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。     

Externally applied stress sign and film elastic properties effects on brittle film fracture

Rectangular stainless steel samples with TiN film deposited on the front lateral surface were loaded in three-point bending to the maximum normal strain of 6%. Scanning electron microscopy showed that vertical cracks appeared in the tension zone when the tensile strain exceeded 1.5%, while horizontal cracks appeared in the compression zone when the compressive strain exceeded –2.9%. Film cracks in the compressive zone originate from the tensile stress imposed by the plastically deformed substrate due to the Poisson’s expansion. Taking plastic deformation and Poisson’s expansion of the substrate in compression into account, theoretical analysis of normal stress distribution along the cracked film segment in compression is presented. Substrate strain and film elastic properties affect film cracking in the compressive zone. At larger compressive strain, some transverse cracks along with buckling cause the film spallation. The presented method is useful for studying brittle film fracture with variable strain levels in a single sample.     

多晶薄膜屈服强度的一个模型

从位错运动的应力功和应变能关系导出了附着在基体上并有钝化层薄膜的屈服强度公式.该式表明多晶薄膜的屈服强度由两个影响因子（晶粒取向和位错类型）和三个强化因子（钝化层强化，基体强化和晶粒强化）确定.和已报道的实验结果基本一致表明了该模型的合理性. 关键词： 多晶薄膜 屈服强度     

Effect of a fullerene C60 addition on the strength properties of nanocrystalline copper and aluminum under shock-wave loading

The Hugoniot elastic limit and the spall strength of aluminum and copper samples pressed from a mixture of a metallic powder and 2–5 wt % C₆₀ fullerene powder are measured under a shock loading pressure up to 6 GPa and a strain rate of 10⁵ s^?1 by recording and analyzing full wave profiles using a VISAR laser interferometer. It is shown that a 5% C₆₀ fullerene addition to an initial aluminum sample leads to an increase in its Hugoniot elastic limit by an order of magnitude. Mixture copper samples with 2% fullerene also exhibit a multiple increase in the elastic limit as compared to commercial-grade copper. The elastic limits calculated from the wave profiles are 0.82–1.56 GPa for aluminum samples and 1.35–3.46 GPa for copper samples depending on the sample porosity. The spall strength of both aluminum and copper samples with fullerene additions decreases approximately threefold because of the effect of high-hardness fullerene particles, which serve as tensile stress concentrators in a material under dynamic fracture.     

基于XRD的镀锌钝化膜残余应力试验研究

利用XRD技术测试了镀锌钝化膜结合界面的残余应力，同时通过电解抛光法检测了其厚度方向残余应力的分布规律，分析了残余应力对镀锌钝化膜结合强度的影响. 试验结果表明，镀锌钝化膜的残余应力均表现为压应力，并随着基体表面残余应力的增大而减小；钝化膜在2—10μm厚度方向的残应力为-274.5—-428.3MPa，其应力为梯度分布；镀锌钝化膜与基体的界面结合强度与其残余应力成反比，减小薄膜残余应力，有利于提高镀锌钝化膜与基体的结合强度. 关键词： X射线衍射法(XRD) 镀锌钝化膜 结合强度 残余应力     

The determination of stresses in thin films; modelling elastic grain interaction

X-ray diffraction is frequently employed for the analysis of mechanical stresses in polycrystalline specimens. To this end, suitable so-called diffraction elastic constants are needed for determining the components of the mechanical stress tensor from measured lattice strains. These diffraction elastic constants depend on the single-crystal elastic constants of the material considered and the so-called grain interaction, describing the distribution of stresses and strains over the crystallographically differently oriented crystallites composing the specimen. Well-known grain interaction models, as due to Voigt, to Reuss, to Neerfeld and Hill and to Eshelby and Kröner, may be applied to bulk specimens, but they are generally not suitable for thin films. In this paper, an average 'effective' grain interaction model is proposed that consists of a linear combination of basic extreme models including new models specially suited to thin films. Experimental verification has been achieved by X-ray diffraction strain measurements performed on a sputter-deposited copper film. This is the first time that anisotropic grain interaction has been analysed quantitatively.     

STRESS ANALYSIS IN CUBIC BORON NITRIDE FILMS BY X-RAY DIFFRACTION USING sin2 ψ METHOD

The boron nitride (BN) films containing cubic boron nitride (c-BN) and hexagonal boron nitride (h-BN) were prepared by radio frequency a ssisted thermal filament chemical vapor deposition. The stress and strain in BN films were investigated by X-ray diffraction analysis using the sin² ψ method. The results showed that both c-BN and h-BN in the same film have similar values of elastic strain, however, the compressive stress in c-BN is much greater than that in h-BN for the same film. Both stress and strain gradually decre ased with the increase of substrate temperature (T_s). The effective stress in the films calculated by the effective stress model increased with the increase of T_s. Furthermore, the dependence of effective stress in the films on T_s was also investigated.     

强激光辐照下纳米晶体铜薄膜层裂破坏的实验研究

采用强激光辐照加载技术和激光速度干涉(VISAR)测试技术,对纳米晶体铜薄膜的层裂特性进行实验测量和分析.基于VISAR实测的自由面速度波形,计算得到纳米晶体铜薄膜在超高拉伸应变率下的层裂强度高达3 GPa,明显高于多晶铜的层裂强度, 其原因归咎于纳米晶体材料中存在大量晶界阻碍了位错运动. 关键词： 纳米晶体铜薄膜 层裂 激光辐照     

强激光辐照下纳米晶体铜薄膜层裂破坏的实验研究

采用强激光辐照加载技术和激光速度干涉(VISAR)测试技术，对纳米晶体铜薄膜的层裂特性进行实验测量和分析.基于VISAR实测的自由面速度波形，计算得到纳米晶体铜薄膜在超高拉伸应变率下的层裂强度高达3 GPa，明显高于多晶铜的层裂强度, 其原因归咎于纳米晶体材料中存在大量晶界阻碍了位错运动.     

平面冲击下铜的拉伸应变率相关特性研究

本文对冲击加载下高纯无氧铜的拉伸应变率相关特性进行了实验研究.实验中利用磁测速系统测试撞击前飞片速度,利用光纤位移仪——多普勒探针系统测试样品自由面粒子速度剖面.对自由面速度剖面的特征参量进行计算分析,结果表明:铜样品的层裂强度随着拉伸应变率的增加而增加,对比发现层裂强度不仅受加载条件的影响,同时受到材料本身微细观结构影响;同时随着拉伸应变率的增加,自由面速度的回跳斜率呈现出先缓慢增加后迅速增加的临界特性;最后,通过层裂样品中波系相互作用,给出了自由面速度回跳过程中的振荡特征随着拉伸应变率增加而逐渐消失的物理过程.     

Strain due to nickel diffusion into hydrogen-terminated Si(1 1 1) surface

We studied the affection of thin (i.e., 0.2–0.8 nm) Ni films on hydrogen-terminated Si(1 1 1) substrate surface by using strain-sensitive X-ray diffraction. It was reported that Ni deposition onto hydrogen-terminated Si surface apparently does not cause film growth, but rather diffuses into the Si crystal, creating an “Ni diffusion layer” up to Ni deposition 0.8 nm thick. Measured rocking curves of the Si 1 1 3 reflection and integrated intensities of the rocking curves for the substrate provide information about the evolution of the strain field introduced near the substrate surface during Ni diffusion into the substrate. Comparing the measured and calculated rocking curves indicates that compression of the {1 1 1} spacing of the Si occurs gradually up to an Ni thickness of 0.6 nm, and that above this thickness, strain relaxation occurs.

We found that the slope of the integrated intensity of the rocking curve versus X-ray wavelength correlates to the strain field near the surface, in the same way that the shape of the rocking curves correlate to the strain field near the surface. Dynamical diffraction calculations indicate that measurement of the slope of the integrated intensity of the rocking curve versus X-ray wavelength is useful for strain analysis, because the dependence is not only sensitive to strain fields, but is also insensitive to the effect of absorption by the overlayer, which otherwise would cause deformation of the shape of the rocking curve.     

非一维应变冲击加载下高纯铜初始层裂行为

提出了一种锥形靶层裂实验新方法,开展非一维应变冲击条件下高纯铜初始层裂行为实验研究,讨论了锥形靶内部损伤分布特征及其与自由面速度典型特征之间的内禀关系.结果显示:1)初始层裂的锥形靶内部出现了连续损伤区,损伤区扩展方向与锥面平行,从锥底到锥顶呈现了不同的损伤状态,从微孔洞独立长大到局部聚集,最后形成宏观裂纹,这种损伤状态分布特征归因于锥形靶内部拉伸应力幅值和持续时间的空间演化;2)通过锥形靶横截面损伤度定量统计分析,揭示损伤演化早期的微孔洞成核与早期长大过程是随机的,而损伤演化后期的微孔洞聚集过程具有显著的局域化特征;3)不同位置处实测的自由面法向粒子速度剖面呈现出典型的层裂Pull-back信号,但是通过与内部损伤分布特征对比,揭示基于Pull-back速度获得高纯铜层裂强度本质是微孔洞成核阈值应力,Pull-back回跳速度斜率反映了损伤演化速率,Pull-back回跳幅值与损伤度引起的应力松弛密切相关.     

单层单晶石墨烯与柔性基底界面性能的实验研究

单晶石墨烯具有更优异的力学及电学性能,有望成为新一代柔性电子器件的核心材料.因此,有必要从实验的角度精细分析化学气相沉积法制得的大尺度单晶石墨烯与柔性基底复合结构的界面力学行为.本文通过显微拉曼光谱实验方法测量了不同长度的单层单晶石墨烯/PET(聚对苯二甲酸乙二醇酯)基底的界面力学性能参数及其在长度方向上界面边缘的尺度效应.实验给出了石墨烯在PET基底加载过程中与基底间黏附、滑移、脱黏三个界面状态的演化过程与应力分布规律.实验发现,单晶石墨烯与柔性基底间由范德瓦耳斯力控制的界面应变传递过程存在明显的边缘效应,并且与石墨烯的长度有关.界面的切应力具有尺度效应,其值随石墨烯长度的增加而减小,而石墨烯界面传递最大应变以及界面脱黏极限则不受试件尺度的影响.     

Elastic modulus-density relationship for amorphous boron suboxide thin films

Boron suboxide thin films have been deposited on Si(100) substrates by reactive RF magnetron sputtering of a sintered B target in an Ar/O₂ atmosphere. Elastic recoil detection analysis was applied to determine the film composition and density. Film structure was studied by X-ray diffraction and transmission electron microscopy. The elastic modulus, measured by nanoindentation, was found to decrease as the film density decreased. The relationship was affected by tuning the negative substrate bias potential and the substrate temperature during film growth. A decrease in film density, by a factor of 1.55, caused an elastic modulus reduction by a factor of 4.5, most likely due to formation of nano-pores containing Ar. It appears evident that the large scattering in the published data on elastic properties of films with identical chemical composition can readily be understood by density variations. These results are important for understanding the elastic properties of boron suboxide, but may also be qualitatively relevant for other B-based material systems. Received: 22 February 2002 / Accepted: 11 April 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +46-13/288-918, E-mail: denmu@ifm.liu.se     

Anharmonic lattice dynamics in germanium measured with ultrafast x-ray diffraction

Damping of impulsively generated coherent acoustic oscillations in a femtosecond laser-heated thin germanium film is measured as a function of fluence by means of ultrafast x-ray diffraction. By simultaneously measuring picosecond strain dynamics in the film and in the unexcited silicon substrate, we separate anharmonic damping from acoustic transmission through the buried interface. The measured damping rate and its dependence on the calculated temperature of the thermal bath is consistent with estimated four-body, elastic dephasing times (T2) for 7-GHz longitudinal acoustic phonons in germanium.     

Investigation on periodic cracking of elastic film/substrate system by the extended finite element method

Multiple cracking behavior in a thin elastic film bonded to a thick elastic substrate is investigated by the extended finite element method. Stress and stress intensity factor are obtained using a periodic finite element model for the cracked film/substrate system. The influences of various parameters including crack length, film thickness, periodic crack spacing, and relative stiffness of the substrate on the stress and stress intensity factor are discussed in detail. It is demonstrated that the effects of geometric parameters are more sensitive than that of material property. In particular, the crack spacing has a saturation value due to interactions of neighboring cracks and relief of tensile stress in the film. The film/substrate couple with multiple periodic cracks can exhibit a positive potential in improving the durability of the film/substrate system.     

Thermoelastic behavior of a thermoelectric thin-film attached to an infinite elastic substrate

Abstract

This paper examines the thermoelectric behaviour of a thermoelectric thin film bonded to an elastic substrate. A calculation model for thermoelectric thin films is developed based on the singular integral equation method. The interface shear stress is found to exhibit singular behaviour at the ends of the films. Numerical results for the thermal stress distribution in the film and the film/substrate interface are obtained. Effects of film thickness and the substrate to film stiffness ratio on the stress of the film and the stress intensity factor of the interface are identified. The effects of interface electricity conductivity and the elastic–plastic deformation of the film are discussed.     

Direct and inverse measurement of thin films magnetostriction

Two techniques of measurements of thin film magnetostriction are compared: direct, when changes of the substrate curvature caused by the film magnetization are controlled, and inverse (“indirect”), when the modification of the magnetic anisotropy induced by the substrate deformation (usually bending) is measured. We demonstrate how both the elastic strength of the substrate and the effective magneto-mechanical coupling between the substrate deformation and magnetic anisotropy of the film depend on different conditions of bending. Equations to be used for magnetostriction value determination in typical cases are given and critical parameters for the corresponding approximations are identified.     

On the method for determining the true strength of inorganic glasses

The possibility of determining the true structural strength of glass by bending of glass fibers with a defect-free surface is considered. Two methods are compared, viz., the method of transverse three-point bending in which the breaking stress (strength) is determined, and the method of two-point bending in which the breaking strain is determined. In the latter case, the dependence of the elastic modulus on strain is required for determining the breaking stress (strength). The strength measured in three-point bending is compared with the strength calculated from the breaking strain measured in two-point bending. It is shown that the measurements based on these two methods give close values of strength for defect-free silica fibers used as optical waveguides. The observed difference of ～12% in the values of strength is explained by the difference in the loading rates obtained using these two methods. The advantages and disadvantages of these two techniques are analyzed.     

Electroless plating of copper on surface-modified glass substrate

This work focuses on developing a novel convenient method for electroless copper deposition on glass material. This method is relied on the formation of amino (NH₂)-terminated film on the surface of glass substrate, by coating polyethylenimine (PEI) on glass matrix and using epichlorohydrin (ECH) as cross-linking agent. The introduced amino groups can effectively adsorb the palladium, the catalysts which could initiate the subsequent Cu electroless plating, onto the glass substrate surface. Finally, a copper film is formed on the palladium-activated glass substrate through copper electroless plating and the surface-coppered glass material is therefore acquired. X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscopy (SEM) images combined with energy diffraction X-ray (EDX) analysis demonstrate the successful copper deposition on the surface of glass substrate.