Journal of Science: Advanced Materials and Devices 3 (2018) 139e144

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Journal of Science: Advanced Materials and Devices

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

Original Article

Hydrothermal synthesis of CeO2eSnO2 nanocomposites with highly

enhanced gas sensing performance towards n-butanol
K. Rackesh Jawaher a, R. Indirajith a, S. Krishnan b, *, R. Robert c, S.K. Khadheer Pasha d,
Kalim Deshmukh a, S. Jerome Das e
a
Department of Physics, B. S. Abdur Rahman Crescent Institute of Science and Technology, Chennai 600048, Tamil Nadu, India
b
Department of Physics, Ramakrishna Mission Vivekananda College (Autonomous), Mylapore, Chennai 600004, Tamil Nadu, India
c
Department of Physics, Government Arts College for Men, Krishnagiri 635001, India
d
Department of Physics, VIT-AP, Amaravati Campus, Guntur 522501, Andhra Pradesh, India
e
Department of Physics, Loyola College, Chennai 600 034, Tamil Nadu, India

a r t i c l e i n f o a b s t r a c t

Article history: CeO2eSnO2 nanocomposite, a sensing material, was successfully synthesized by a hydrothermal method.
Received 22 January 2018 The structural, optical and morphological properties of as-prepared CeO2eSnO2 nanocomposites were
Received in revised form characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-Vis diffuse
21 March 2018
reflectance spectroscopy and field emission scanning electron microscopy (FESEM). The results reveal
Accepted 22 March 2018
Available online 30 March 2018
that the highly crystalline nanocomposite heterostructure is formed, and it possesses a spherical-like
morphology with an average grain size of 30 nm. Furthermore, the gas sensing properties towards
several volatile organic compounds (VOCs) such as n-butanol, isopropanol, ethanol and acetone were
Keywords:
TEM
studied. Interestingly, comparing with bare SnO2 and CeO2, the CeO2eSnO2 sensor shows the highest
FESEM sensitivity towards n-butanol at an operating temperature of 110
C. This indicates that the CeO2eSnO2
CeO2eSnO2 nanocomposites nanocomposite can be a promising candidate for sensor application towards the detection of n-butanol.
VOCs © 2018 The Authors. Publishing services by Elsevier B.V. on behalf of Vietnam National University, Hanoi.
Gas sensors This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

1. Introduction to extensive applications such as gas sensors [9e11], dye sensitized

Volatile organic compounds (VOCs) include a category of
organic compounds, such as alcohols and aromatic hydrocarbons,
which can easily evaporate at room temperature [1]. In general, it is
difficult to detect VOCs because they are colorless and odorless.
However, after evaporation, VOCs are toxic, irritating smell and can
cause serious adverse effects on human health [2]. In VOCs detec-
tion, gas sensors play a significant role in the areas of emission
control, biological detection, public safety, and environmental
protection [3]. Recently, there has been substantial interest in the
preparation of binary oxide nanocomposite materials such as
ZnOeCdO [4], In2O3eSnO2 [5], CeO2eZnO [6], and SnO2eTiO2 [7],
which plays a vital role in the detection of different VOCs. Hung et
al. have provided an updated review on semiconductor metal oxide
nanowires for VOCs gas sensors [8]. SnO2 is an n-type semi-
conductor, with a wide band gap (Eg) of 3.6 eV. It has been devoted
* Corresponding author. Fax: þ91 44 42169045.
E-mail address: skrishnanjp@gmail.com (S. Krishnan).
Peer review under responsibility of Vietnam National University, Hanoi.
solar cells [12], and catalytic process [13]. Particularly, it has
received a high degree of interest in the field of gas sensor. It has
been well studied as a sensor material for the detection of both
reducing and oxidizing gases [14e17]. Meanwhile, mixing with rare
earth oxides, especially cerium oxide, is particularly attractive as an
additive, due to its low cost, rich surface oxygen vacancies and low
redox potential between Ce3þ and Ce4þ [18]. Due to this, CeO2 and
SnO2 could remarkably enhance the gas sensing mechanism. A few
literature reports are available on the study of CeO2eSnO2 based
sensors for the detection of VOCs. Recently, Liu et al. prepared CeO2
decorated SnO2 hollow spheres by the two-step hydrothermal
technique showing the enhanced gas sensing property to 100 ppm
in ethanol [19]. Qin et al. successfully synthesized porous
CeO2eSnO2 composite nanofibers using electrospinning technique,
thereby exhibiting the excellent sensing performances towards H2S
and ethanol [20]. However, to the best of our knowledge, the gas-
sensing performance of CeO2eSnO2 binary oxides towards n-
butanol has not been reported yet. N-butanol is very largely used as
an industrial solvent, an extracting agent and an organic synthesis
intermediate. Prolonged exposure to the n-butanol environment

https://doi.org/10.1016/j.jsamd.2018.03.006
2468-2179/© 2018 The Authors. Publishing services by Elsevier B.V. on behalf of Vietnam National University, Hanoi. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/).
140 K.R. Jawaher et al. / Journal of Science: Advanced Materials and Devices 3 (2018) 139e144

could cause symptoms such as dizziness, headache, somnolence
and dermatitis [21e23]. Hence, it is very necessary to detect n-
butanol gas for both environmental safety and human healthcare.
Herein, a CeO2eSnO2 nanocomposite was successfully synthesized
through a simple hydrothermal method. The obtained product was
further used to investigate the structural, optical and the
morphological properties. The gas-sensing properties such as
sensitivity, selectivity and response and recovery time were eval-
uated, and the possible gas sensing mechanism was also discussed.
This binary oxide nanocomposite will be very useful for gas sensing
applications.
2. Experimental
2.1. Synthesis of CeO2 nanoparticles
For the synthesis of CeO2 nanoparticles, ammonium ceric sulfate
((NH)4)4 [Ce (SO4)4]$2H2O) and C2H2O4$2H2O were used as pre-
cursor materials. 0.1 M of ((NH)4)4[Ce(SO4)4]$2H2O) was dissolved
in 20 ml of deionized water and then the solution was stirred
vigorously. Subsequently, 0.3 M of C2H2O4$2H2O was dissolved in
20 ml of deionized water and added drop by drop to the solution of
((NH)4)4[Ce(SO4)4]$2H2O) under continuous stirring. Then, 0.75 g
of polyvinylpyrrolidine (PVP) was dissolved in 10 ml of deionized
water and added drop by drop to the mixture of C2H2O4$2H2O and
((NH)4)4[Ce(SO4)4]$2H2O). The resulting solution was continuously
stirred for 5 h. Finally, the precipitated solution was transferred to a
100 ml Teflon-lined stainless steel autoclave and heated for 24 h at
180
C. Then, the autoclave was cooled down to room temperature.
The resulting product was collected by centrifugation and washed
several times with distilled water and ethanol followed by drying at
100
C for 12 h. The dried product was grounded in agate mortar
and calcined at 450
C for 3 h to get bare cerium oxide nanopowder.
2.2. Synthesis of SnO2 nanoparticles
For the synthesis of SnO2 nanoparticles, inorganic compounds
such as tin chloride dihydrate (SnCl2$2H2O) and oxalic acid
(C2H2O4$2H2O) were used as starting materials. In a typical process,
0.2 M of SnCl2$2H2O was dissolved in 20 ml of deionised water and
stirred for 30 min. Subsequently, 0.3 M of oxalic acid was dissolved
in 20 ml deionised water. The solution of tin chloride dihydrate was
added drop by drop into the solution of oxalic acid and then 0.75 g
of PVP was added. This solution was stirred for few hours until the
milky white precipitate was obtained. Later, this white solution was
transferred into a 100 ml Teflon-lined stainless-steel autoclave and
heated for 12 h at 180
C under static conditions. Then, the auto-
clave was cooled down to room temperature. The precipitate was
centrifuged and washed several times with distilled water and
ethanol and dried at 100
C. The dried product was grounded in
agate mortar. Finally, the powder was transferred into alumina
crucible and calcined at 450
C for 3 h to get bare tin oxide
nanopowder.
precipitate. The precipitated solution was transferred to a 100 ml
Teflon-lined stainless steel autoclave and kept at 180
C for 24 h and
then cooled down to room temperature. The resulting products
were washed with deionized water and absolute ethanol for several
times by centrifugation and finally dried at 100
C for 24 h. The
conversion of Ce(OH)4 and Sn(OH)2 to CeO2 and SnO2 nano-
structures was carried out in muffle oven at 450
C for 4 h.
2.4. Characterizations
The synthesized samples were characterized by X-ray diffraction
(XRD) using XPERT PRO X-ray diffractometer with Cu-Ka radiation
(l ¼ 1.5406 Å) in the 2q range between 20
and 80
at room tem-
perature. The optical absorption spectra of the samples were
recorded using a UV-VIS spectrophotometer (Shimadzu, UV-1800)
in the wavelength range 200e800 nm. Surface morphology and
elemental compositions of the as-prepared nanocomposites have
been determined using field emission scanning electron microscope
(FESEM with EDAX, Carl Zeiss, Supra 55). High-resolution trans-
mission electron microscopy (HRTEM) observations were carried
out with Tecnai G2 (TF20) microscope operated at an accelerating
voltage of 200 kV.
2.5. Gas sensing measurement
The gas sensor setup was constructed within a glass chamber
having provision of inlet and outlet with a semiconducting alumina
ceramic tube and heating coil. In order to produce and maintain
temperature of the surrounding of a sensor, a temperature
controller is connected with power and voltage suppliers. The
dimension of the tube was taken as 5e6 mm in length and 2e3 mm
in radius. Initially, the CeO2eSnO2 composites were mixed and
grounded with the binder polyvinyl alcohol (PVA) which was
subsequently coated on a alumina ceramic tube. The thickness of
coated film was kept around 20e30 mm.
3. Results and discussion
3.1. Structural characteristics
XRD measurement was performed to identify the phase com-
positions of the as-prepared SnO2, CeO2 and CeO2eSnO2 nano-
composites and the results are shown in Fig. 1. All the diffraction
peaks can be perfectly indexed with those of standard patterns for
cubic structure of CeO2 (JCPDS.34-0394) and tetragonal rutile
structure of SnO2 (JCPDS 41-1445). For bare CeO2, the diffraction
peaks at 28.5
, 33.1
, 47.4
, 56.3
, 59.1
, 69.4
, 76.7
and 79.1
were

2.3. Synthesis of CeO2eSnO2 nanocomposite

For synthesis of CeO2eSnO2 nanocomposite, SnCl2$2H2O,

((NH)4)4[Ce(SO4)4]$2H2O) and C2H2O4$2H2O were used as pre-
cursors. In a typical synthesis process, 0.2 M of SnCl2$2H2O and
0.1 M of ((NH)4)4[Ce(SO4)4]$2H2O were first dissolved individually
in de-ionized water and stirred for 1 h and subsequently 0.3 M of
C2H2O4$2H2O was dissolved into 20 ml of deionised water. This
solution was added drop by drop to the mixture of SnCl2$2H2O and
0.1 M of ((NH)4)4[Ce(SO4)4]$2H2O under continuous stirring. Later,
0.75 g of PVP was slowly added into the solution resulting in a white Fig. 1. XRD patterns of pure SnO2, pure CeO2 and CeO2/SnO2 nanocomposite.
 K.R. Jawaher et al. / Journal of Science: Advanced Materials and Devices 3 (2018) 139e144
detected which can be assigned to the face-centered cubic CeO2
phase. For bare SnO2, the diffraction peaks at 26.6
, 33.8
, 37.8
,
51.7
, 52.1
, 54.7
and 65.1
are primarily ascribable to the tetrag-
onal rutile SnO2 phase. Furthermore, two sets of diffraction peaks
exist for CeO2eSnO2 nanocomposites, corresponding to the cubic
structure CeO2 and the rutile structure of SnO2. No obvious phase
shift and no additional peaks were observed, suggesting that the
synthesized materials are composed of nanocrystalline CeO2 and
SnO2. The intensity of the CeO2 peaks was relatively low. This in-
dicates a relatively small amount of CeO2 present in the composite
nanostructure. According to the Scherrer equation, the crystallite
sizes of CeO2 and SnO2 nanostructures are estimated to be 25.6 nm
and 23.19 nm, respectively.
3.2. Optical characteristics
Fig. 2 shows the typical room-temperature UVeVis absorption
spectra for synthesized nanocomposites calcined at 450
C. The
band gap energy (Eg) of CeO2, SnO2 and CeO2eSnO2 are obtained
from the wavelength value corresponding to the intersection point
of the vertical and horizontal part of the spectrum using the
following equation:
hc 1240
Eg ¼ eV ¼ eV:
l l
where, Eg is the band gap energy (eV), l is the wavelength (nm), h is
the Planck's constant (6.626  1034 Js) and C is the velocity of light
(3  108 m/s). The absorbance edge wavelengths of CeO2 and SnO2,
CeO2eSnO2 nanocomposite were measured to be 280, 336 and
285 nm with the corresponding band gap energies of 4.42, 4.35,
3.6 eV, respectively. Furthermore, the absorption edge of the
CeO2eSnO2 nanocomposite lies in between that of the bare CeO2
and SnO2. Compared to the pure CeO2, the CeO2eSnO2 nano-
composite showed an obvious absorption edge decrement of about
51 nm. Nevertheless, it was close to that of SnO2 because of 2:1
composition of the material. This result suggests that the absorp-
tion edge of the heterostructure such as CeO2eSnO2 nano-
composite is due to contribution of the each component in the
system.
3.3. Morphological characteristics
The morphology of CeO2eSnO2 nanocomposite was investi-
gated by FE-SEM as shown in Fig. 3 (a). The typical FESEM image of
the as-prepared products revealed that the CeO2eSnO2 nano-
composites are homogeneously dispersed and composed of
Fig. 2. UVevis absorption spectra of SnO2, CeO2 and CeO2/SnO2 nanocomposite.
141
spherical morphology. Moreover, the heterointerface contact be-
tween CeO2eSnO2 nanoparticles can be envisaged. Further, the
elemental analysis of the CeO2eSnO2 nanocomposites was carried
out by using energy dispersive X-ray spectrometer (EDS) and the
results are shown in Fig. 3 (b). It distinctly shows that the synthe-
sized sample contains only Ce, Sn, and O elements which confirm
that cerium oxide has been successfully mixed with SnO2 crystal
lattice. This is further revealed by the respective TEM and HRTEM
images of CeO2eSnO2 nanocomposites which are shown in Fig. 4a
and b. From Fig. 4a, the TEM image clearly shows an interconnected
agglomeration with highly crystalline in nature which is in good
agreement with FESEM result. The magnified HRTEM image in
Fig. 4b exhibits a clear lattice fringes with an interplanar distance of
0.314 and 0.336 nm, corresponding to the (111) and (110) planes of
cubic CeO2 and tetragonal rutile SnO2, respectively. The result
suggests that the particle size was about 28 nm and this value is in
the close vicinity to value obtained from XRD analysis. Further, the
selected area electron diffraction (SAED) pattern reveals the dif-
fracted rings of CeO2 and SnO2 which are presented in Fig. 4c.
3.4. Gas sensing performances
The sensor response (Sg) was defined as (Ra  Rg)/Ra or Sg ¼ Ra/
Rg, where Ra and Rg were the electrical resistances of the sensor in
air and in test to each organic vapor, respectively [24]. The sensor
response towards each gas is substantially governed by its oper-
ating temperature. Fig. 5 depicts the sensor response of the CeO2,
SnO2 and CeO2eSnO2 nanocomposites towards n-butanol gas were
examined over a range of operating temperature. The optimal
operating temperatures of corresponding sensors were determined
to be 110
C. The maximum sensor response of CeO2eSnO2, SnO2
and CeO2 gas sensors were found upon exposure toward n-butanol
vapor at 100 ppm concentration with the value of 75.6, 59.8 and
44.8, respectively. It is clearly evident that CeO2eSnO2 sensor
shows the remarkably improved sensor response compared to the
bare CeO2 and SnO2 sensor. It was manifested that the sensing
response of the sensor initially was increased with working tem-
perature, attains the maximum, and then gradually decreased.
Furthermore, the sensor response also depends on the con-
centration of the gas. Fig. 6 illustrates the sensor response of the
CeO2, SnO2 and CeO2eSnO2 nanocomposite sensor at the different
concentrations of n-butanol ranging from 0 to 400 ppm at 110
C.
The response of the sensor was found to increase with increasing
the gas concentration. With further increasing the gas concentra-
tion above 100 ppm, the response gets saturated.
Similarly, Fig. 7 shows the selectivity of sensor response towards
100 ppm of various gases such as acetone, ethanol, isopropanol and
n-butanol was conducted at 110
C. The selectivity of gas sensors
are usually defined as the ratio of sensitivity to different test gases
atmosphere at the same concentration and temperature. The
maximum sensor response enhancement toward n-butanol vapor
with the highest value is 75.52. It can be clearly seen that n-butanol
exhibits high selectivity as compared with other gases recorded.
Response and recovery times are very important basic parame-
ters to determine the working of a sensor in real time fast changing
environment [25]. Fig. 8 shows the response transients of
CeO2eSnO2, CeO2 and SnO2 gas sensors exposed to 100 ppm n-
butanol gas at 110
C. The sensing measurements were performed by
injecting n-butanol gas into the chamber first and sensor's resistance
was measured in air and in the presence of n-butanol gas. Similarly,
the same experimental conditions were used for measuring the
sensing behavior of bare sensor. The response and recovery time of
CeO2eSnO2, CeO2 and SnO2 sensor towards n-butanol gas were
determined to be 5/18 s, 10/32 s, and 12/39 s, respectively. Mani-
festly, CeO2eSnO2 sensor exhibits faster response/recovery time
142 K.R. Jawaher et al. / Journal of Science: Advanced Materials and Devices 3 (2018) 139e144

Fig. 3. (a) FE-SEM image, (b) EDS spectra of the as-prepared CeO2/SnO2 nanocomposite.

Fig. 4. (a) TEM image, (b) HRTEM image and (c) SAED pattern of the as-prepared CeO2/SnO2 nanocomposite.

than the bare sensor. As a consequence, n-butanol shows the faster
reaction of adsorbed oxygen with enhancement in the electrical
conductivity of the sensor and as a result enhances the sensitivity.
3.5. Gas sensing mechanism
As typical n-type semiconductor oxides, the sensing mechanism
can be mainly induced by the oxygen adsorption on the surface of
the material leading to the resistance variation of the gas sensor.
When the CeO2eSnO2 sensor is exposed to air, oxygen molecules
can be adsorbed easily onto the surfaces of both the oxides. Espe-
cially, the presence of CeO2 nanoparticles onto the surface of SnO2
nanoparticles could lead to the formation of heterojunction inter-
face between two oxides. This may due to difference in their work
functions (4.69 eV for CeO2 and 4.90 eV for SnO2) [26,27]. As the
work function of SnO2 is higher than that of CeO2, the Fermi energy
level of SnO2 is lower than that of CeO2. As a consequence, the
lower energy conduction band from CeO2 stimulates the electron
transfer to SnO2, equalizing the Fermi energy level between them,
leading to the formation of depletion layer at CeO2 surface (due to
 K.R. Jawaher et al. / Journal of Science: Advanced Materials and Devices 3 (2018) 139e144
Fig. 5. Sensor responses of the SnO2, CeO2 and CeO2/SnO2 composite at different
working temperatures.
Fig. 6. Sensing response of the SnO2, CeO2 and CeO2/SnO2 composite towards n-
Butanol gas at different concentrations at 110
C.
Fig. 7. Sensing response of the SnO2, CeO2 and CeO2/SnO2 composite toward 100 ppm
concentration of various VOCs gases.
loss of electrons) and to the formation of an accumulation layer at
the surface of SnO2 (due to gain of electrons). Finally, the
enhancement of oxygen adsorption is found. Furthermore, the
accumulation layer can be depleted by subsequent oxygen
adsorption on the surface of SnO2, further increasing the potential
energy barrier at the interface can significantly enhance the sensor
143
Fig. 8. Variation of the sensor response with time of the SnO2, CeO2 and CeO2/SnO2
composite towards n-butanol gas.
response. When the CeO2eSnO2 sensor is exposed to reductive
VOCs gases, the gas molecules react with adsorbed oxygen species
and enormous amount of electrons will transfer into the conduc-
tion bands of the CeO2 and SnO2 simultaneously, decreasing the
height of the potential barrier and consequently increasing the
conductivity which eventually leads to the drastic improvement in
the sensitivity of the CeO2eSnO2 sensor.
4. Conclusion
A simple hydrothermal route was employed for the synthesis of
the CeO2eSnO2 nanocomposite. The XRD spectral analysis clearly
reveals the existence of both phases in the synthesized material.
The crystallite sizes of CeO2 and SnO2 nanostructures are estimated
to be 25.6 nm and 23.19 nm, respectively. The optical properties of
the CeO2eSnO2 nanocomposite suggest that the absorption edge of
the heterostructure is the contribution of both the components of
nanocomposites. The FESEM image clearly indicates the formation
of the spherical-like morphology with uniform agglomeration. The
gas sensing studies were recorded towards n-butanol, acetone,
ethanol, and isopropanol vapor at an operating temperature of
30e200
C. The maximum sensor response of CeO2eSnO2, SnO2
and CeO2 gas sensors were found upon exposure toward n-butanol
vapor at a 100 ppm concentration with the values of 75.6, 59.8 and
44.8, respectively, at an operating temperature of 110
C. As a result,
the CeO2eSnO2 nanocomposite exhibits a higher sensor response
and a good selectivity toward n-butanol gas. From the above
studies, it can be concluded that the CeO2eSnO2 nanocomposite is
a promising candidate for gas sensor application for the detection
of VOCs gases.
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