 [24],
MoO3 [18], ZnO [19], WO3 [10], In2 O3 [3], and TiO2 [11]
can all be used to detect NH3 vapor concentration. Of these,
ZnO is an interesting chemically and thermally stable
n-type semiconductor with a large exciton binding energy
of 60 meV and a large bandgap energy of 3.37 eV at room
temperature [21]. With these properties, ZnO has become
widely used in detectors sensitive to toxic and combustible
gases [4].
ZnO gas sensors with various forms, such as thick
films [22], thin films [25], heterojunctions [17], nanopar-
ticles [14] and nanowires [19], have all been demon-
strated. It should be noted that the gas sensing of the
the chemical reaction of gas molecules on the oxide
surface [6]. In recent years, one-dimensional (1D) ZnO
nanowires have attracted considerable attention since
they provide a much larger surface-to-volume ratio than
bulk ZnO and ZnO films [9]. With a large surface area,
nanowire-based gas sensors should be able to provide a
larger sensitivity. The other possible way to enhance the
sensitivity of the metal oxide gas sensor is to use noble
metal catalyst such as Pt, Pd and Au. It has been shown that
the presence of these noble metal elements on the surface
of a metal oxide can enhance its interaction with the reduc-
ing gases [1,12]. In this study, we report the growth of high
density ZnO nanowires on a patterned ZnO:Ga/SiO2 /Si
template and the adsorption of platinum (Pt) on nanowire
surfaces. In addition, the sensing properties of the ZnO
nanowires to NH3 gas will also be discussed.
2. Experiments

∗ Corresponding author. Tel.: +886 6 5050650x6641; fax: +886 6
5050553.
E-mail address: tj.Hsueh@gmail.com (T.J. Hsueh).
1878-7789/$ – see front matter © 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.nancom.2010.09.005
Prior to the growth of ZnO nanowires, a Si substrate
was thermally oxidized to form a 500 nm-thick SiO2 film.
A 100 nm-thick Ga-doped ZnO thin film was subsequently
284 S.J. Chang et al. / Nano Communication Networks 1 (2010) 283–288
80 µm
ZnO:Ga
SiO2
Si
Fig. 1. Schematic diagram of the patterned ZnO:Ga film after the etching
process.
deposited onto the SiO2 film by RF magnetron sputtering.
Standard photolithography was then performed to par-
tially etch away the ZnO:Ga film and define the pattern.
During wet etching, the template was dipped in 2% HCl
for 3 min to remove the exposed ZnO:Ga. Then, the etch-
ing mask was designed to make the fingers of the comb-
like pattern 10 µm wide and 80 µm long with a spacing
of 10 µm. Fig. 1 shows a schematic diagram of the pat-
terned ZnO:Ga/SiO2 /Si template used in this study. Two
small pieces of glass were used to cover the two electrodes
of the patterned ZnO:Ga film so that no ZnO nanowires
were grown in these regions. We then placed the patterned
ZnO:Ga/SiO2 /Si template and 99.9% pure zinc metal pow-
der on an alumina boat, and inserted them into a quartz
tube to grow the ZnO nanowires. During the growth, we
introduced argon and oxygen gases into the reaction sys-
tem and kept the Ar flow rate at 54.4 sccm. On the other
hand, we kept the O2 flow rate at 0.8 sccm. We also kept the
pressure inside the quartz tube, the reaction temperature
and the total growth time at 10 Torr, 600 °C and 60 min,
respectively.
To adsorb the Pt, we prepared an ethanol solution of
PtCl2 with an ethanol: PtCl2 ratio of either 50:1 or 2000:1
in a square alumina bath. We then immersed the sample
in the solution and placed the alumina bath in a Kinsten
KVB-30D ultraviolet (UV) box. Subsequently, the solution
and the alumina bath were irradiated by UV light for
4 min to absorb the Pt particles onto the surface of the
ZnO nanowires. During irradiation, the UV wavelength
and the UV power were kept at 380 nm and 100 W,
respectively. Finally, the sample was annealed at 480 °C
for 1 h in Ar ambient to remove any chlorine. A JEOL
JSM-7000F field emission scanning electron microscope
(FESEM) operating at 5 keV and an energy dispersive
X-ray (EDX) spectroscopy operating at 10 keV were then
used to characterize the structural properties of the ZnO
nanowires. To measure the gas sensing properties of the
nanowires, the sample was placed in a sealed chamber
and the resistivity of the sample in air was measured
from the two electrodes of the patterned ZnO:Ga film. We
then injected NH3 gas into the chamber and measured the
resistivity of the sample again in the presence of NH3 gas.
3. Results and discussion
Fig. 2(a) shows a top view FESEM image of the as-grown
ZnO nanowires prepared on the patterned ZnO:Ga/SiO2 /Si
template. It was found that ZnO nanowires were grown
vertically on the conducting ZnO:Ga finger regions. This
can be attributed the fact that these ZnO nanowires
were grown along the columnar grains of the underneath
sputtered ZnO:Ga film [8]. In contrast, the ZnO nanowires
(a)
SiO2
ZnO:Ga ZnO:Ga
1.5x10
-5
-5
(b)
1.0x10
-6
5.0x10
Current (A)
0.0
-6
-5.0x10
-5
-1.0x10
-1.5x10
-5
-5 -4 -3 -2 -1 0 1 2 3 4 5
Voltage (V)
Fig. 2. (a) FESEM image of the ZnO nanowires grown on the ZnO:
Ga/SiO2 /Si template. The inset shows Enlarged SEM photographs of the
ZnO nanowires grown on the SiO2 spacer regions. (b) I–V characteristics
measured from the two electrodes of the sample.
grown on SiO2 spacer regions were randomly oriented.
The inset in Fig. 2(a) shows an enlarged SEM photograph
of the ZnO nanowires grown on the SiO2 spacer regions.
It could be estimated from the inset of Fig. 2(a) that
the density of randomly oriented ZnO nanowires is
∼1.9 × 1012 cm−3 . Notably, these randomly oriented
ZnO nanowires provided electrical paths between the
neighboring fingers. With these randomly oriented ZnO
nanowires in the spacer regions, the two electrodes
were no longer electrically open. Fig. 2(b) plots the
current–voltage (I–V) characteristics measured from the
two electrodes in air. The active area of randomly oriented
ZnO nanowires is 4.4 mm2 . Since the resistivity, mobility
and electron concentration of the sputtered ZnO:Ga film
are 2.14 × 10−4  cm, 8.32 cm2 /V s and 3.51 × 1021 cm−3 ,
respectively, we should be able to neglect the resistance of
the ZnO:Ga film. In other words, the resistance measured
from the sample should originate from the resistance of the
randomly oriented ZnO nanowires in the spacer regions.
Fig. 3(a) and (b) show SEM photographs of the ZnO
nanowires treated with ethanol: PtCl2 ratio of 50:1 and
2000:1, respectively. As shown in Fig. 3(a), it was found
that large size Pt particles almost covered the entire
surface of the ZnO nanowires due to the extremely high
PtCl2 concentration used during Pt adsorption. This could
result in a smaller sensitivity of the gas sensor due to
the fact that the exposed ZnO surface was significantly
 S.J. Chang et al. / Nano Communication Networks 1 (2010) 283–288
a For NH3 gas sensing, it is known that oxygen sorp-
b O2 (absorbed) + e
c temperatures. A Ru2 O heating electrode was deposited
1 2 3 4 5 6 7 8
Full Scale 602 cts Cursor: o.ooo keV
Fig. 3. SEM photographs of the ZnO nanowires grown on the SiO2 spacer
regions with different ethanol solutions of PtCl2 (a) ethanol: PtCl2 = 50:1
or (b) 2000:1. (c) EDX spectrum measured from the surface of the stained
ZnO nanowires.
smaller. In contrast, it can be seen that nanometer-sized
particles were adsorbed on the nanowire surface for the
sample treated with an ethanol: PtCl2 ratio of 2000:1.
These nanometer-sized Pt particles should act as a catalyst
that can enhance the interaction of the reducing gas and
the ZnO nanowires. Fig. 3(c) shows the EDX spectrum
measured from the surface of the stained ZnO nanowire.
It can be seen that we observed a clear Pt peak while no
Cl-related signal was found. Such a result indicates that we
have indeed adsorbed Pt nano-particles onto the nanowire
surfaces (i.e., ZnO nanowires with Pt).
285
tion plays an important role in the electrical transport
properties of ZnO nanowires. The oxygen ionosorption
removes conduction electrons and thus lowers the con-
ductance of ZnO [16]. Hence, the sensing mechanism of
ZnO on NH3 vapor may be described as follows. The re-
active oxygen species such as O− 2 , O
2−
and O− are first
adsorbed on the ZnO surface at elevated temperatures. It
should be noted that the chemisorbed oxygen species de-
pend strongly on temperature. At low temperatures, O− 2 is
commonly chemisorbed. At high temperatures, however,
O− and O2− are commonly chemisorbed while O− 2 disap-
pear [12]. The reaction kinematics can be described as fol-
lows [20]:
O2 (gas) ↔ O2 (absorbed) (1)
−
↔ O2−
(2)
−
O2 + e −
↔ 2O . −
(3)
Thus, the resistance of the ZnO nanowires will decrease as
the reducing NH3 gas is introduced into the test chamber
due to the exchange of electrons between the ionosorbed
species and the ZnO itself. On the other hand, the reaction
between the reducing NH3 gas and the surface of the ZnO
nanowires can be described by [22]:
2NH3 + 3O− (ads) ↔ 3H2 O + N2 + 3e− . (4)
It should be noted that this reaction involves a change
of surface state charges. Fig. 4(a) shows the detector
responses of the ZnO nanowire sensor with Pt nano-
particles (ethanol: PtCl2 = 2000:1) measured at various
on the back side of the Si substrate [7]. The sensor
thus can operate at life environment by heating the
electrode to control the substrate temperature. During
these measurements, 1000 ppm of NH3 gas was introduced
into a sealed chamber and we measured the resistivity of
the sensor both in air (Ra ) and in the presence of NH3
gas (Rb ). To quantify the sensor performance, we define
the response of our sensor as [((Ra − Rb )/Ra ) × 100%].
With this definition, it was found that the measured sensor
responses were 17.2%, 25.62%, 33.45%, 36% and 32.26%
when the device was operated at 150, 200, 250, 300 and
350 °C, respectively. Fig. 4(b) shows the sensor responses
of the ZnO nanowires with various ethanol: PtCl2 ratios
measured at 300 °C with 1000 ppm NH3 introduced. It was
found that measured sensor responses were 0%, 13.2%, 36%,
30% and 23% when the device was operated with ethanol:
PtCl2 ratios of 50:1, 1000:1, 2000:1, 4000:1 and 10000:1,
respectively. With the use of a high PtCl2 concentration
(ethanol: PtCl2 = 50 : 1), the large size Pt particles almost
covered the entire surface of the ZnO nanowires, as shown
in Fig. 3(a). They caused a low resistivity in the NH3
sensor which resulted in no observed sensor response.
With an ethanol: PtCl2 ratio of 10000:1, it was found that
almost no Pt nano-particles adsorb on the ZnO nanowires.
The sensor response thus is almost equal to that from
pure ZnO nanowires. It could be noticed that the use of
ethanol: PtCl2 = 2000:1 solution provides the largest
sensor response on the fabricated ZnO-nanowire based
NH3 sensors.
286 S.J. Chang et al. / Nano Communication Networks 1 (2010) 283–288

a 40 a
NH3=1000 ppm Temperature = 300°C 1000 ppm
40
35 Nanowires active area=4 mm2
500 ppm
Sensor response (%)

Sensor response (%)

30 30 300 ppm
200 ppm
25 20 100 ppm

ZnO nanowires with Pt

20 (Ethanol : PtCl2 = 2000 : 1)
10
Nanowires active area=4 mm2
15
150 200 250 300 350
0
Temperature (°C) 0 500 1000 1500 2000 2500

b 45 Time (sec)

40
Temperature=300°C b 10
NH3 =1000 ppm Temperature = 300°C
Sensor response (%)

35
Nanowires active area=4 mm2 60 ppm
30 8

Sensor response (%)

40 ppm
25
6 20 ppm
20
10 ppm
15 Gas out
4 5 ppm
10
5 Nanowires active area=4 mm2 Gas
2 in
0
50:1 1000:1 2000:1 4000:1 10000:1
0
Ethanol : PtCl2 ratio 0 500 1000 1500 2000 2500 3000
Time (sec)
Fig. 4. (a) Sensor responses of the ZnO nanowires sensor with Pt
adsorption (ethanol : PtCl2 = 2000:1) measured at various temperatures. Fig. 6. (a) and (b) show the sensor responses of the ZnO nanowires
(b) Sensor responses of ZnO nanowires with various ethanol: PtCl2 ratios with Pt adsorption (ethanol: PtCl2 = 2000:1) measured at various NH3
measured at 300 °C. concentrations.

50
Temperature = 300°C NH3 gas injection and pumping. These measurements were
NH3 = 1000 ppm performed by injecting various amounts of NH3 gas into
40 Nanowires active area=4 mm2 Gas out
the sealed chamber followed by pumping at 300 °C. It was
Sensor response (%)

found that the measured sensitivities were around 16%,

30
20
Gas in
10
0
0 100 200
Fig. 5. Detector responses of the ZnO nanowire-based NH3 vapor sensors
measured at 300 °C.
Fig. 5 shows the detector responses of the pure and
adsorbed Pt ZnO nanowire NH3 gas sensor measured at
300 °C. It can be seen that the sensor response was 36%
for the ZnO nanowires with Pt adsorption. In contrast, the
sensor response was only around 22.5% for the pure ZnO
nanowires. In other words, we can indeed significantly
enhance the sensitivity of NH3 gas by the adsorption of
Pt nano-particles on the ZnO nanowire surface. Fig. 6(a)
shows the sensitivity variations of the ZnO nanowires with
Pt adsorption (ethanol: PtCl2 = 2000:1) when exposed to
22%, 26% and 36% when the concentration of the injected
NH3 gas was 100, 200, 500 and 1000 ppm, respectively.
In other words, the sensor response increased with the
increase in NH3 gas concentration. To know the detected
limit of NH3 concentration, a small NH3 concentration
was also introduced into the test chamber and the sensor
pure ZnO nanowires response measured. As shown in Fig. 6(b), it was found
ZnO nanowires with Pt
that the measured responses were around 2.88%, 3.97%,
300 400 500 600 700 5.04%, 6.21% and 7.58% when the concentration of the
Time (sec)
injected NH3 gas was 5, 10, 20 40 and 60 ppm, respectively.
From the results, it was noticed that the Pt adsorbed ZnO
nanowire sensor can detect small NH3 concentrations of
even 5 ppm for a given active area of 4 mm2 . It was also
found that the rise and fall times of the ZnO nanowire
sensor were both around 100 s. The gas response time
following an Arrhenius-type behavior is described by:
τ (T ) = τ0 exp(Ea/kB T ) (5)
where Ea is the activation energy for adsorption and T
is the operation temperature [5]. When NH3 molecules
reach the Pt surface, the NH3 dissociates and subsequently
reacts with the adsorbed oxygen species more rapidly. This
contributes to a reduced activation energy for adsorption.
 S.J. Chang et al. / Nano Communication Networks 1 (2010) 283–288
b
a
c
Fig. 7. (a) and (b) are sketches of the surface-depletion model, (c) and (d) are sketches of the surface independent model and (e) is the sketch of the noble
metal catalyst model.
Using the adsorption of the noble metal Pt to improve
the NH3 gas sensitivity of ZnO nanowires, the sensing
mechanism included the grain boundary model, the
surface depletion model and the noble metal catalyst
model (Fig. 7) [2]. Fig. 6(a) shows the surface of the
ZnO nanowires adsorbing oxygen species and abstracting
electrons, and thus, causing an increase in the potential
barrier at the interface between ZnO nanowires. As the
reducing gas NH3 was introduced, the potential barrier
was decreased thereby decreasing the resistance of the
sensor, as shown in Fig. 6(b). As a result, the sensing
mechanism is similar to the grain boundary model [23].
For the surface depletion model, as shown in Fig. 6(c),
when the ZnO nanowire is surrounded by air, oxygen
molecules will adsorb on the nanowire surface to generate
287
d
chemisorbed oxygen species by capturing electrons from
the conductance band. Thus, the ZnO nanowire will
become highly resistive. When NH3 gas is introduced,
the ZnO nanowire is exposed to the traces of reductive
gas. By reacting with the oxygen species on the nanowire
surface, the reductive gas will reduce the concentration of
oxygen species on the nanowire surface and thus increase
the electron concentration, as shown in Fig. 6(d) [2].
The larger sensitivities observed from the ZnO nanowires
with Pt can be attributed to the the noble metal catalyst
model [12]. With Pt on the ZnO nanowire surface, O2
molecules dissociate and generate chemisorbed oxygen
species very rapidly due to the enhanced interaction by Pt.
As shown in Fig. 6(e), we can thus achieve a much greater
sensitivity from the ZnO nanowires with Pt nano-particles.
288 S.J. Chang et al. / Nano Communication Networks 1 (2010) 283–288
4. Conclusions
In summary, we report the growth of high-density
single crystalline ZnO nanowires on a patterned ZnO:Ga/
SiO2 /Si template, the adsorption of Pt nano-particles
on the nanowire surface, and the fabrication of a ZnO
nanowire-based NH3 gas sensor. It was found that the
sensor responses were 22.5% and 36% for the nanowires
without and with Pt adsorption when the chamber was
injected with 1000 ppm NH3 gas at 300 °C. It was also
found that the sensitivity increased from 16% to 36% as
we increased the concentration of the NH3 gas from 100
to 1000 ppm.
Acknowledgements
This work was supported in part by the Center for Fron-
tier Materials and Micro/Nano Science and Technology,
National Cheng Kung University, Taiwan (D97-2700). This
work was also in part supported by the Advanced Opto-
electronic Technology Center, National Cheng Kung Uni-
versity, under projects from the Ministry of Education.
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Shoou-Jinn Chang was born in Taipei, Taiwan,
on January 17, 1961. He received a B.S.E.E.
degree from the National Cheng Kung University
(NCKU), Tainan, Taiwan, in 1983, a M.S.E.E.
degree from the State University of New York,
Stony Brook, in 1985, and a Ph.D. degree in
electrical engineering from the University of
California, Los Angeles, in 1989.
He was a Research Scientist with NTT Basic
Research Laboratories, Musashino, Japan, from
1989 to 1992. In 1992, he became an Associate
Professor with the Department of Electrical Engineering, NCKU, and was
promoted to Full Professor in 1998. Currently, he also serves as the
Deputy Director of the Center for Micro/Nano Science and Technology
and the Director of Semiconductor Research Center, NCKU. He was a
Royal Society Visiting Scholar with the University of Wales, Swansea, U.K.,
from January 1999 to March 1999, a Visiting Scholar with the Research
Center for Advanced Science and Technology, University of Tokyo, Japan,
from July 1999 to February 2000, a Visiting Scholar with the Institute of
Microstructural Science, National Research Council, Canada, from August
2001 to September 2001, a Visiting Scholar with the Institute of Physics,
Stuttgart University, Germany, from August 2002 to September 2002, and
a Visiting Scholar with the Faculty of Engineering, Waseda University,
Japan, from July 2005 to September 2005. He is also an Honorary Professor
of the Changchun University of Science and Technology, China. His
current research interests include semiconductor physics, optoelectronic
devices, and nanotechnology.
Prof. Chang received the outstanding research award from the
National Science Council, Taiwan, in 2004.
Wen-Yin Weng received a B.S. degree in the
Department of Electrical Engineering from the
National University of Kaohsiung, Kaohsiung,
Taiwan, in 2006, and a M.S. degree in 2008
from the Institute of Electro-Optical Science and
Engineering, National Cheng Kung University
(NCKU), Tainan, where he is currently working
toward a Ph.D. degree at the Institute of Mi-
croelectronics and Department of Electrical En-
gineering, Advanced Optoelectronic Technology
Center, Center for Micro/Nano Science and Tech-
nology. His current research interests include optoelectronics devices of
III–V compound semiconductors and nanoscale 1D semiconductors.
Cheng-Liang Hsu received a B.S. degree in elec-
tronic engineering from Chung Yuan Christian
University, Chung-Li, Taiwan in 1996. He re-
ceived a M.S. degree in 1998 from the Depart-
ment of Electronic Engineering, National Taiwan
University of Science and Technology, Taipei,
Taiwan, and received a doctorate in 2005 from
the Department of Electrical Engineering, Na-
tional Cheng Kung University, Tainan, Taiwan.
From 2000 to 2003, he was an Engineer with
the Taiwan Semiconductor Manufacturing Com-
pany. From 2003 to 2005, he was with the Material Research Laboratories
of Industrial Technology Research Institute. From 2005 to 2006, he joined
the Department of Electrical & Electronic Engineering, Ming Chi Univer-
sity of Technology, Taiwan as an Assistant Professor. In 2006, he joined
the Department of Electronics Engineering, National University of Tainan,
Taiwan as an Assistant Professor. His current research interests focus on
nanoscale one-dimensional semiconductors.
Ting-Jen Hsueh received a M.S. degree in Elec-
trical Engineering from the National Kaohsi-
ung University of Applied Sciences, Kaohsiung,
in 2004, and a Ph.D. degree in Microelectron-
ics from the National Cheng Kung University
(NCKU), Tainan, Taiwan, in 2008. From Septem-
ber 2008 to January 2009, he was a postdoctoral
researcher with the Institute of Microelec-
tronics, Advanced Opto-electronic Technology
Center, Center for Micro/Nano Science and Tech-
nology, NCKU; he is currently a postdoctoral re-
searcher with the National Nano Device Laboratories (NDL). His current
research interests include nanoscale 1D semiconductors and solar cells.