涂层界面结合强度检测研究(Ⅱ)：涂层结合界面应力检测系统

利用X射线衍射技术(XRD)测试了涂层及其基体材料的应力及其变化规律，建立了一种涂层结合界面应力检测系统，进行界面结合状态的检测研究.利用涂层从基体脱粘前后的界面应力变化量，结合涂层材料的物性参数和涂层-基体系统温度场参数，用涂层残余应力衍射峰来表征涂层与基体的结合强度，创立一种研究检测涂层结合强度理论的实验新方法，适用于各种热障涂层的界面结合强度测量. 关键词： X射线衍射法(XRD) 界面结合强度 涂层 残余应力     

涂层界面结合强度检测研究(Ⅰ):涂层结合界面应力的理论分析

利用激光划痕测试法和弯曲应力理论，建立了涂层结合界面应力的理论模型，推导出结合界面剪应力、正应力和剥离应力分布公式，分析了结合界面应力产生的机理.理论分析结果表明，界面正应力主要集中在界面中心区域内，而在界面边缘附近，正应力迅速下降，在界面边缘处其值降为0；剪应力和剥离应力主要集中在界面边缘区域内，在远离界面边缘区域，剪应力和剥离应力则迅速下降；涂层中正应力和涂层厚度、基体厚度以及杨氏模量无关，界面间剪应力以及剥离应力随涂层厚度增加而增加，并且由涂层与基体厚度以及杨氏模量所共同决定.     

金刚石膜厚度尺寸对热残余应力的影响

 采用有限元方法对钼基体上不同厚度（20~1 000 μm）金刚石膜的热残余应力进行了全面的模拟与分析,得出了它们在膜内分布的等值线图,研究了金刚石膜厚度尺寸对整个膜内的最大主拉应力和界面处每个应力分量最大值的影响。结果表明：在整个膜内,最大主拉应力的位置出现在膜的表面、界面或侧面,其值随膜厚度的增加而增大;在界面处,最大轴向应力随膜厚度的增加而增大,而最大径向压应力、最大周向压应力和最大剪应力则随膜厚度的增加而减小,其中最大剪应力减幅较小;膜厚度越大时,以上各量随厚度增（减）的速度越慢。其结论对于在金刚石膜的制备中合理地选择厚度、有效地进行应力控制有一定的参考价值。     

涂层界面结合强度检测研究（I）：涂层结合界面应力的理论分析

利用激光划痕测试法和弯曲应力理论，建立了涂层结合界面应力的理论模型，推导出结合界面剪应力、正应力和剥离应力分布公式，分析了结合界面应力产生的机理．理论分析结果表明，界面正应力主要集中在界面中心区域内，而在界面边缘附近，正应力迅速下降，在界面边缘处其值降为0；剪应力和剥离应力主要集中在界面边缘区域内，在远离界面边缘区域，剪应力和剥离应力则迅速下降；涂层中正应力和涂层厚度、基体厚度以及杨氏模量无关，界面间剪应力以及剥离应力随涂层厚度增加而增加，并且由涂层与基体厚度以及杨氏模量所共同决定．     

采用深度刻蚀与XPS能谱研究缓蚀膜/镀铜层/铁基体界面成分

为了探索焦磷酸盐镀铜层与铁基体结合强度差的原因,采用波谱技术,分析了纵向界面各种元素的成分变化,讨论了金属基体表面粗糙度对元素分布的影响.根据刻蚀时间可将膜层分为三部分:N,O量迅速减少的表面层,有基本固定组成的中间层和占一半厚度的出现基体元素的混合干扰层.通过对后期混合层中氧含量的分析,可得出镀铜层/铁基体界面含氧层的存在是影响电镀层与基体结合强度的主要原因的结论.     

原位等离子体逐层氧化a-Si:H/SiO2多层膜的光致发光研究

采用在等离子体增强化学汽相沉积系统中沉积a-Si:H和原位等离子体逐层氧化的方法制备a-Si:H/SiO2多层膜.改变a-Si:H层的厚度，首次在室温下观察到来自a-Si:H/SiO2多层膜较强的蓝色光致发光和从465到435nm的蓝移.x射线能谱证明，SiO2层是化学配比的SiO2；C-V特性表明，a-Si:H/SiO2界面得到了很好的钝化；透射电子显微镜表明，样品形成了界面陡峭的多层结构.结合光吸收谱和光致发光谱的研究，对其发光机理进行了讨论.用一维量子限制模型对光致发光峰随着a-Si:H层厚度的减小 关键词： a-Si:H/SiO2多层膜 光致发光     

Nb-Al合金高温氧化机理

通过自编软件建立了铝氧化膜与基体铌界面的原子集团模型,用递归法计算了合金的原子埋置能、原子结合能等电子参数,从电子层面分析铌合金高温氧化机理.研究表明:铝通过晶界扩散偏聚在合金表面,并与氧结合生成致密的Al2O3氧化膜,阻挡氧向铌基体扩散.晶界和稀土元素能提高氧化膜与基体间的原子结合能,增加其界面的结合强度,加强氧化膜与基体铌间的黏附性.因此,通过在合金中添加稀土元素或细化合金晶粒均能提高铌合金的抗高温氧化性能.     

附着铜膜的内应力及屈服强度

用X-射线衍射和热循环基片弯曲方法测量了附着在基体上纯铜膜的内应力和屈服强度。内应力为张应力且随工作气体（氩气）压强的增加而减小但随膜厚的增加而增加。钢基体上铜膜的张屈服强度与膜厚的倒数成反比。压屈服强度也同样依赖于膜厚，即膜越薄，压屈服强度越高。     

ZA27/CNT界面特性电子理论研究

依据原子结合能定义了界面结合能. 采用递归法计算了纳米管增强锌铝基复合材料中ZA27/CNT界面电子结构，揭示了纳米管在ZA27合金晶界分布的微观物理本质，及其ZA27/CNT弱界面结合的电子层面的原因. 研究发现：金属基体对纳米管增强相上的碳原子态密度影响很大，而纳米管对基体金属中的铝、锌原子影响很小. 碳原子态密度与基体金属原子趋于同化，使纳米管与基体金属结合，但因同化程度不高导致界面结合较弱，影响强化效果. 如果在纳米管装饰或镀上与基体金属性质相近的原子层，会极大改善复合材料的界面结合强度，提高复合材料性能. 关键词： 复合材料 纳米管 电子结构 界面     

SiC纤维增强Ti17合金复合材料轴向残余应力的拉曼光谱和X射线衍射法对比研究

准确测量和分析SiC纤维增强Ti合金复合材料(SiC_f/Ti)中残余应力状态对优化复合材料的成型工艺和理解其失效模式具有重要意义,但其残余应力的实验测量和分析仍是一个挑战.石墨C涂层作为SiC纤维与Ti17基体合金之间必需的扩散障涂层,承载了由纤维与基体之间热不匹配引入的残余应力.本文采用显微拉曼光谱法对比测量纤维表面C涂层在复合材料中和去掉基体无应力态下G峰的峰位,通过石墨C涂层应力态下峰位移动计算出SiCf/C/Ti17复合材料中SiC纤维受到～705.0 MPa的残余压应力.采用X射线衍射方法测量了不同方向上该复合材料中基体钛合金的晶面间距以获取其空间应变,根据三轴应力模型分析了复合材料中基体钛合金沿轴向方向的残余应力为～701.3 MPa的张应力,并通过线性弹性理论转化为SiC纤维的残余压应力为～759.4 MPa.两种测试方法都确定了SiC纤维在成型过程中受到残余压应力,且获得的应力值较为接近,都可以用于对SiC_f/Ti复合材料的残余应力测量.     

Synthesis surface effects on the stress and deformation of film/substrate system

The closed-form solutions of bending curvature and stress distribution in film/substrate system with the synthesis surface effect are proposed by minimizing the total potential energy. Effects of the roughness and the residual surface stress on stress in film are addressed. Results reveal that, at a given thickness of the substrate, effects of roughness and residual surface stress on the bending curvature become significant with decreasing the film thickness. The roughing surface will enlarge the magnitudes of bending curvature and film stress. The direction change of residual surface stresses can lead to a reversed bending of film/substrate system.     

Determination of residual stresses within plasma spray coating using Moiré interferometry method

In this paper, residual stresses of the Ni-Cr-B-Si coatings prepared by supersonic plasma spray processing were measured by moiré interferometry and X-ray diffraction method. Moiré interferometry method was used in measuring the distribution of residual stresses of the Ni-Cr-B-Si coatings alongside the specimen thickness direction, then the distribution of residual stresses both in the substrate and the coating was also analyzed. Experimental results showed that residual stresses in the coating and the substrate are tensile and compressive separately; residual stresses of the coating are diminished with the increase of the distance from the coating surface and almost zero at the coating-substrate interface; the maximum of compressive residual stresses of the substrate are present to the vicinity of the coating-substrate interface. It could be concluded that residual stresses in the specimen would result from the dismatch of thermophysical properties between the coating and substrate during the spray process, and the distribution of residual stresses of the substrate would be influenced by the sandblasting prior to spraying.     

Elastic-plastic analyses on the residual stresses and curvature of the film/substrate bilayer system

During thermal cycling, the residual stresses are often generated in the film/substrate bilayer due to the material mismatch between the substrate and the film. If the thickness of the film is relatively high, the thermal residual stresses in it may be of different signs. When the film is subjected to elastic-plastic deformation, two plastic zones with different thicknesses may be generated in the film at a significantly high temperature difference. In this paper, a theoretical model which reflects the complete history of thermal residual stresses and curvatures in the elastoplastic film/substrate bilayer system is developed. Solutions are derived to estimate the residual stresses and curvature in the film as functions of temperature difference. The case of Al/Si system is used to illustrate the implementation of this model. Results show that the critical temperature difference at which the second plastic zone near the film surface is generated near the Al film surface is dependent on the film thickness. The strain hardening of the film has an obvious influence on the magnitude of residual stresses within the film at high temperature difference.     

Transformation behavior of Ni-Mn-Ga/Si(100) thin film composites with different film thicknesses

A series of Ni_51.4Mn_28.3Ga_20.3/Si(100) thin film composites with different film thicknesses varying from 0.1 to 5 μm have been prepared by magnetron sputtering and subsequently annealed. X-ray powder diffraction patterns of the films show the features associated with the lattice-modulated martensitic phase and/or cubic austenite at room temperature. 220-fiber texture was confirmed by the X-rays measurements made at 150 °C. While the Curie temperature is almost film thickness independent, the martensitic transformation temperature shows a strong descended dependence in the submicron range. The substrate curvature measurements demonstrate that the forward and reverse martensitic transformation in the films is accompanied by the reversible relaxation and accumulation of residual stress, originally created by the thermal treatment due to the difference in thermal expansion of the film and substrate. The values of residual stresses measured by both substrate curvature and X-rays diffraction methods at constant temperatures are found to be dependent on the film thickness. This behavior appears in correlation with the thickness dependence of the transformation temperature.     

Residual stress in Ni-Mn-Ga thin films deposited on different substrates

Four series of Ni_51.4Mn_28.3Ga_20.3/substrate thin film composites, where the substrate is either Si(100), MgO(100), alumina or Mo foil, and two series of Ni_53.5Mn_23.8Ga_22.7/substrate composites where the substrate is either alumina or Mo foil, with different film thicknesses varying from 0.1 to 5 μm have been studied in the cubic phase by XRD stress measurements. The values of residual stresses are found to be dependent on both substrate and film thickness. In the submicron range, a correlation between thickness dependencies of residual stress and transformation temperatures is experimentally obtained. The temperature dependence of the d-spacing d₂₂₀ is studied for the films deposited on Si(100).     

光学薄膜残余应力分配预测模型计算方法研究

残余应力是光学薄膜研究的一个重要组成部分，它对光学元器件有很大的影响。根据弹性力学原理，基于应变不匹配，提出了一种可以预测薄膜残余应力分配的理论模型计算方法，并将计算结果与干涉仪测量值进行了对比。利用所建立的模型分析了薄膜参数变化时基底残余应力的变化情况。结果表明：所建模型合理；随着镀膜温度的增加，基底总残余应力随镀膜温度升高而呈增大的趋势;本征应力变化不太大；随着基底厚度的减小，基底上下表面应力呈增大的趋势，而薄膜应力则呈减小趋势，但变化趋势很小。基底的中心轴约位于基底上表面以下2／3处。     

Investigations on macroscopic intrinsic stress in amorphous binary-alloy films

Macroscopic tensile and compressive mechanical stresses in the film plane are observed during the growth of amorphous binary-alloy films of ZrCo and TbCo prepared by the condensation of the metal vapours from two electron-beam evaporators. The mechanical stress is measured by a capacitive cantilever beam technique. Both kinds of stresses are affected by composition and substrate temperature, but the compressive stress additionally depends on the film thickness, evaporation rate and substrate material. The results are discussed in terms of a model for the growth of amorphous films published earlier.     

Spatially resolved Raman spectroscopy evaluation of residual stresses in 3C-SiC layer deposited on Si substrates with different crystallographic orientations

Raman scattering studies were performed on hot-wall chemical vapor deposited (heteroepitaxial) silicon carbide (SiC) films grown on Si substrates with orientations of (1 0 0), (1 1 1), (1 1 0) and (2 1 1), respectively. Raman spectra suggested that good quality cubic SiC single crystals could be obtained on the Si substrate, independent of its crystallographic orientation. Average residual stresses in the epitaxially grown 3C-SiC films were measured with the laser waist focused on the epilayer surface. Tensile and compressive residual stresses were found to be stored within the SiC film and in the Si substrate, respectively. The residual stress exhibited a marked dependence on the orientation of the substrate. The measured stresses were comparable to the thermal stress deduced from elastic deformation theory, which demonstrates that the large lattice mismatch between cubic SiC and Si is effectively relieved by initial carbonization. The confocal configuration of the optical probe enabled a stress evaluation along the cross-section of the sample, which showed maximum tensile stress magnitude at the SiC/Si interface from the SiC side, decreasing away from the interface in varied rate for different crystallographic orientations. Defocusing experiments were used to precisely characterize the geometry of the laser probe in 3C-SiC single crystal. Based on this knowledge, a theoretical convolution of the in-depth stress distribution could be obtained, which showed a satisfactory agreement with stress values obtained by experiments performed on the 3C-SiC surface.     

Yield strength of attached copper film

Variation of stress in attached copper film with an applied strain is measured by X-ray diffraction combined with a four-point bending method.A lower slope of the initial elastic segment of the curve of X-ray measured stress versus applied strain results from incomplete elastic strain transferred from the substrate to the film due to insufficiently strong interface cohesion.So the slope of the initial elastic segment of the X-ray stress (or X-ray strain directly) of the film against the substrate applied strain may be used to measure the film-substrate cohesive strength.The yield strength of the attached copper film is much higher than that of the bulk material and varies linearly with the inverse of the film thickness.