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磁控溅射法制备WO3电致变色薄膜和钛掺杂改性研究

The Study on Preparation of WO3 Films and Modification by Doping Titanium by Magnetron Sputtering Method

【作者】 胡远荣

【导师】 李国卿;

【作者基本信息】 大连理工大学 , 等离子体物理, 2006, 硕士

【摘要】 WO3薄膜因具有着色效率高、可逆性好、响应时间短、寿命长、着色和褪色时的光学变化范围较宽等优点,被认为是最有发展前景的电致变色材料之一。 采用中频孪生非平衡磁控溅射制备WO3薄膜,室温沉积的薄膜为非晶态。运用X射线衍射(XRD),拉曼光谱、红外光谱、紫外分光光度计、计时安培分析仪和原子力显微镜(AFM)等测试手段分析了薄膜的结构和光学性能。实验结果表明:热处理温度低于300℃时,WO3薄膜呈非晶态,热处理温度在300℃~400℃之间WO3薄膜发生非晶态向多晶的转变,流量比大于95%时制备的非晶WO3薄膜,经过200℃热处理1h后,具有较好的电致变色性能,尤其对于波长大于500~800nm的绿光到红光范围,薄膜的平均透光率差值大于50%。 采用中频孪生非平衡磁控溅射,以纯金属钨和钛的组合靶源,制备钛掺杂WO3电致变色薄膜。实验结果表明,钛掺杂薄膜在相同的热处理条件下晶化程度降低,晶粒细化,离子抽出和注入的通道增多,钛掺杂5.1%的着色响应速度的提高,循环寿命提高了4倍以上。着色态时W-O-W对应的峰减弱,W=O对应的峰增强,这归因于Li+离子进入薄膜使得W-O-W键被破坏,形成大量终端W=O键,掺杂薄膜在着色态有更多的W-O-W键被破坏,更有利于Li+注入。 采用“Glass/ITO/WO3/Electrolyte/ITO/Glass”结构制成电致变色器件,有很好的变色效果,着色和褪色均匀,着色效率高,对于波长范围600~800nm内,着色和褪色透光率之差达45%以上,电致变色器件的着色响应时间为20s,褪色响应时间为10s左右。

【Abstract】 Tungsten oxide is probably the most promising one of various electrochromic materials due to its excellent electrochromic properties including good color efficiency, excellent response speed, long term stability and large variation of optical modulation.WO3 films were prepared by mid-frequency dual target magnetron sputtering system. The structure and electrochromic properties of the films were analyzed by X-Ray diffraction, Raman Spectroscopy. Spectrophotometer, cyclic chronoamperometry and atomic force microscopy .The result show that the as-deposited WO3 films are amorphous. WO3 crystalline are formed at 300 - 400 ℃ . The films deposited at high oxygen content show good electrochromic property after annealing at 200℃. And the variation of average transmittance difference between the bleached and colored state can reach 60% in the wavelength range between 500nm and 800nm.Ti-doped WO3 films were prepared by mid-frequency dual-target magnetron sputtering method. The results indicate that the crystallinity decrease after doping titanium, And the channels for ions injecting and extracting increase. Accordingly, the responding speed of doping 5.1% of titanium gets faster and its circle life increases more than four times. In the colored state, the intensity of peak corresponding to W-O-W bonds decrease, and the intensity of peak corresponding to W=O bonds increase, since W-O-W bonds break down for Li+ion injecting and more W=O bonds form. It is more convenient for Li+ ions to inject into film corresponding to the doped film than undoped one because of more W-O-W bonds breaking down.The structure of "glass/ ITO/ WO3/ electrolyte /ITO/ glass" was fabricated, which has good color efficiency, even the variation of average transmittance difference between the bleached and colored state can reach 45% in the wavelength range between 600nm and 800nm. The color responding time of the device is about 20 second, and its bleach responding time is about 10 second.

【关键词】 电致变色氧化钨钛掺杂磁控溅射
【Key words】 ElectrochromicWO3doping Timagnetron sputtering
  • 【分类号】O484.1
  • 【被引频次】2
  • 【下载频次】488
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