【作者】 徐艳；

【导师】 唐一科；

【作者基本信息】 重庆大学 ， 机械电子工程， 2006， 硕士

【摘要】 三氧化钨(WO3)薄膜是一种重要的功能材料,因具有良好的电致变色、气致变色、光致变色、电化学性能而得到广泛的研究和应用,尤其是其气致变色性能在气体传感器方面有广阔的应用前景。由于三氧化钨薄膜在常温下对氢气不敏感,本文采用掺杂改性来改善三氧化钨薄膜材料的氢敏性能,分别采用直流磁控溅射法和溶胶凝胶法制备了均匀的三氧化钨掺铂和掺钯薄膜材料,并对它的光学性质、表面形态、结构等进行了深入的研究。首先简要概述了三氧化钨掺杂薄膜的氢敏机理及发展现状,其次详细介绍了掺杂薄膜的制备方法、使用的材料设备及工艺流程。然后对制作出的各种条件的薄膜进行性能测试,并一一作了比较,最后对影响薄膜性能的重要因素作了细致分析。本文分别用X衍射仪、隧道-原子力显微镜、傅立叶变换红外光谱仪、双束紫外可见分光光度计、快速伏安循环法等表征了用以上两种方法制备的三氧化钨掺杂薄膜。X衍射结果表明:磁控溅射掺铂薄膜样品在400℃退火处理后得到的谱图中出现明显尖锐衍射峰,说明已经是晶态;溶胶掺铂和掺钯薄膜样品在400℃退火后得到的谱图中没有尖锐的衍射峰,说明此时样品还呈非晶态,在460℃退火处理后有半峰宽较大的晶体衍射峰,溶胶掺杂样品的晶化温度有所提高,其原因还待进一步研究。隧道-原子力显微镜测试结果表明:非晶态时,磁控溅射掺铂薄膜样品表面和溶胶凝胶掺铂样品表面都有明显的平行线状结构,长程无序,分子趋于四面体结构,只是前者比后者表面较平整;晶态时,磁控掺铂样品在自然生长面上原子呈平面分布,长程有序,溶胶掺铂样品则呈WO6面心结构。傅立叶变换红外光谱仪测试结果表明:掺钯三氧化钨凝胶粉体的特征振动在400～1000nm波段内随退火温度的提高越明显。透光率测试结果表明:掺铂的样品比掺钯的样品具有更好的氢敏效应,溶胶掺铂样品又比磁控掺铂样品具有更快的氢响应速度,但其对同一氢浓度透光率减少量相同,即达到相同的氢原子吸附-抽出平衡态。快速伏安循环法测试结果表明:溶胶掺钯样品具有良好的电致变色性能,其着色态与退色态的透光率变化约60%。这两种方法结合制备的三氧化钨掺杂薄膜中溶胶掺铂样品综合了溶胶凝胶法与直流磁控溅射法的优点,其薄膜疏松多孔,充分快速响应了铂催化剂离化的氢,具有良好的氢敏性能,是制备氢气传感器薄膜的首选方法。更多还原

【Abstract】 Tungsten oxide film material is a important functional material. It is studied and applied extensively because of its electrochromic property, gasochromic property, photochromic property, electrochemistry, etc. Especially gasochromic property is applied to gas sensors extensively. Because of it is not sensitive to hydrogen at normal temperature, so tungsten oxide with doped catalyst to improving its hydrogen response was adopted. The tungsten oxide films with Pt and PdCl2 catalyst were prepared with sol-gel and DC reactive magnetron sputtering methods. Simultaneously the optical property and surface structure of the catalyst films was studied.Firstly, the mechanism of hydrogen response and developmental actuality were summarized in brief. Secondly, preparative methods and main materials, instrumentation, technological process were introduced in detail. Thirdly, all the films in various condition were tested and compared each. At last, the importance factors which affect the properties of the films were analyzed particularly.The tungsten oxide films with catalyst by two methods were characterized by X- diffractometer, tunnel scan-atomic force microscope, FT-IR, double-beam UV-VIS-NIR spectrophotometer and speediness volt-ampere cycle meter. As results of x-diffractometer, Pt/WO3 sputtered film samples are crystal when annealed at 400℃with distinct diffractive acuti-apices. Reversely, Pt sputtered tungsten oxide sol-gel films and tungsten oxide sol-gel films with PdCl2 catalyst are amorphous when annealed at 400℃without distinct diffractive acuti-apices. When annealed at 460℃the films are crystal with bigger FWHM and diffractive acuti-apices. The temperature from amorphous to crystal of tungsten oxide sol-gel films with catalyst is increased and the reason is in studying.As results of tunnel scan-AFM, both Pt sputtered tungsten oxide films and Pt sputtered tungsten oxide sol-gel films there is distinct and out-of-order parallel line structure on the surface of amorphous. Molecules of the sample tend to tetrahedron and the former has more planarer structure. Atoms of the film by DC reactive magnetron with Pt sputtered tend to plane ordinal structure. Molecules of the the film by sol-gel with Pt sputtered tend to be surface center structure as WO6.As results of FT-IR, the characteristic oscillation of the tungsten oxide sol-gel film with PdCl2 catalyst is more distinct with the higher temperature at the wave band更多还原