Cr-Doped Hollow In2O3
Cr-Doped Hollow In2O3
Cr-Doped Hollow In2O3
⁎ ⁎
Jing Sun a, Yanzheng Wang b, Peng Song a, , Zhongxi Yang a, Qi Wang a,
a
School of Material Science and Engineering, University of Jinan, Jinan 250022, China
b
Shandong Academy of Building Research Co., LTD, China
a r t i cl e i nfo a bstr ac t
Article history: Transition metal ions doping is an effective method to improve the gas sensing performance of metal oxide
Received 21 December 2020 semiconductors. Herein, we report the synthesis of Cr-doped In2O3 samples by calcining metal-organic
Received in revised form 13 May 2021 frameworks (MOFs)-precursors prepared by a simple oil bath method. The experimental characterization
Accepted 17 May 2021
results show that the as-prepared samples exhibit uniform hollow nanoboxes with large specific surface
Available online 20 May 2021
areas. Through comparison, the 0.5 wt% Cr-doped In2O3 sample with complete and regular morphology was
selected for a series of gas-sensitive performance tests. The results show that the sensor has good detection
Keywords:
Indium oxide performance for ammonia (NH3). Gas-sensing tests revealed that the sensor exhibited excellent sensing
Cr-doping performance towards NH3 with low operating temperature (140 °C), high selectivity, good repeatability,
Nanobox relatively high response, low detection concentration (~ 1 ppm), and short response time (~ 1 s). The
Metal-organic framework generation of lattice defects and the increased conductivity after doping are the reasons for the excellent
Gas sensor performance of the sensor. This provides a new strategy for the research and preparation of high perfor
Ammonia mance gas sensors.
© 2021 Elsevier B.V. All rights reserved.
1. Introduction However, sensors made solely from pure In2O3 often exhibit pro
blems such as high operating temperatures, high detection limits,
In recent years, environmental pollution has become more and and low response values. To some extent, the application of indium
more serious. As a toxic gas pollutant, ammonia has caused wide oxide gas sensors is limited, so doping [15], compounding [16] or
spread concern [1,2]. Ammonia is a colorless gas with strong pun noble metal modification [17] is performed to improve the gas
gent odor. It is easy to liquefy and can be directly synthesized from sensitivity performance. Similarly, the preparation of nano-scale
nitrogen and hydrogen. Ammonia irritates the respiratory tract and samples is also conducive to the detection of gases [18–21].
corrodes the skin [3,4], and exposure to high concentrations of Metal-organic framework materials are composed of metal cations
ammonia may cause death. Due to ammonia is used in many ways, (divalent, trivalent, and tetravalent) and organic ligand molecules [22].
real-time monitoring of its concentration is particularly important. MOFs with different structures can be obtained by using different
As indicated in literatures that people should not be exposed to metal ions and organics, which is also in line with a major advantage
25 ppm ammonia atmosphere for more than 8 h or 35 ppm for more of MOFs – the controllable structure. At the same time, because of the
than 10 min [5–7]. Consequently, accurate detection of ammonia is developed pore structure, open active sites, and high specific surface
essential to protect human health. In the field of gas sensing, metal area [23,24], MOFs have been applied in more and more fields, espe
oxides (MOS) have become a suitable material for the detection of cially gas detection and chemical sensing that are closely related to
toxic gases due to their advantages such as low production cost [8], human health [25]. Take an example, Wei et al. synthesized MOF-
small size [9], and long service life [10] compared to other materials. derived rGO/α-Fe2O3 nanocomposites with the simple solvothermal
As a typical n-type semiconductor with a wide bandgap [11–14], method, which reveal high-performance, excellent selectivity and
In2O3 shows very superior application in the field of gas sensing. quick response-recovery on triethylamine gas [26]. For instance,
Drobek et al. uniformly covered the ZIF-8 molecular sieve membrane
on the surface of ZnO nanowires. Alarmingly, the ZnO@ZIF-8-based
nanocomposite sensor prepared in this way exposed excellent se
⁎
Corresponding authors. lectivity for H2 in comparison with the pristine ZnO nanowires sensor
E-mail addresses: mse_songp@ujn.edu.cn (P. Song),
mse_wangq@ujn.edu.cn (Q. Wang).
[27]. In view of this, the preparation of metal oxides using MOFs as
https://doi.org/10.1016/j.jallcom.2021.160472
0925-8388/© 2021 Elsevier B.V. All rights reserved.
J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
precursors or the combination of MOS and MOFs structure may have a pure In2O3 to acetone gas [28]. The Cr doped WO3 nanofibers syn
promising effect on improving gas sensing performance. thesized by Zhu et al. can detect 3-hydroxy-2-butanone biomarker
Studies have also shown that doping rare earth elements or with a concentration as low as 0.05 ppm, indicating that the sensor
transition metal elements can effectively enhance the gas sensing prepared from this material is extremely promising, and provides
performance of metal oxides. For example, Wei et al. prepared Ce- new ideas for cheaper and portable 3H-2B detection devices [29].
doped hierarchical flower-like In2O3 microspheres by hydrothermal Meanwhile, it is also a good method to prepare nano-scale samples.
method and tested their gas-sensitive properties. The results in Now some people have prepared MOF-derived In2O3 hollow mi
dicate that Ce-doped In2O3 exhibited a much higher response than crotubes [30–32], which have also been studied in the direction of
Fig. 3. (a) XRD patterns of pure In2O3 and Cr-doped In2O3 hollow nanoboxes with different doping levels; (b) partial enlarged detail in the range of 28°–53°.
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Fig. 4. (a, b) SEM images of pure In2O3 hollow nanoboxes; (c, d) SEM images of 0.25 wt% Cr-doped In2O3 hollow nanoboxes; SEM images of 0.5 wt% Cr-doped In2O3 hollow
nanoboxes; (g, h) SEM images of 1 wt% Cr-doped In2O3 hollow nanoboxes.
gas sensing. But their length is about tens of microns, and the spe is smaller than In3+ (0.08 nm), the doping of Cr3+ to replace the po
cific surface area is large. On the basis, it is necessary to improve the sition of In3+ in the unit cell and the occurrence of lattice distortion are
experimental scheme and reduce the sample size. the reasons for improving the sensitivity. In the following, the gas
In the paper, we use a simple oil bath method to prepare the sensing mechanism of Cr-doped In2O3 will be explained.
precursor nanoboxes, and obtained Cr-doped In2O3 hollow nanoboxes
by calcining them. After comparing the structure and morphological 2. Experimental
characterization of samples with different doping amounts, we se
lected samples with a Cr doping amount of 0.5 wt% for gas-sensitivity 2.1. Preparation of precursor nanoboxes and Cr-doped In2O3 hollow
testing. The results indicate that 0.5 wt% Cr-doped In2O3 show ex nanoboxes
cellent gas sensing response to 10 ppm ammonia at 140 °C. In addition,
the sample exposed quick response-recovery and low detection limit In the typical process, 160 mL N, N-dimethylformamide was
(can detect 1 ppm ammonia). Since the ion radius of Cr3+ (0.0615 nm) measured and transferred into a 250 mL beaker labeled A, then
Fig. 5. (a) EDS energy spectrum diagram of 0.5 wt% Cr-doped In2O3 hollow nanoboxes; (b–d) EDS mapping images of 0.5 wt% Cr-doped In2O3 hollow nanoboxes.
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Fig. 6. (a, b) TEM image of 0.5 wt% Cr-doped In2O3 hollow nanoboxes; (c) high-resolution TEM image of 0.5 wt% Cr-doped In2O3 hollow nanoboxes.
0.0730 g 1,4-benzenedicarboxylic acid and 0.0700 g Indium nitrate therein was poured out. The powder was collected by centrifugation
hydrate was dissolved in the N, N-dimethylformamide that has been and washing 3 times with absolute ethanol or deionized water, thus
measured. In addition, 200 mL N, N-dimethylformamide was mea we can obtain the precursor nanoboxes. Finally, Cr-doped In2O3
sured and transferred into a 250 mL beaker labeled B, then 200 mg hollow nanoboxes are obtained by calcining the precursor nano
Chromium nitrate nonahydrate was added in the N, N-di boxes at 400 °C for 3 h in air atmosphere. The growth process of the
methylformamide. Ultimately, measure a certain amount of solution Cr-doped In2O3 hollow nanoboxes is shown in the Fig. 1.
from the B beaker (the corresponding Cr doping amounts are 0.25,
0.5 and 1 wt%) and transfer it into the A beaker, and stir until well. 2.2. Characterization
Pure samples can be prepared without adding chromium nitrate
solution. The Powder X-ray diffractometer (XRD, Bruker D8 Advance) was
Subsequent to this procedure, A beaker was placed in an oil bath used to determine the crystal structure of the sample. The micro
for heating and heated to 120 °C for 30 min. After reaction, the A scopic morphology of the sample was characterized by a field
beaker was slowly cooled to room temperature and the mixture emission scanning electron microscope (FESEM, FEI Company,
Fig. 7. (a–d) Pore-size distribution (inset) and N2 adsorption-desorption isotherm of pure and 0.25, 0.5, 1 wt% Cr-doped In2O3 hollow nanoboxes.
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Fig. 8. XPS spectra of 0.5 wt% Cr-doped In2O3 hollow nanoboxes: (a) survey spectrum, (b) In 3d spectrum, (c) Cr 2p spectrum.
QUANTA FEG 250). The element mapping spectra was exported also measured by a UV–vis (UV–vis, SHIMADZU UV-3600) spectro
through the FESEM attachment. In order to obtain high-magnifica photometer.
tion images and the interplanar spacing of the sample, a transmis
sion electron microscope (TEM, Hitachi H-800) was used for further 2.3. Sensor fabrication and test
testing. X-ray photoelectron spectroscopy (XPS, Thermo Scientific
Escalab 250Xi) can determine the valence state and proportions of The production process of the gas sensor is shown in Fig. 2. First
elements. The specific surface area of the sample is calculated using of all, take an alumina ceramic tube with four platinum wires (length
the Brunauer–Emmett–Teller (BET) method, which depends on N2 7 mm, diameter 1.5 mm) using tweezer, unfold the platinum wire
adsorption-desorption isotherms (Micromeritics Instrument Corp., with another tweezer, and connect the platinum wire to the com
ASAP2460). Photoluminescence (PL) spectra were characterized on a ponent base with conductive silver paste. Afterwards, insert a small
PL spectrophotometer (Hitachi Model F-7000). The band gaps were Ni-Cr alloy coil into the ceramic tube, and also connect it to the base.
Fig. 9. (a) Sensor response of pure In2O3 and Cr-doped In2O3 hollow nanoboxes to 10 ppm ammonia gas corresponds to the operating temperature (100–200 °C); (b) Dynamic
response-recovery curve (10 ppm ammonia) of pure In2O3 at 160 °C and 0.5 wt% Cr-doped In2O3 hollow nanoboxes at 140 °C; (c) Response and recovery curves and the stability of
the sensors based on pure In2O3 and 0.5 wt% Cr-doped In2O3 hollow nanoboxes exposure to 10 ppm ammonia at 160 °C and 140 °C, respectively; (d) Concentration-dependent
response curves of pure In2O3 and 0.5 wt% Cr-doped In2O3 hollow nanoboxes sensors to 1–50 ppm ammonia.
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Fig. 10. (a) Sensor responses to different gases (10 ppm) of 0.5 wt% Cr-doped In2O3 hollow nanoboxes sensor at 140 °C; (b) Long-term stability of 0.5 wt% Cr-doped In2O3 hollow
nanoboxes sensor on successive exposure to 10 ppm ammonia at 140 °C.
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Fig. 11. Schematic diagrams for possible gas sensing mechanism of Cr-doped In2O3 hollow nanoboxes.
addition, Fig. 5(d) further proves the presence of Cr in the sample. It 444.3 eV and 531.3 eV, corresponding to In 3d5/2 and In 3d3/2 [34,39].
can be seen that Cr is very uniformly distributed in the resulting Moreover, the XPS spectrum of Cr 2p is depicted in Fig. 8(c). It il
product, indicating that Cr successfully entered the In2O3 lattice. In lustrates that the Cr 2p2/3 at 576.2 eV and Cr 2p2/3 at 586.1 eV, thus
order to observe the morphological structure at a more microscopic determining the valence state of the dopant as Cr3+ [40].
scale, the samples need to be tested by TEM.
As indicated in the TEM images of 0.5 wt% Cr-doped In2O3 sam 3.2. Gas sensing properties
ples (Fig. 6(a and b)), it can be observed that the hollow structure of
the nanobox and the wall of the nanobox is found to be very thin, The sensor was made using all samples. It is well known that
only about 36 nm. The thickness of the entire nanobox is approxi operating temperature is a principal factor to affect the response of
mately 660 nm. The hollow structure is conducive to gas diffusion the sensor. Fig. 9(a) presents the responses of sensors to 10 ppm
and transmission, so it can produce high gas sensitivity. According to ammonia at various operating temperatures, the responses were
the HRTEM images (Fig. 6(c)) we can clearly see that the interplanar measured in the range of 100–200 °C with 20 °C as interval. It is clear
spacing exposed by Cr-doped In2O3 hollow nanobox was 0.308 nm, that as the temperature increases, the response of sensor experience
and it was found that it matches well with the (222) crystal plane by a climb firstly and then decreases gradually. Among them, the sensor
comparing with In2O3 standard card. prepared from the 0.5 wt% Cr-doped In2O3 shows the best perfor
The Brunauer–Emmett–Teller (BET) method was usually used to mance for ammonia, and has a response value of 11.11 at 140 °C,
calculate the specific surface area of the material. The Fig. 7(a–d) which is higher than sensors based on other samples (the sensitivity
indicates that the pore-size distribution (inset) and N2 adsorption- of the pure In2O3 sensor is 3.9, the sensitivity of the 0.25 wt% Cr-
desorption isotherm, respectively. The N2 adsorption-adsorption doped In2O3 sensor is 9.2, the sensitivity of the 1 wt% Cr-doped In2O3
isotherm could be appeared as typical type IV isotherm which sensor is 8.8, and the optimum working temperature for the pure
shown that the obtained samples contained the mesoporous struc In2O3 sensor and 0.25 wt% Cr-doped In2O3 sensor is 160 °C). This is
ture [37,38]. The Brunauer–Emmett–Teller surface areas of the pure because at the optimum operating temperature, the adsorbed
In2O3, 0.25, 0.5 and 1 wt% Cr-doped In2O3 hollow nanoboxes were oxygen on the surface of the material has sufficient capacity to
calculated to be 46.4, 66.7, 51.3 and 58.2 m3/g. At the same time, in participate in the reaction. When the temperature is lower than the
the figure of pore-size distribution, it can be obtained that the pore optimal temperature, the surface activity of the material is low and
sizes with the largest volume ratio are located at 6.68, 6.26, 5.79, and the amount of adsorbed oxygen that can react with ammonia is
4.53 nm. For MOF-derived oxides, the volatilization of organics small. If the temperature exceeds the optimal temperature, the
during the calcination process is responsible for its large specific desorption rate eventually exceeds the adsorption rate, resulting in a
surface area. When the specimen are used for gas sensing, this high decrease in the amount of adsorbed oxygen, which leads to the
specific surface area can promote gas diffusion, adsorption and decrease in sensitivity [26]. It is worth noting that compared with
desorption process. Therefore, we can infer that the Cr-doped In2O3 pure In2O3 sensors, the optimal operating temperature has dropped
hollow nanoboxes structure derived from MOF are highly likely to from 160 °C to 140 °C, and the sensitivity to ammonia has also been
possess great gas sensing performance. greatly improved.
To further explore the chemical state of the elements, the sam As shown in Fig. 9(b), we plot the typical response/recover curve
ples were subjected to XPS analysis. From the full survey spectrum toward 10 ppm ammonia at 140 °C. In this situation, the results show
(Fig. 8(a)), only three elements present in the as-prepared samples. that the sensor based on the 0.5 wt% Cr-doped In2O3 has rapid re
In Fig. 8(b), there are two peaks where the binding energy is sponse (1 s)/recover times (18 s).
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Fig. 12. O 1s spectra of (a) pure In2O3 hollow nanoboxes, (b) 0.25 wt% Cr-doped In2O3 hollow nanoboxes, (c) 0.5 wt% Cr-doped In2O3 hollow nanoboxes and (d) 1 wt% Cr-doped
In2O3 hollow nanoboxes; (e) Room-temperature PL spectra pure In2O3 and 0.5 wt% Cr-doped In2O3 hollow nanoboxes; (f) UV–vis diffuse reflectance spectra of pure In2O3 and
0.5 wt% Cr-doped In2O3 hollow nanoboxes.
We can reach conclusion that the Cr-doped In2O3 gas sensor shows the dynamic response curve to ammonia with concentra
displays excellent reproducibility from three reversible cycles of tions of 1–50 ppm. Visibly, as the gas concentration increases, the
response-recovery curve (Fig. 9(c)) which is due to the maximum sensitivity also gradually increases. The sensor has a sensitivity of
response value under 10 ppm ammonia. 2 when bathed at a gas concentration of 1 ppm, proving that the
At the optimum temperature, the sensitivity of Cr-doped In2O3 Cr-doped In2O3 gas sensor can detect lower concentrations of
to different concentrations of ammonia gas can be tested. Fig. 9(d) ammonia. When the sensor is at 50 ppm test gas, the sensitivity
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
2NH3 + 3O− → N2 + 3H2O + 3e− (4) Jing Sun: Writing - original draft, Methodology, Investigation.
Normally, the resistance will gradually return to the initial value Yanzheng Wang: Validation, Formal analysis. Peng Song: Writing -
after the target gas reaction ends. review & editing, Resources. Zhongxi Yang: Project administration.
Qi Wang: Supervision, Funding acquisition.
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J. Sun, Y. Wang, P. Song et al. Journal of Alloys and Compounds 879 (2021) 160472
Declaration of Competing Interest [22] X.F. Wang, X.Z. Song, K.M. Sun, L. Cheng, W. Ma, MOFs-derived porous nano
materials for gas sensing, Polyhedron 152 (2018) 155–163.
[23] Y.S. Liu, H. Jiang, J.Y. Hao, Y.L. Liu, H.B. Shen, W.Z. Li, J. Li, Metal-organic frame
The authors declare that they have no known competing fi workderived reduced graphene oxide-supported ZnO/ZnCo2O4/C hollow nano
nancial interests or personal relationships that could have appeared cages as cathode catalysts for aluminum-O2 batteries, ACS Appl. Mater.
to influence the work reported in this paper. Interfaces 9 (2017) 31841–31852.
[24] J.N. Zhang, H. Lu, L.Z. Zhang, D.Y. Leng, Y.Y. Zhang, W. Wang, Y. Gao, H.B. Lua,
J.Z. Gao, G.Q. Zhu, Z.B. Yang, C.L. Wang, Metal–organic framework-derived ZnO
Acknowledgment hollow nanocages functionalized with nanoscale Ag catalysts for enhanced
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This work was financially supported by National Natural Science MOF-derived hierarchical hollow ZnO nanocages with enhanced low-con
Foundation of China (No. 61102006), and Natural Science Foundation centration VOCs gas-sensing performance, Sens. Actuators B Chem. 225 (2016)
of Shandong Province, China (Nos. ZR2018LE006 and ZR2015EM019). 158–166.
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