气体传感器用Au掺杂WO<sub>3</sub>基复合涂层的组织及气敏性研究

摘要: 为了提高气体传感器的测试精度, 选择等离子喷涂工艺来制备Au掺杂WO₃基(WO₃/Au)复合涂层, 并对复合涂层的组织和气敏性展开分析。结果表明: 在WO₃/Au复合涂层的X射线衍射谱图上, 只观察到WO₃与Au对应的两种衍射峰, 没有出现其他物相的衍射峰; 相对于纯WO₃涂层, WO₃/Au复合涂层没有发生颗粒尺寸、结晶度与微观结构的显著改变; WO₃/Au复合涂层的吸脱附曲线发生了分离的现象, 出现了脱附滞后的情况。当温度上升, 气体传感器用纯WO₃涂层和WO₃/Au复合涂层都出现了响应值先升高到峰值又逐渐降低的现象, 其中最大值出现在300℃处; 不同于纯WO₃涂层, 气体传感器用WO₃/Au复合涂层可以实现对NO₂的快速响应, 并获得更短的恢复时间, 说明WO₃/Au复合涂层具备更优的气敏性。
- 等离子体喷涂 /
- WO₃涂层 /
- 掺杂 /
- 显微组织 /
- 气敏性
Abstract: To improve the accuracy of gas sensor, the Au-doped WO₃-based (WO₃/Au) composite coatings were prepared by the plasma spraying process, and the microstructure and gas sensitivity were analyzed. The results show that, only two diffraction peaks, corresponding to Au and WO₃, are formed in the X-ray diffraction patterns of the WO₃/Au composite coatings, and no other phase diffraction peaks are generated. Compared with the pure WO₃ coatings, the WO₃/Au composite coatings do not significantly change in the particle size, crystallinity, and microstructure. The separation phenomenon occurs in the desorption curve of the WO₃/Au coatings, which results in the desorption lag. When the temperature rises, the response values of the pure WO₃ coatings and the WO₃/Au composite coatings used in gas sensors rise to the peak and then gradually decrease, and the maximum value appears at 300℃. Compared with the pure WO₃ coatings, the WO₃/Au composite coatings used in gas sensors can achieve the rapid response to NO₂ and obtain the shorter recovery time, showing the better gas sensitivity of WO₃/Au composite coatings.
- plasma spraying /
- WO₃ coatings /
- doping /
- microstructure /
- gas sensitivity

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图 1 原材料微观组织：(a)Au纳米颗粒；(b)WO₃涂层

Figure 1. Microstructure of raw materials: (a)Au nanoparticles; (b)WO₃ coatings

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图 2 不同喷涂距离下所制备WO₃涂层的表面形貌：(a)150 mm; (b)175 mm; (c)200 mm

Figure 2. Surface morphology of the WO₃ coatings prepared the under different spraying distances: (a)150 mm; (b)175 mm; (c)200 mm

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图 3 WO₃/Au复合涂层X射线衍射图谱

Figure 3. XRD of the WO₃/Au composite coating

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图 4 WO₃/Au复合涂层的表面微观形貌：（a）低倍；（b）高倍

Figure 4. Surface morphology of the WO₃/Au composite coatings: (a)low magnification; (b)high magnification

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图 5 WO₃/Au复合涂层吸附‒脱附等温线及孔径分布曲线

Figure 5. Adsorption‒desorption isotherm and the pore size distribution of WO₃/Au composite coatings

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图 6 纯WO₃涂层和WO₃/Au复合涂层的孔径分布曲线

Figure 6. Pore size distribution of the pure WO₃ coatings and the WO₃/Au composite coatings

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图 7 纯WO₃涂层和WO₃/Au复合涂层传感器对NO₂的响应结果

Figure 7. Sensor response results to NO₂ gas of the pure WO₃coatings and the WO₃/Au composite coatings

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图 8 纯WO₃涂层和WO₃/Au复合涂层的NO₂气体响应电阻信号

Figure 8. NO₂ gas response resistance of the pure WO₃ coatings and the WO₃/Au composite coatings used in the gas sensor

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表 1 试验用化学试剂

Table 1. Chemical reagents used in experiment

试剂	制造商
WC₁₆, NH₃H₂O, Au	永华化学股份有限公司
C₂H₅O, C₃H₅O, HO(C₂H₄O)_nH	天津市恒兴化学试剂制造有限公司

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表 2 等离子体喷涂参数

Table 2. Plasma spraying parameters

编号	电流/A	电压/V	喷涂速度/(mL·min^-1)	喷涂距/mm
1	550	60	15	150
2	550	60	15	175
3	550	60	15	200

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表 3 WO₃/Au复合涂层能谱分析

Table 3. EDS analysis of WO₃/Au composite coatings

元素	质量分数/%	摩尔分数/%
O	46.86	68.62
Al	4.46	3.51
W	41.56	23.61
Au	7.12	4.26

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