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SiO_x渐变折射率薄膜与ZnO透明导电薄膜的反应磁控溅射工艺及机理研究

Technology and Mechanism Study of Preparing Silicon Oxide Graded Refractive-Index Filters and Transparent Conductive ZnO Films by Reactive Magnetron Sputtering

【作者】 宋秋明

【导师】 王海千;

【作者基本信息】 中国科学技术大学 , 凝聚态物理, 2008, 博士

【摘要】 光学薄膜被广泛应用于科研、国防军事以及民用产品等各个领域。随着光通信、平板显示等技术的出现与发展,以及军事、科学研究等领域新的需求,对光学薄膜性能的要求越来越高,对光学薄膜材料也提出了新的挑战。SiOx和ZnO材料体系都是储量丰富,绿色环保的新型光学薄膜材料,在光学及半导体电器件等工业领域具有广泛的应用前景。SiOx具有折射率在大范围可调,红外光波段透明性好的特点;掺杂的ZnO可以具有良好的透明导电性能。磁控溅射技术是一种已经被广泛采用的成熟的产业化生产技术。精确及可重复地控制SiOx薄膜材料的折射率及膜厚,抑制ZnO薄膜制备过程中的反溅射现象,是决定这两种材料体系能否真正获得产业化应用的关键问题。本论文以SiOx和ZnO材料体系为研究对象,系统地研究了磁控溅射工艺条件对薄膜的化学成分、微结构及光学特性等的影响。从应用的角度重点研究了用反应磁控溅射稳定地获得SiOx中间折射率材料及相关光学薄膜器件的工艺,分析了利用自由基辅助磁控溅射技术制备ZnO薄膜的反溅射现象和机理。通过大量的实验和分析,取得了如下一些结果:1.SiOx渐变折射率材料的反应磁控溅射工艺研究及SiOx/SiO2多层膜红外滤波片光学薄膜器件的制备:(1)利用反应磁控溅射镀膜技术,通过改变氧气流速或溅射功率,精确可重复地获得了折射率在3.69到1.44(@λ=1550 nm)之间可任意调控的SiOx(0≦x≦2)薄膜材料;(2)利用SiOx/SiO2材料组合,成功地演示了具有高折射率比的多层膜带通和反射红外滤光片光学薄膜器件;(3)从原理和实验上证明了采用单一的硅溅射靶材可以制备具有良好光学特性的红外光学器件,为产业化生产提供了一种经济而实用的技术和方法。2.用SiOx制备渐变折射率Rugate Filter的理论及工艺研究:(1)从理论分析的角度讨论了材料的选择及折射率分布的设计对rugate filter光学性质的影响。结果表明,选择合适的折射率振幅调制函数及引入界面折射率匹配层,可以使rugate filter的光学特性得到很大的改善。(2)通过调节SiOx中的氧含量,成功地制备了具有较好光学性能的渐变折射率rugate filter光学薄膜器件。3.用自由基辅助磁控反应溅射法制备ZnO透明导电薄膜过程中的反溅射现象研究:(1)溅射损失主要来源于扩散沉积和反溅射两种机制;(2)在溅射区高能氧负离子对低氧化状态ZnOx膜的轰击是导致反溅射的主要因素。反溅射效应的强弱取决于沉积ZnOx膜的溅射阈值以及溅射区氧负离子的浓度。(3)提出了通过调节真空室中溅射区和氧化区的氧平衡分布抑制ZnO反溅射现象的方法。为下一步制备高质量的ZnO透明导电薄膜提供了实验和理论方面的依据。

【Abstract】 Optical coating technologies have been widely applied in many areas,such as scientific research,national defense,military and civilian products etc.To match the fast growing application requirements of optical communication,flat panel display etc, the performance requirements of optical coating is became more and more stringent, which issue new challenge in optical coating materials.The SiOx and ZnO are both abundant,environmentally friendly and non-toxic new type optical coating materials,which have a wide application prospect in optical and semiconductor device industry.SiOx materials have a wide range tunable refractive index and high transparency in infrared band,and doped ZnO has a good transparent conductive performance,make them win widespread attention.Magnetron sputtering is a widely used,mature and industrialized production technology.The two importance problem,about how to precisely and repeatedly control refractive index and thickness variation of fabricated SiOx films,and how to suppress the resputtering effect during the sputtering process of ZnO,are crucial in applying to the industrialized production.The main purpose of this article is about a comprehensive study on the SiOx and ZnO materials,concerning how magnetron sputtering parameters affect the chemical composition,microstructure and optical properties of deposited films.We do some research from view of application mainly about using reactive magnetron sputtering to get a steady SiOx material with middle-refractive index and optical coating devices related,analyzing the resputtering phenomenon and the cause in the ways using radical assisted sputtering to prepare ZnO films.From plenty of experiments and careful analysis,we get the following result:1.The art to fabricate SiOx graded refractive index material and relative SiOx/SiO2 multilayer infrared filters by reactive magnetron sputtering:(1) Graded refractive index SiOx(0≦x≦2) thin film material with precisely controlled refractive index ranging from 3.69 to 1.44(@λ=1550 nm) have been obtained by changing the oxygen flow rate or sputtering power through reactive magnetron sputtering.(2) Successfully demonstrated SiOx/SiO2 multilayered band-pass filters and infrared reflective filters by combining the high refractive index SiO2 and low refractive SiOx(0≦x≦2) materials together as multilayer thin films.(3) Proved the feasibility to fabricate high quality infrared optical filters by using Si targets only,which provides a practical and economical technology for industrial fabrication.2.Theoretical and practical research on fabricating Rugate Filter by using SiOx graded refractive index material:(1) Theoretically discussed the effect of material choice and refractive index distribution design on the optical property of rugate filter.It is shown by the experimental results that the optical property of rugate filter can by improved greatly by choosing proper refractive index amplitude modulation function and introducing refractive index matching layer on the interface.(2) Successfully manufactured high optical quality graded refractive index rugate filter by adjusting the oxygen content of the SiOx layers.3.Research on the resputtering phenomena in radical assisted magnetron sputtering of ZnO transparent conductive film:(1) Sputtering loss mainly orients from diffused deposition and resputtering mechanisms.(2) The bombardment of negative oxygen ions on the deposited low oxide degree ZnOx film is the main reason yielding the resputtering phenomena. The degree of reputtering is determined by the sputtering threshold of the as deposited ZnOx film and the concentration of negative oxygen ions in sputtering zone.(3) Suggested a method to suppress the resputtering effect in ZnO film sputtering by adjusting the balance of oxygen distribution between sputtering zone and oxidation zone,provide guidance in both theory and experiment for preparing high quality ZnO transparent conductive film in future.

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