SnO2/NiO复合半导体纳米纤维的制备及气敏性能研究

doi:10.15541/jim20200675

无机材料学报 ›› 2021, Vol. 36 ›› Issue (9): 950-958.DOI: 10.15541/jim20200675 CSTR: 32189.14.10.15541/jim20200675

SnO₂/NiO复合半导体纳米纤维的制备及气敏性能研究

储宇星¹(), 刘海瑞¹^,², 闫爽¹()

1.大连工业大学纺织与材料工程学院, 大连 116034
2.东北大学材料科学与工程学院, 沈阳 110819

收稿日期:2020-11-26 修回日期:2020-12-31 出版日期:2021-09-20 网络出版日期:2021-01-25
通讯作者: 闫爽, 讲师. E-mail: yanye150@outlook.com
作者简介:储宇星(1994-), 男, 硕士研究生. E-mail: 434611816@qq.com
基金资助:
辽宁省自然科学基金计划指导项目(2019-ZD-0129)

Preparation and Gas Sensing Properties of SnO₂/NiO Composite Semiconductor Nanofibers

CHU Yuxing¹(), LIU Hairui¹^,², YAN Shuang¹()

1. School of Textile and Materials Engineering, Dalian Polytechnic University, Dalian 116034, China
2. School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China

Received:2020-11-26 Revised:2020-12-31 Published:2021-09-20 Online:2021-01-25
Contact: YAN Shuang, lecturer. E-mail: yanye150@outlook.com
About author:CHU Yuxing(1994-), male, Master candidate. E-mail: 434611816@qq.com
Supported by:
Natural Science Foundation of Liaoning Province(2019-ZD-0129)

摘要/Abstract

摘要：

采用静电纺丝技术结合化学沉淀法和高温煅烧处理, 制备了具有不同Sn含量的SnO₂/NiO复合半导体纳米纤维。采用扫描电子显微镜(SEM), X射线衍射仪(XRD)和能量色散X射线光谱仪(EDS)对样品的形貌, 结构以及各元素含量进行表征。以乙醇为目标气体, 探究SnO₂/NiO纳米纤维的气体传感性质, 以及Sn含量对复合纳米纤维气敏性能的影响。研究结果表明, SnO₂/NiO复合纳米纤维具有三维网状结构, SnO₂复合对NiO纳米纤维的气敏性能具有明显的增强作用。随着SnO₂含量的增加, 复合纤维对乙醇气体的响应灵敏度增强, 其中响应最高的复合纳米纤维在最佳工作温度160 ℃条件下对体积分数为100×10^-6乙醇气体的响应灵敏度为13.4, 是NiO纳米纤维最大响应灵敏度的8.38倍。与市面常见的乙醇气体传感器MQ-3相比, SnO₂/NiO复合纳米纤维的最佳工作温度更低, 响应灵敏度更高, 具有一定的实际应用价值。

关键词: 氧化镍, 二氧化锡, 纳米纤维, 气敏性能, 复合材料

Abstract:

SnO₂/NiO composite semiconductor nanofibers with different Sn contents were prepared by electrospinning combined with chemical precipitation and high temperature calcination. Morphology, structure and elemental content of the samples were characterized. Taking ethanol as the target gas, the gas sensing properties of SnO₂/NiO nanofibers and the influence of Sn content on the gas sensing properties of the composite nanofibers were investigated. The results show that the SnO₂/NiO composite nanofibers have a three-dimensional network structure, and the SnO₂ composite can significantly enhance gas sensing properties of NiO nanofibers. With the increase of SnO₂ content in composite fibers, the response of samples to ethanol is enhanced. Among them, the SnO₂/NiO nanofibers with the highest sensitivity show response value of 13.4 to 100×10^-6 ethanol (volume fraction) at the optimum working temperature of 160 ℃. The maximum response value of the SnO₂/NiO nanofibers exhibits 8.38 times enhancement compared to that of NiO nanofibers. Compared with comercial MQ-3, a commonly used ethanol sensor, the SnO₂/NiO composite nanofibers have lower optimal working temperature and higher response sensitivity, which shows great potential in practical application.

Key words: nickel oxide, tin dioxide, nanofibers, gas sensitivity, composite materials

中图分类号:

TQ340
TP212

储宇星, 刘海瑞, 闫爽. SnO₂/NiO复合半导体纳米纤维的制备及气敏性能研究[J]. 无机材料学报, 2021, 36(9): 950-958.

CHU Yuxing, LIU Hairui, YAN Shuang. Preparation and Gas Sensing Properties of SnO₂/NiO Composite Semiconductor Nanofibers[J]. Journal of Inorganic Materials, 2021, 36(9): 950-958.

图/表 10

图1 SnO2/NiO NFs的制备机理示意图

Fig. 1 Preparation mechanism diagram of SnO2/NiO NFs

图2 (a)CNFs@Ni(OH)2和(b)NiO NFs的SEM照片

Fig. 2 SEM images of (a) CNFs@Ni(OH)2 and (b) NiO NFs

图3 (a, b)SnO2/NiO-1 NFs、(c, d)SnO2/NiO-2 NFs、(e, f)SnO2/NiO-3 NFs和(g, h) SnO2/NiO-4 NFs的SEM照片

Fig. 3 SEM images of (a, b) SnO2/NiO-1 NFs, (c, d) SnO2/NiO-2 NFs, (e, f) SnO2/NiO-3 NFs, and (g, h) SnO2/NiO-4 NFs

表1 NiO NFs和SnO2/NiO NFs样品中Ni和Sn元素的相对摩尔百分含量

Table 1 Relative molar percentages of Ni and Sn in NiO NFs and SnO2/NiO NFs samples

Sample	Ni/%	Sn/%
NiO NFs	100	0
SnO₂/NiO-1 NFs	76.79	23.21
SnO₂/NiO-2 NFs	25.46	74.54
SnO₂/NiO-3 NFs	0.51	99.49
SnO₂/NiO-4 NFs	0.08	99.92

图4 SnO2/NiO-1 NFs、SnO2/NiO-2 NFs、SnO2/NiO-3 NFs和SnO2/NiO-4 NFs的XRD图谱

Fig. 4 XRD patterns of SnO2/NiO-1 NFs, SnO2/NiO-2 NFs,SnO2/NiO-3 NFs, and SnO2/NiO-4 NFs

表2 SnO2/NiO NFs样品的晶粒尺寸(D)和晶界密度(δ)

Table 2 Respective grain size (D) and grainboundary density (δ) of SnO2/NiO NFs samples

Sample	Grain size, D/nm	Grain boundary density, $\delta $/(×10⁹, mm^-2)
SnO₂/NiO-1 NFs	11.1	8.12
SnO₂/NiO-2 NFs	7.4	18.46
SnO₂/NiO-3 NFs	6.3	25.16
SnO₂/NiO-4 NFs	6.3	25.16

图5 NiO NFs、SnO2/NiO-1 NFs、SnO2/NiO-2 NFs、 SnO2/NiO-3 NFs和SnO2/NiO-4 NFs在不同温度下对乙醇气体的灵敏度曲线(a), 在最佳工作温度下对体积分数为100×10-6乙醇气体的响应恢复曲线(b)

Fig. 5 (a) Sensitivity curves of NiO NFs, SnO2/NiO-1 NFs, SnO2/NiO-2 NFs, SnO2/NiO-3 NFs, and SnO2/NiO-4 NFs to ethanol gas at different temperatures, and (b) response recovery curve to 100×10-6 ethanol gas (volume fraction) at the optimal working temperature

图6 SnO2/NiO-1 NFs、SnO2/NiO-2 NFs、SnO2/NiO-3 NFs和SnO2/NiO-4 NFs对各种目标气体的选择性(100 mg/L)

Fig. 6 Selectivity of SnO2/NiO-1 NFs, SnO2/NiO-2 NFs, SnO2/NiO-3 NFs, and SnO2/NiO-4 NFs to various target gases(100 mg/L)

图7 SnO2/NiO-3 NFs和MQ-3在不同工作温度下对体积分数为100×10-6乙醇气体的灵敏度曲线(a), 最佳工作温度下对体积分数为100×10-6乙醇气体的响应恢复曲线(b)

Fig. 7 (a) Sensitivity curves of SnO2/NiO-3 NFs and MQ-3 to 100×10-6 ethanol gas at different working temperatures, and (b) response recovery curve to 100×10-6 ethanol gas at the optimal working temperature

表3 文献报道的部分SnO2基乙醇传感器特性与本工作的比较

Table 3 Comparison of the characteristics of some SnO2-based ethanol sensors reported in the literature with this work

Materials	Temperature/ ℃	Response/(100 mg·L^-1)	Ref.
Hierarchical SnO₂	300	24.1	[40]
ZnO-SnO₂ nanofibers	300	18.0	[41]
Horseshoe-shaped SnO₂	225	17.3	[42]
NiO-decorated SnO₂nanorods	300	30.0	[43]
SnO₂/NiO composite nanofibers	160	13.0	This work

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SnO₂/NiO复合半导体纳米纤维的制备及气敏性能研究

Preparation and Gas Sensing Properties of SnO₂/NiO Composite Semiconductor Nanofibers

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