Ionics (2021) 27:3647–3653

https://doi.org/10.1007/s11581-021-04057-2

ORIGINAL PAPER

Highly sensitive ethanol gas sensor based on In2O3 spheres

Chao Shen 1 & Ning Xu 2 & Rongfeng Guan 1 & Lu Yue 1 & Wenhui Zhang 1

Received: 14 January 2021 / Revised: 22 March 2021 / Accepted: 11 April 2021 / Published online: 1 June 2021
# The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2021

Abstract
In2O3 spheres were successfully prepared by nitric acid-assisted solvothermal method. The morphology and structure of the
products can be controlled by the content of nitric acid. After adding with nitric acid, the sensing performance of In2O3 has been
improved. In particular, the In2O3 spheres with partial broken structures prepared with 100 μL nitric acid show high response of
250 to 50 ppm ethanol at the operating temperature of 250 °C and exhibit good selectivity and stability.

Keywords In2O3 . Spheres . Materials preparations . Crystal structures . Sensors

Introduction methods. In2O3 morphology with cracked or broken configu-

ration possesses a high permeation for gas diffusion and is
In2O3 is widely used in various devices such as transparent beneficial to improve the gas-sensing properties. For example,
electrodes, gas sensors, photocatalysts, and solar cells due to Yang et al. prepared broken In2O3 microtubes using a chem-
its unique properties, such as wide band gap lower resistivity, ical conversion method, and they exhibited a significant re-
lower absorbance rate in the visible region, and prolific defects sponse toward triethylamine at 1–100 ppm and the lowest
on the surface. The stable phase of In2O3 is body-centered cubic detected concentration can reach 0.1 ppm [14]. Wei et al. re-
(c-In2O3) and the metal stable phase is rhombohedral (rh-In2O3). ported that 3.0 mol% La-doped In2O3 hollow microspheres
The band gap for c-In2O3 and rh-In2O3 are 2.93 ± 0.15 and 3.02 with some cracked architecture exhibited the high response
± 0.15 eV, respectively [1]. Particularly, In2O3 has been ac- toward 10 ppm hydrogen sulfide at 200 °C [15]. Hu et al.
knowledged as promising gas sensor materials for toxic and reported that CeO2-loaded In2O3 hollow spheres with some
harmful gas to our health and environment including formalde- broken structures exhibited enhanced gas-sensing response to
hyde [2], ethanol [3], and NO2 [4, 5] owing to its high electrical hydrogen gas at 160 °C [16]. Ding et al. prepared Ag-doped
conductance and the strong interaction with certain gas hollow urchin-like spheres In2O3 hierarchical nanostructures
molecules. with high response to NO2 [17].
The gas-sensing performance of In2O3 sensors is based on Herein, we report on a nitric acid-assisted solvothermal
their morphologies and structures. Until now, In2O3 nano- method for the synthesis of In2O3 spheres with partial broken
structures such as nanobelts [6], nanowires [7], nanosheets structures. Gas-sensing performance of the gas sensors based
[8], nanoplates [9], porous [10], nanoflowers [11], hollow on In2O3 spheres was systematically investigated. In addition,
[12], and hierarchical structure [13] have been obtained to structure and morphology of In2O3 were characterized and the
improve the gas-sensing properties by various synthesis effects of nitric acid on the gas-sensing property were also
investigated.

* Lu Yue
yuelu66@126.com
* Wenhui Zhang The experiment
zwhuizi000@sina.com

1
Key Laboratory for Advanced Technology in Environmental
Synthesis of In2O3
Protection of Jiangsu Province, Yancheng Institute of Technology,
Yancheng 224051, People’s Republic of China In a typical synthetic procedure, 0.1145 g In(NO3)3·4.5H2O
2
School of Mechanical Engineering, Yancheng Institute of was dispersed to 5 ml deionized water and 10 ml triethylene
Technology, Yancheng 224051, Jiangsu, China glycol. Then, nitric acid (0 μL, 50 μL, 100 μL, 150 μL, 400
3648 Ionics (2021) 27:3647–3653

μL) was added dropwise into the mixture solution with stir- the planar ceramic substrate with a space of 0.2 mm. The ceramic
ring. The solution was sealed in a 50 ml autoclave and heated substrate has a width, length, and thickness of 7, 13.4, and 1 mm,
at 180 °C for 12 h. After the reaction, when the autoclave was respectively. The sample was mixed with terpineol to form a paste,
cooled to room temperature, the products were collected by which was coated on the planar ceramic substrate and calcined in
centrifugation and washed several times with deionized water. air at 450 °C for 2 h. Finally, the fabricated sensor was aged in an
The products were dried at 80 °C for 2 h and then calcined in aging test chamber at 80 °C for 48 h and then pre-heated for 30 min
the furnace at 450 °C in the air for 2 h. until they reached a stable resistance at the operating temperature.
The sensor response to the test gas was defined as Ra/Rg, where Rg
Characterizations and Ra were the resistances of the sensors in target gases and in air,
respectively. The response and recovery times were defined as the
X-ray diffraction (XRD) was performed by PANalytical time taken by the sensor to achieve 90% of the total resistance
X’Pert3 Powder diffractometer. Scanning electron microscopy change in the case of adsorption and desorption, respectively. All
(SEM) was measured using scanning electron microscopy the measurements were carried out at room temperature under
(FEI Nova NanoSEM 450). Brunauer–Emmett–Teller (BET) atmospheric pressure.
surface areas were measured on an Autosorb-iQ-C-TCD ad-
sorption analyzer. Fourier-transform infrared (FT-IR) spectra
were recorded on a NEXUS-670 spectrometer from 4000 to Results and discussion
400 cm−1 at resolution of 4 cm−1. Zeta potential was measured
by a Nano ZS90 Zeta potential and molecular weight analyzer. The crystal structure of the samples was examined by XRD, as
shown in Fig. 2. All the diffraction peaks of the sample pre-
Gas-sensing measurements pared without nitric acid were assigned to the mixed phase of
c-In2O3 (JCPDS 06-0416) and rh-In2O3 (JCPDS 22-0336),
Gas-sensing properties were detected on a CGS-1TP gas-sensing and the main phase was rh-In2O3. After adding nitric acid,
measurement system (Beijing Elite Tech Co., Ltd.), which is the main phase of all samples converted to c-In2O3 (JCPDS
shown as Fig. 1a. The system offered an external temperature 06-0416), and the diffraction peaks of rh-In2O3 were very
control (from room temperature to 500 °C with a precision of 1 weak. It can be seen that the growth of rh-In2O3 was restrained
°C), which could conductively adjust the sensor temperature di- under acid environment.
rectly. Two probes were pressed on sensor substrates to export The effect of nitric acid content on the morphology was
electrical signals. The target gas was injected into the test chamber. investigated by SEM, as shown in Fig. 3. In the absence of
The target gas was mixed with air by two fans in the analysis nitric acid, the obtained sample was porous nanosheets with a
system. Fig. 1b displays the schematic representation of the planar width of about 340 nm. Further, 50 μL nitric acid was added,
ceramic substrate. Ag-Pd interdigital electrodes were preplaced on and the morphology was changed to spheres with a diameter
of about 470 nm and nanocubes tightly connected together
onto the sphere surface. When nitric acid was increased to
100 μL, the spheres grew bigger with a diameter of about
620 nm and was composed of many small nanoparticles,
and some spheres were broken, which was probably due to
the chemical etching of strong acid [18]. When nitric acid was
increased to 150 μL, spheres further grew bigger. When the
nitric acid was increased to 400 μL, the product was trans-
formed into agglomerated irregular sphere. Hence, nitric acid
was vital for the morphology of In2O3 spheres. Porous nano-
sheets were gradually etched to form spheres and some
spheres were broken, which was probably due to the chemical
etching of strong acid. Nitric acid also provided specific acidic
conditions for the hydrolysis of In3+ in a controllable manner.
The BET surface area for the sample prepared with 0, 50, 100,
150, and 400 μL nitric acid was 57.7, 46.7, 81.2, 49.8, and
60.6 m2/g, respectively.
Figure 4 shows the FT-IR spectra of the In2O3 precursor
prepared with 100 μL nitric acid before and after calcining.
Fig. 1 a Schematic representation of the planar ceramic substrate, b gas- Before calcining, the absorption peak at the wave number of
sensing measurement system 3500–3200 cm−1 corresponds to the stretching vibration of the
Ionics (2021) 27:3647–3653 3649

Fig. 2 XRD patterns of the

samples

Fig. 3 FE-SEM image of samples

prepared with a 0 μL; b 50 μL; c,
d 100 μL; e 150 μL; f 400 μL
nitric acid
3650 Ionics (2021) 27:3647–3653

100 250
0 l nitric acid
2265 50 l nitric acid
Transmittance (%)

1068 100 l nitric acid

80 200
1630 852 150 l nitric acid

Response (Ra/Rg)
1627 400 l nitric acid
60
784 150
3431 603
40 565
100
3388
1157
20 In2O3 precursor 501
In2O3 50
3124
3234 425
0
0
3500 3000 2500 2000 1500 1000 500 100 150 200 250 300
-1 o
Wavenumbers (cm ) Temperature ( C)
Fig. 4 FT-IR spectra of In2O3 precursor and In2O3 prepared with 100 μL Fig. 5 Response of the samples to 50 ppm ethanol at different operating
nitric acid temperatures

1000 ppm. It can be noticed from Fig. 6b that the response

O–H bond, and the absorption peak at 1627 cm−1 may be the increased as the ethanol concentration increased. The response
vibration absorption peak of the hydroxyl group of adsorbed of the sample using nitric acid was superior to the sample
water molecule, the strong absorption peak at 1200–780 cm−1 without nitric acid with increasing of ethanol concentration.
should be attributed to the In-OH deformed vibration absorp- In particular, In2O3 prepared with 100 μL nitric acid showed a
tion band, and the absorption peak at 501 cm−1 should be more pronounced response, probably due to its partial broken
attributed to the stretching vibration of In–O bond. After cal- sphere structure and highest surface areas for better adsorption
cining, the absorption peak at the wave number of 3431 cm−1 and desorption of ethanol.
corresponds to the stretching vibration of the O–H bond, and Figure 6c displays four representative reversible cycles of
the absorption peak near 1630 cm−1 may be the vibration samples to 50 ppm ethanol. It illustrated that this series of gas
absorption peak of the hydroxyl group of adsorbed water mol- sensors were well cycled and offer possibilities for the next
ecule, the three sharp absorption peaks at 425, 565, and 603 work. Fig. 6d shows the response of the samples to 50 ppm
cm−1 are the phonon vibration characteristic peaks of c- various gases or vapors at 250 °C. It can be seen that the
In2O3. The pH of the In2O3 precursor prepared with 100 sensor of In2O3 prepared with 100 μL nitric acid had highest
μL nitric acid before and after calcining was 4.0 and response to ethanol than other gases. Furthermore, compared
6.8, respectively. And the Zeta potential of the In2O3 to the sample without nitric acid, it showed more obvious high
precursor prepared with 100 μL nitric acid before and response to each gas. This demonstrates the sample showed
after calcining was 4.6 and − 6.9 mV. good selectivity when nitric acid was used.
The response of the sensors to 50 ppm ethanol as a function As a major factor in the performance of gas sensors, its useful
of the operating temperature is shown in Fig. 5. After adding life for sensor testing is an important measure of its further in-
nitric acid, the response of all the sensors was improved, and dustrialization. To investigate the stability of the sample prepared
the sample prepared with 100 μL nitric acid showed highest with 100 μL nitric acid, the response to 50 ppm ethanol at 250 °C
response to 50 ppm ethanol. In particular, the response of the over 30 days is indicated in Fig. 7. It can be clearly seen that even
sample prepared with 100 μL nitric acid reached 252 at 250 after 30 days of testing, the sensor response did not change much,
°C, which was about 10 times of the response (25) of the still maintaining high response to ethanol.
sensor without adding nitric acid. The response of the sensor Table 2 summarizes the gas-sensing properties of various
prepared with 100 μL nitric acid first increased with the op- In2O3 structures to ethanol in the literatures and present study.
erating temperature, reached highest at 250 °C, and then de-
creased at 300 °C. The response and recovery time of the
sample prepared with 100 μL nitric acid at different operating
Table 1 Response and recovery time of the sample prepared with 100
temperatures are shown in Table 1. The response and recovery μL nitric acid at different operating temperatures
time of the sample prepared with 100 μL nitric acid at 250 °C
was 16 and 14 s, respectively. The optimum operating tem- Operating temperature/°C 100 150 200 250 300
perature was around 250 °C. Response time/s 100 45 20 16 12
Figure 6a shows that the response of all the samples in-
Recovery time/s 80 60 30 14 8
creases rapidly as the ethanol concentration ranges from 5 to
Ionics (2021) 27:3647–3653 3651

Fig. 6 a Typical dynamic a

0 l nitric acid
1000 ppm b 1600 0 l nitric acid
1500
response curve of samples to 5– 50 l nitric acid
750 ppm
1400 50 l nitric acid
100 l nitric acid
100 l nitric acid
1000 ppm ethanol. b Response of

Response (Ra/Rg)
150 l nitric acid 1200 150 l nitric acid
1200 400 l nitric acid 400 l nitric acid
the samples to 5–1000 ppm etha-

Response (Ra/Rg)
500 ppm
1000
nol. c Response curve of samples 900
250 ppm 800
to 50 ppm ethanol at operating
temperature of 250 °C. d 600
on off
100 ppm 125 ppm
600

Response of the sample prepared 50 ppm 400

with 0 and 100 μL nitric acid to 300
200
25 ppm
various gases or vapors of 50 ppm 0
5 ppm

0
at operating temperature of 250 0 400 800 1200 1600 2000
0 200 400 600 800 1000
°C Time (s)
Volume (ppm)

0 l nitric acid
d 0 l nitric acid
250
c 300 50 l nitric acid
100 l nitric acid
100 l nitric acid
150 l nitric acid

Response (Ra/Rg)
400 l nitric acid
250 200
Response (Ra/Rg)

200 150

150 100

100
50

50
0

l
ne
ia
de

in

no
ol
e

yc ene
l

ne
no

en

on

m
xa

n
hy
to

pa
0

ha
ha

lu

nz

la
m

he
de
ce

To

ro
hy
Be
Et

et
lo
A

al
0 200 400 600 800

op
A

M
et
rm

Is
M
C
Fo
Time (s) Gases or vapors

Compared to previous reports, the In2O3 spheres in this work on an alkaline surface [26], CH3CHO may react with
showed a higher response to ethanol. the adsorbed oxygen ions on the sensor surface, and at
When the In2O3 sensor was placed in the air, oxygen the same time, the electrons are released back to the
molecules were absorbed on the surface of In 2 O 3 conduction band, resulting in a decrease in electrical
spheres, and electrons were trapped from the conduction resistance. The specific reaction process is shown in
band of the material to form chemisorbed oxygen ions the following equation [11].


O−2 ; O2− ; O− , resulting in an increase in electrical resis-
O2 ðgÞ↔O2 ðadÞ ð1Þ
tance. When ethanol gases (a kind of reducing gas) was


injected, the chemisorbed oxygen ions reacted with the O2 ðadÞ þ e‐ ↔ O−2 ; O2− ; O ðadÞ −
ð2Þ
ethanol molecule, C2H5OH is proved to be converted to
CH3CHO when In2O3 was used as the catalytic material C2 H5 OH↔CH3 CHO þ H2 ð3Þ

CH3 CHO ðadÞ þ 5O− ðadÞ↔2H2 O ðgÞ þ 2CO2 ðgÞ þ 5e− ð4Þ
250
In addition, we know that materials with a high specific
surface area are more advantageous for improving gas re-
200
sponse. The unique sphere structure of In2O3 using 100 μL
Response (Ra/Rg)

nitric acid not only provided a bonding site to absorb more

150 ethanol molecules but also provided an unobstructed path for
easy absorption and desorption of gas molecules. The gas-
100 sensing properties of metal oxides also depend on grain size,
porosity, lattice defects, active surface state, oxygen adsorp-
50
tion quantity, active energy of adsorption of the test gas on
their surface, and so on. The unique sphere structure of In2O3
using 100 μL nitric acid with partial broken structures may be
0
0 5 10 15 20 25 30 beneficial to the gas diffusion. The main phase of In2O3 was
Time (day) transformed from rh-In2O3 into c-In2O3 after adding nitric
acid, and the phase transformation may also lead to the change
Fig. 7 Long-term stability of the sample prepared with 100 μL nitric acid
to 50 ppm ethanol at operating temperature of 250 °C
of surface area. More detailed reason and qualitative
3652 Ionics (2021) 27:3647–3653

This study
Reference
explanation about the mechanism of interaction between eth-
anol and In2O3 need further investigation.

[11]

[20]

[24]
[19]

[21]
[22]
[23]

[25]
[3]
Conclusion

In summary, In2O3 spheres were prepared by nitric acid-

assisted solvothermal method. After adding nitric acid,
In2O3 nanosheets were changed into spheres, the main phase
of In2O3 was transformed from rh-In2O3 into c-In2O3, and the
Temperature (°C)

gas-sensing properties of In2O3 was improved. The In2O3

spheres with partial broken structures prepared with 100 μL
nitric acid showed highest response of 250 to 50 ppm ethanol
at the operating environment of 250 °C, short response-
250
235

260
320

200

200
320

250
210
280

recovery time (16 and 14 s, respectively), good selectivity,

cyclicity, and stability toward 50 ppm ethanol. The excellent
gas-sensing properties are mainly attributed to the spheres
with partial broken structures and relatively large surface area.
It is foreseeable that such In2O3 spheres assisted by nitric acid
are promising gas-sensitive materials in the field of gas
sensors.
Response

Funding This work was supported by the National Natural Science

32.6
24.4

11.7

250
185

Foundation of China (Nos. 51802276, 21878257).

30

28
22
24

23
Gas-sensing properties of various In2O3 structures to ethanol in the literatures and present study

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