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本文采用水热法成功制备了Au纳米颗粒负载的WO3纳米花材料, 并运用XRD, SEM, TEM等手段对其晶体结构和形貌进行了表征, 并详细研究了其对二甲苯的气敏性能. 首先对Au的浓度和气敏元件的工作温度进行了优化, 结果表明, 0.4 μl Au纳米颗粒负载的WO3对二甲苯的灵敏度最高, 最佳工作温度为250 ℃. 同纯WO3相比, Au纳米颗粒负载的WO3纳米花具有更快的响应/恢复速度和更高的目标气体选择性, 在100 ppm二甲苯中灵敏度达到了29.5. 此外, 检测限度可以低至5 ppm水平. 最后对气敏元件表面可能发生的氧化还原反应的机理进行了研究和讨论, 认为Au负载的WO3纳米花材料有望应用于二甲苯气体传感器.Pure and Au nanoparticles loaded WO3 nanoflowers are synthesized by the hydrothermal method.The structures and morphologies of the as-prepared products are characterized by X-ray diffraction (XRD),scanning electron microswcope (SEM), and transmission electron microscope (TEM). The gas sensing performance of the Au/WO3 sensor to xylene is investigated. The Au content and the operating temperature are first optimized. It is found that WO3 with 0.4 μL Au nanoparticles shows the highest sensitivity at an operating temperature of 250 ℃. Compared with pure WO3, Au(0.4)/WO3 possesses fast response/recovery speed and high target gas selectivity. Its sensitivity to 100 ppm xylene is 29.5. Meanwhile, the practical detection limitation is as low as 0.5 ppm. Finally, the mechanism of Au/WO3 gas sensing is also proposed and discussed. Au nanoparticles loaded WO3 nanoflowers are considered to be a promising sensing material for detecting xylene pollutants.
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Keywords:
- WO3 /
- Au nanoparticles /
- xylene /
- gas sensing properties
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图 1 制备气敏传感器的实物图 (a)陶瓷管; (b)加热丝; (c)制备好的传感器; (d)底座; (e)外罩套环
Fig. 1. The photos of the gas sensor: (a) Ceramic tube; (b) heating wire; (c) prepared sensor; (d) base; (e) cover.
图 2 纯WO3和不同含量的Au负载的WO3复合体系的XRD图
Fig. 2. XRD pattern of pure WO3 and Au-loaded WO3 composites with different content of Au nanoparticles.
图 3 复合体系Au(0.4)/WO3的SEM (a)低倍和(b)高倍照片及(c) TEM和(d) HRTEM照片
Fig. 3. SEM (a) low magnification, (b) high magnification, (c) TEM and (d) HRTEM photograph of Au(0.4)/WO3 composites.
图 4 复合体系Au(0.4)/WO3的(a) W 4f和(b) Au 4f的X射线光电子能谱
Fig. 4. (a) W 4f and (b) Au 4f XPS spectra for Au(0.4)/WO3 composites.
图 5 (a)在不同操作温度下各个气体传感器对50 ppm二甲苯的的响应曲线; (b)在最佳操作温度时, 各个气体传感器对不同浓度二甲苯的响应曲线
Fig. 5. (a) Response curves of various gas sensors exposed to 50 ppm xylene at different operating temperatures; (b) response curves of various gas sensors to different concentrations of xylene at optimal operating temperatures.
图 6 250 ℃时Au(0.4)/WO3和纯WO3对50 ppm二甲苯的动态感应响应
Fig. 6. Dynamic response of Au(0.4)/WO3 and pure WO3 to 50 ppm xylene at 250 ℃.
图 7 (a) Au(0.4)/WO3和纯WO3样品在250 ℃, 50 ppm不同气体中的灵敏度; (b) Au(0.4)/WO3对50 ppm二甲苯的稳定性
Fig. 7. (a) Sensitivity of Au(0.4)/WO3 and pure WO3 samples to 50 ppm different gases at 250 ℃; (b) the stability evaluation of Au(0.4)/WO3 to 50 ppm xylene.
图 8 (a) WO3对二甲苯的气敏机理图; (b) Au/WO3的能带示意图
Fig. 8. (a) Gas-sensitive mechanism diagram of WO3; (b) the schematic diagram of the energy band in Au/WO3.
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[1] Zhang Y M, Zhao J H, Du T F, Zhu Z Q, Zhang J, Liu Q J 2017 Sci. Rep. 7 1960
Google Scholar
[2] Zhang F J, Qu G, Mohammadi E, Mei J G, Diao Y 2017 Adv. Funct. Mater. 27 1701117
Google Scholar
[3] Wang S, Li Q W, Yu H M, Li J Z 2018 Non-Ferrous Min. Metall. 34 39
[4] Gui Y H, Yang L L, Wang H Y, Li X M, Zhang H Z 2018 J. Synth. Cryst. 47 2115
[5] Li F, Guo S J, Shen J L, Shen L, Sun D M, Wang B, Chen Y 2017 Sens. Actuators, B 238 364
Google Scholar
[6] Rong X R, Chen D L, Qu G P, Li T, Zhang R, Sun J 2018 Sens. Actuators, B 269 223
Google Scholar
[7] Li Y X, Chen N, Deng D Y, Xing X X, Xiao X C, Wang Y D 2017 Sens. Actuators, B 238 264
Google Scholar
[8] Yildiz A, Crisan D, Dragan N, Iftimie N, Florea D, Mardare D 2011 J. Mater. Sci.- Mater. Electron. 22 1420
Google Scholar
[9] Su P G, Liao W H 2017 Sens. Actuators, B 252 854
Google Scholar
[10] Zhao S K, Shen Y B, Zhou P F, Zhong X X, Han C, Zhao Q, Wei D Z 2019 Sens. Actuators, B 282 917
Google Scholar
[11] Su X T, Li Y N, Jian J K, Wang J D 2010 Mater. Res. Bull. 45 1960
Google Scholar
[12] Shi J C, Hu G J, Sun Y, Geng M, Wu J, Liu Y F, Ge M Y, Tao J C, Cao M, Dai N 2011 Sens. Actuators, B 156 820
Google Scholar
[13] Righettoni M, Tricoli A, Gass S, Schmid A, Amann A, Pratsinis S E 2012 Anal. Chim. Acta 738 69
Google Scholar
[14] Wang C, Sun R, Li X, Sun Y F, Sun P, Liu F M, Lu G Y 2014 Sens. Actuators, B 204 224
Google Scholar
[15] Lv C, Wang M H, Liu Z Q, Liu Y K, Shen X Q 2018 J. Synth. Cryst. 47 1237
[16] Zhang H W, Wang Y Y, Zhu X G, Li Y, Cai W P 2019 Sens. Actuators, B 280 192
Google Scholar
[17] Kabcum S, Kotchasak N, Channei D, Tuantranont A, Wisitsoraat A, Phanichphant S, Liewhiran C 2017 Sens. Actuators, B 252 523
Google Scholar
[18] Ma J H, Ren Y, Zhou X R, Liu L L, Zhu Y H, Cheng X W, Xu P C, Li X X, Deng Y H, Zhao D Y 2018 Adv. Funct. Mater. 28 1705268
Google Scholar
[19] Comini E, Faglia G, Sberveglieri G, Pan Z W, Wang Z L 2002 Appl. Phys. Lett. 81 1869
Google Scholar
[20] Liu X H, Zhang J, Yang T L, Guo X Z, Wu S H, Wang S R 2011 Sens. Actuators, B 156 918
Google Scholar
[21] Vallejos S, Stoycheva T, Umek P, Navio C, Snyders R, Bittencourt C, Llobet E, Blackman C, Moniz S, Correig X 2011 Chem. Commun. 47 565
Google Scholar
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