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氧化钒热敏薄膜的制备及结构性能研究

Preparations and Properties of the Thermosensitive Vanadium Dioxide Thin Films

【作者】 刘涛

【导师】 李合琴;

【作者基本信息】 合肥工业大学 , 材料学, 2012, 硕士

【摘要】 VO2是一种热敏功能材料,在68℃会发生从单斜结构半导体相向金红石结构金属相的可逆转变,同时伴随着光学、电学等性能的突变,其在光电开关、光存储、非制冷红外、智能窗等诸多方面有广阔的应用前景,使得VO2薄膜的制备及性能的研究成为研究热点。第一章介绍了VO2的晶体结构,相变机理及性能,并阐述VO2薄膜作为一种新型薄膜材料的应用前景。第二章介绍了VO2薄膜的常用制备方法,重点介绍了本文实验采用的磁控溅射法的镀膜机理及制备VO2薄膜的实验过程,实验中采用的薄膜表征检测技术。第三章研究直流磁控溅射法制备VO2薄膜的工艺,重点研究了氧分压,溅射时间及基底对薄膜相变性能的影响,结果表明:当溅射功率为100W,溅射气压为1.5Pa,氧分压为3%,溅射时间为1h,并在氮气中450℃退火保温2小时的薄膜样品相变性能优异,VO2含量最多。薄膜的可见光透过率随着溅射时间的减少而增加。第四章采用直流/射频反应磁控共溅射法制备了掺钨的VO2薄膜及掺钛的VO2薄膜;采用直流磁控溅射法,通入氮气作为掺杂源制备了掺氮的VO2薄膜。实验结果表明:掺钨VO2薄膜的相变温度降低到了37℃,掺钛VO2薄膜的相变温度升高到了67℃,而掺氮VO2薄膜的相变温度为55℃,掺杂后VO2薄膜的相变性能都有所改变。第五章采用直流磁控溅射法制备了TiO2/VO2双层膜,还研究了在不同工艺下制备的TiO2缓冲层对VOX薄膜性能的影响。综合上述研究成果,用直流磁控溅射法在玻璃基片上先沉积TiO2缓冲层,再用直流/射频反应磁控共溅射法制备掺钨VOX薄膜,经过在氮气中退火,得到在TiO2缓冲层上的掺钨VO2智能玻璃,研究结果表明:在溅射气压为1Pa,氧分压为20%,Ti靶采用100W直流电源时,所制备的TiO2缓冲层上的掺钨VO2薄膜致密,晶粒大小均匀。掺钨VO2薄膜样品的相变温度降低至35℃,可见光透过率较高,对红外光的屏蔽效果明显。

【Abstract】 Vanadium dioxide is a kind of thermo-sensitive functional material which changes itsphase reversibly from semiconductor to metal status and accompanies with an abruptchanges in its electrical and optical properties at68℃while heated. It has a wideapplication in many technological fields, such as photo electric switch, optical storage,uncooled infrared detector, intelligent window and so on. The preparing methods andperformances of VO2thin films have been the researching focuses.The first chapter describes the crystal structure, the phase transformation mechanism,and the applications of VO2thin film. It also describes the applicable prospects of VO2thinfilm as a new type of functional thin film materials.The second chapter describes the preparing methods of VO2thin film. It focuses on thecoating mechanism of the reactive magnetron sputtering and the experimental process ofthe preparing VO2thin film as well as the characterization techniques used in ourexperiments.Chapter3studies the DC magnetron sputtering processes prepared VO2thin films. Itfocuses on the influence of partial pressure of oxygen, sputtering time and differentsubstrates on the phase transformation and properties of prepared VO2thin films. Theexperimental results show with the gas pressure of1.5Pa, the power of100W, the sputteringtime of1hour, the partial pressure of oxygen is3%after annealing in argon at450℃for2hours, the phase transition of the VO2thin film sample is better, it contains more VO2phase.With the decreasing of the sputtering time the visible light transmittance of the VO2thinfilm is increased.Chapter4studies the processes of the W doped VO2thin films and the Ti doped VO2thin films prepared by direct current/radio frequency reactive magnetron co-sputtering, andthe N doped VO2thin films prepared by the DC magnetron sputtering at that the N2is usedas for the dopant source. The experimental results show that the phase transitiontemperature of W-doped VO2thin film is reduced to37℃, however, the phase transitiontemperature of Ti-doped VO2thin film is increased to67℃, and the phase transitiontemperature of N-doped VO2thin film is55℃. The phase transitions of the VO2thin filmsare changed after doping.In chapter5the TiO2/VO2double bilayer were prepared by DC magnetron sputtering,The influences of the TiO2buffer layers of different process parameters on the phases and properties of prepared VO2thin films have been studied. Based on the research results, theTiO2buffer layers were deposited on glass substrate by magnetron sputtering equipment,next W-doped VOXthin films were deposited on them by direct current/radio frequencyreactive magnetron co-sputtering, and then they were annealed under nitrogen atmosphere.The W-doped VO2thermosensitive intelligent glasses that based on the TiO2buffer layershave been prepared. The results show that when the sputtering gas pressure is1Pa, thepartial pressure of oxygen is20%, and the DC power of Ti target is100W, the W-dopedVO2thin film has a dense and homogeneous size, and the phase transition temperature ofW-doped VO2thin film is reduced to35℃,the visible light transmittance is high,and theshielding effect of infrared transmittance is obviously.

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