醋酸钾溶液体系中α-Fe2O3纳米微球的离子液体辅助合成及气敏性能研究

doi:10.7503/cjcu20170804

高等学校化学学报 ›› 2018, Vol. 39 ›› Issue (8): 1631.doi: 10.7503/cjcu20170804

• 研究论文: 无机化学 • 上一篇下一篇

醋酸钾溶液体系中α-Fe₂O₃纳米微球的离子液体辅助合成及气敏性能研究

潘帅¹, 胡校兵¹, 宋润民¹, 解丽丽^1,², 朱志刚^1,²(), 郑嘹赢³

1. 上海第二工业大学工学部环境与材料工程学院, 上海 201209
2. 上海材料创新研究院, 上海 200444
3. 中国科学院上海硅酸盐研究所, 上海 200050

收稿日期:2017-12-11 出版日期:2018-08-10 发布日期:2018-04-28
作者简介:联系人简介: 朱志刚, 男, 博士, 教授, 主要从事智能传感材料与器件研究. E-mail: zgzhu@sspu.edu.cn
基金资助:
国家自然科学基金(批准号: 61471233)、上海高校特聘教授(东方学者)计划、中国科学院无机功能材料与器件重点实验室开放课题(批准号: 201602)和上海第二工业大学研究生项目(批准号: EGD16YJ022)资助.

Ionic Liquid Assisted Synthesis of α-Fe₂O₃ Nanospheres Based on Potassium Acetate Solution and Their Gas-sensing Properties^†

PAN Shuai¹, HU Xiaobing¹, SONG Runmin¹, XIE Lili^1,², ZHU Zhigang^1,^2,^*(), ZHENG Liaoying³

1. School of Environmental and Materials Engineering, College of Engineering,Shanghai Polytechnic University, Shanghai 201209, China
2. Shanghai Innovation Institute for Materials, Shanghai 200444, China
3. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

Received:2017-12-11 Online:2018-08-10 Published:2018-04-28
Contact: ZHU Zhigang E-mail:zgzhu@sspu.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(No.61471233), the Program for Professor of Special Appointment(Eastern Scholar) at Shanghai Institations of Higher Learning, the Open Project Program of Key Laboratory of Inorganic Functional Materials and Devices of Chinese Academy of Sciences, China(No.201602) and the Graduate Program Foundation of Shanghai Polytechnic University, China(No.EGD16YJ022).

摘要/Abstract

摘要：

以FeCl₃·6H₂O和CH₃COOK为反应物, 以离子液体1-丁基-3-甲基咪唑氯化物([Bmim]Cl)为结构导向剂和表面活性剂, 采用水热合成法在150 ℃反应8 h制备出结晶度好、形貌规整, 直径为10~30 nm的α-Fe₂O₃纳米微球. 考察了[Bmim]Cl的添加量对氧化铁形貌和气敏性能的影响. 气敏性能测试结果表明: 当离子液体添加量为12 mmol时, α-Fe₂O₃纳米微球对乙醇的气敏性能最佳. 在工作温度为300 ℃时, 对50 μL/L乙醇的灵敏度达到7.56, 是不添加离子液体时制备的α-Fe₂O₃的5.6倍, 在10~200 μL/L的检测范围内灵敏度与浓度具有良好的线性关系(R=98.8%), 并且具有良好的选择性和稳定性. 本文还详细探讨了α-Fe₂O₃纳米微球对乙醇的敏感机理, 以及工作温度对其气敏性能的影响.

关键词: 水热合成法, 氧化铁, 离子液体, 气敏性能

Abstract:

α-Fe₂O₃ nanospheres with good crystallinity and uniformity, diameter of 10—30 nm were synthesized from FeCl₃·6H₂O and CH₃COOK with 1-butyl-3-methylimidazolium chloride([Bmim]Cl) as ionic liquid structure-based agent and surfactant by hydrothermal method at a constant temperature of 150 ℃ for 8 h. The effects of different amounts of [Bmim]Cl on the formation of iron oxide and its gas sensing properties were investigated. The gas-sensing results show that α-Fe₂O₃ nanospheres exhibit the best gas-sensing properties to ethanol when the amount of ionic liquid is 12 mmol. When the working temperature is 300 ℃, the sensitivity of as-prepared α-Fe₂O₃ nanospheres to 50 μL/L ethanol is 7.56, which is 5.6 times that of α-Fe₂O₃ generated without ionic liquid. There is also a good linear relationship(R=98.8%) in the range of 10—200 μL/L, and the sensor has good selectivity and stability. In addition, the gas-sensing mechanism of α-Fe₂O₃ nanospheres to ethanol, and the influence of operating temperature on its gas-sensing properties were discussed in detail.

Key words: Hydrothermal method, Iron oxide, Ionic liquid, Gas-sensing

中图分类号:

O614.81

TrendMD:

潘帅, 胡校兵, 宋润民, 解丽丽, 朱志刚, 郑嘹赢. 醋酸钾溶液体系中α-Fe₂O₃纳米微球的离子液体辅助合成及气敏性能研究. 高等学校化学学报, 2018, 39(8): 1631.

PAN Shuai, HU Xiaobing, SONG Runmin, XIE Lili, ZHU Zhigang, ZHENG Liaoying. Ionic Liquid Assisted Synthesis of α-Fe₂O₃ Nanospheres Based on Potassium Acetate Solution and Their Gas-sensing Properties^†. Chem. J. Chinese Universities, 2018, 39(8): 1631.

图/表 9

Fig.1 Gas sensor preparation process based on α-Fe2O3 nanospheres and the test system

Fig.2 XRD patterns of α-Fe2O3 nanospheres prepared with different amounts of ionic liquid(A) and FTIR spectra of S-0(a), S-4(b) and [Bmim]Cl(c)(B)(A) a. S-0; b. S-1; c. S-2; d. S-3; e. S-4; f. S-5.

Fig.3 SEM images of α-Fe2O3 nanospheres prepared with different amounts of ionic liquid (A) S-0; (B) S-1; (C) S-2; (D) S-3; (E) S-4; (F) S-5.

Fig.4 N2 adsorption-desorption isotherms and pore size distribution(inset) of samples S-0(A) and S-4(B)

Fig.5 Temperature-dependent gas sensing response(A) and response-recovery curves(B) of different α-Fe2O3 nanospheres to 50 μL/L ethanol gasa. S-0; b. S-1; c. S-2; d. S-3; e. S-4; f. S-5. Inset of (B) shows tres and trec of S-4.

Fig.6 Dynamic response transient(A) and sensitivity-ethanol concentration plot(B) for the gas sensor based on sample S-4 at 300 ℃

Fig.7 Stabiliity test of sample S-4 at operating temperature of 300 ℃ to 10 μL/L ethanol(A) and response sensitivity for sample S-4 to different gases at operating temperature of 300 ℃(B) (B) a. C2H5OH; b. CH3COH3; c. H2S; d. NH3; e. NO; f. Cl2; g. NO2.

Fig.8 Reaction mechanism of α-Fe2O3 nanospheres exposed to ethanol gas

Fig.9 Reaction mechanism of α-Fe2O3 nanospheres exposed to ethanol gas at different operating temperatures

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醋酸钾溶液体系中α-Fe₂O₃纳米微球的离子液体辅助合成及气敏性能研究

Ionic Liquid Assisted Synthesis of α-Fe₂O₃ Nanospheres Based on Potassium Acetate Solution and Their Gas-sensing Properties^†

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