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题名	光学薄膜应力表征及其与微观结构的关系
作者	肖祁陵
学位类别	博士
答辩日期	2009
授予单位	中国科学院上海光学精密机械研究所
导师	邵建达
关键词	残余应力 薄膜 形成机理 X射线衍射 应力测量 微观结构
其他题名	Measurements of residual stress and its relationship with microstructure in optical films
中文摘要	薄膜应力是薄膜生产、制备中的一种普遍现象，几乎所有的薄膜都处于一定的应力状态。已有的研究表明，残余应力对薄膜的电学、力学性能、尺寸稳定性和使用寿命有着直接的影响。因此，残余应力的研究一直是薄膜研究关注的热点。 本文采用了干涉仪法和不同的X射线衍射应力测试方法对几种常用氧化物薄膜中的应力进行了表征，对应力随沉积条件的变化规律进行了深入研究，从微观结构的角度对应力的产生机理进行了分析，探讨了薄膜微观结构与其应力之间的联系，并对YSZ/ SiO2组合多层膜中的应力在厚度方向的变化进行了初步实验研究。 首先为获取能用X射线衍射方法表征的样品，研究了沉积温度和退火温度对ZrO2薄膜结晶性能和应力的影响，结果表明，在沉积温度为300℃或经400℃退火后的ZrO2薄膜才出现明显的结晶，结晶的薄膜为四方相与单斜相混合结构。随沉积温度升高，ZrO2薄膜的应力性质由张应力逐渐向压应力转变，对应薄膜的结构由非晶逐渐向单斜相和四方相混合结构转变。退火使薄膜结构的变化，薄膜应力也相应的改变。对已结晶的ZrO2薄膜样品，由于其结构的复杂性，采用X射线同倾法与侧倾法不能获得确定的应力值。 通过对Y2O3，TiO2及不同Y2O3含量掺杂的ZrO2薄膜的X射线应力表征，发现侧倾法适用于表征光学薄膜的应力，掠入射多个衍射峰方法对无择优取向的薄膜可获得较好的测试结果。 通过对HfO2、Y2O3、TiO2及不同Y2O3含量掺杂的ZrO2薄膜应力随沉积条件变化的研究，发现对于单相结构的薄膜，物相结构不变，薄膜的应力性质不变；薄膜应力值的改变受薄膜结构的择优取向，晶粒尺寸，堆积密度等多种因素的影响。 在ZrO2膜料中添加不同含量的Y2O3后，在沉积温度为200℃时，Y2O3的加入使得薄膜由非晶结构向立方相转变，薄膜的应力性质由张应力向压应力演变，在沉积温度为300℃时，Y2O3的加入使得薄膜由单斜相与四方相混合结构向立方相转变，并且结晶性逐渐增强，应力性质从压应力向张应力转变。这说明把Y2O3加入ZrO2中，可以改变薄膜的应力状态，薄膜中的残余应力与薄膜沉积过程中微结构的变化有密切关系。 在单层膜实验研究的基础上，通过调节两种应力性质相反材料的厚度组合比例可以有效的调节YSZ/SiO2多层膜中的应力。利用X射线掠入射方法，对多层膜的应力在薄膜厚度方向的变化作了初步的研究，通过改变掠入射角，测量了多层膜表层不同深度的结构信息，定性的给出了薄膜应力随深度变化的规律，发现薄膜微结构应变与最终残余应力表现出一致的变化趋势。
英文摘要	It is well known that almost thin film materials deposited are in a state of stress, which is generated in various process of condensation. The analysis of the residual stress state is of great technological importance because stresses can be beneficial or detrimental with respect to the electrical, mechanical properties etc. In this dissertation, the residual stresses in oxide optical films were determined by using an optical interference method and different X-ray diffraction (XRD) techniques. The residual stresses of these films depending on deposition parameters were systematically studied. The relationships between residual stresses and microstructure of thin films were also investigated. The evolution of the residual stress in function of the thickness of YSZ/SiO2 multilayer was given a preliminary study by using glancing incident XRD. Firstly, the crystallization and residual stress of ZrO2 films were studied under different deposition and annealing temperatures. The results showed that crystal structure was observed for deposition temperatures above 200℃ or annealing temperatures above 300℃. The residual stress in ZrO2 films changed from tensile to compressive with the increase of deposition temperature and the structure transform from amorphous to the mixed structure of monoclinic and tetragonal phase. Annealed films showed stress change which is explained by complex structure transformation. The residual stress in crystallization ZrO2 films was uncertain by using XRD iso-inclination method and side-inclination method. The residual stress of Y2O3, TiO2 and YSZ thin films was measured by X-ray methods. The results showed that XRD side-inclination method was more suitable for measuring the stress of optical thin films and Fixed Incidence Multiplane XRD techniques can be used to determine the stress of thin films without obvious texture. The influences of deposition parameters on the residual stress of HfO2、Y2O3、TiO2 and YSZ films were investigated. The experimental results indicated that when the crystal structure remains unchanged for single phase thin films, the same of the residual stresses characteristic. The magnitude of residual stresses was found to be related to multifactor such as preferred orientation, packing density, grain size affected by deposition parameters. Y2O3 stabilized ZrO2 coating material with different Y2O3 molar content were prepared. The effects of different Y2O3 content on residual stresses and structures of YSZ thin films were revealed. When deposition temperatures was 200℃, residual stresses of films transformed from tensile stress into compressive stress and the structures of films changed from the amorphous into high temperature cubic phase with the increase of Y2O3 content. When deposition temperatures was 300℃, residual stresses of films transformed from compressive stress into tensile stress and the structures of films changed from the monoclinic and tetragonal phase into only cubic phase. The adding Y2O3 had more effect in residual stresses and structures of YSZ thin films. The variations of residual stress corresponded to the evolutions of structures induced by adding of Y2O3. The total stress in YSZ/SiO2 multilayer was adjusted effectively by alternating the thickness ratio of two thin films. The pilot study was performed on the evolution of the residual stress in thickness of multilayer by using glancing incident XRD. The result showed that this method can give the characterization of thin film stress changes with depth by changing the grazing angle of incidence. The variation of the microstructure examined by the X-ray diffraction showed that the microscopic deformation did correspond to the macroscopic stress.
语种	中文
内容类型	学位论文
源URL	[http://ir.siom.ac.cn/handle/181231/15269]
专题	上海光学精密机械研究所_学位论文
推荐引用方式 GB/T 7714	肖祁陵. 光学薄膜应力表征及其与微观结构的关系[D]. 中国科学院上海光学精密机械研究所. 2009.

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