Annealing effects on residual stress of HfO2/SiO2 multilayers

HfO2/SiO2 multilayer films were deposited on BK7 glass substrates by electron beam evaporation method.The effects of annealing at the temperature between 200 and 400℃ on residual stresses have been studied.It is found that the residual stress of as-deposited HfO2/SiO2 multilayers is compressive.It becomes tensile after annealing at 200℃,and then the value of tensile stress increases as annealing temperature increases.And cracks appear in the film because tensile stress is too large when the sample is annealed at 400℃.At the same time,the crystallite size increases and interplanar distance decreases with the increase of annealing temperature.The variation of residual stresses is corresponding with the evolution of structures.     

磁控溅射制备极紫外高反射率多层膜应力研究

为制备硼边附近6.7 nm波长的极紫外高反射率多层膜反射镜,研究了Mo_2C/B_4C,Mo/B_4C周期多层膜,重点解决薄膜应力难题。采用直流磁控溅射技术制备了膜层厚度为30 nm的Mo,Mo_2C,B_4C,单层膜,周期厚度为3.5 nm,30对的Mo_2C/B_4C,Mo/B_4C周期多层膜。利用台阶仪测试了镀膜前后基底面形,计算并比较了不同薄膜样品的应力值。结果表明Mo_2C/B_4C多层膜压应力要远小于Mo/B_4C多层膜,且成膜质量与Mo/B_4C相当。因此Mo_2C/B_4C是应用于6.7 nm反射镜较好的多层膜材料组合。     

极紫外多层膜残余应力初步研究

 针对极紫外多层膜在激光等离子体诊断、极紫外光刻等方面的应用,进行了Mo/Si多层膜残余应力的实验研究,讨论了多层膜残余应力的成因。实验结果表明：Mo单层膜表现为张应力, Si单层膜表现为压应力;通过传统方法制备的13.0 nm处高反射率的40对Mo/Si多层膜会产生-500 MPa左右的压应力,其压应力主要是由膜层之间的贯穿扩散引起的;通过改变膜层比率可以在一定程度上补偿因贯穿扩散产生的压应力,但是以牺牲多层膜反射率为代价。     

磁控溅射制备的W,WSi2,Si单层膜和W/Si,WSi2/Si多层膜应力

采用直流磁控溅射技术制备了厚度约100 nm的W,WSi2,Si单层膜和周期约为20 nm,Si膜层厚度与周期的比值为0.5的W/Si,WSi2/Si周期多层膜.利用台阶仪对镀膜前后基底表面的面形进行了测试,计算并比较了不同膜系的应力值.结果表明:W单层膜表现出较大的压应力,而W/Si周期膜则表现为张应力.WSi2单层...     

Structure evolution and mechanical properties enhancement of Al/AlN multilayer

A set of Al/AlN multilayers with various modulation periods were prepared using DC magnetron sputtering method. Low angle X-ray diffraction (LAXRD) was used to analyze the layered structure of multilayers. The phase structure of the films was investigated with grazing angle X-ray diffraction (GAXRD). LAXRD results indicate that well-defined multilayer modulation structures are formed for the relatively larger modulation periods. However, the loss of mutilayered structure is detected in the multilayer with low modulation period. A very wide amorphous peak is observed in multilayer with modulation period of 4 nm. The multilayers show obvious crystallization at larger modulation periods, however, the diffraction peaks are much wider than the Al single layer because of the interruption of the continuous columnar grain growth by alternating deposition processes. Nanoindentation experiments were performed to study the mechanical properties as a function of multilayer modulation period. It is found that the hardness of the multilayers is greater than the hardness calculated from rule of mixtures. With the modulation periods adjusted, the multilayers are even harder than its hard component (AlN). A maximum hardness of 24.9 GPa, about 1.9 times larger than its hard component (AlN) and 3.7 times larger than the hardness calculated from the rule of mixtures, is found at the multilayer with modulation period of 16 nm. The wear test results show that the multilayers possess lower and stable friction coefficient, and superior wear properties.     

Characterization of the surface topography and nano-hardness of Cu/Ni multilayer structures

This article describes the results of a study of Cu/Ni multilayer coatings applied on a monocrystalline Si(100) silicon substrate by the deposition magnetron sputtering technique. Composed of 100 bilayers each, the multilayers were differentiated by the Ni sublayer thickness (1.2 to 3 nm), while maintaining the constant Cu sublayer thickness (2 nm). The multilayer coatings were characterized by assessing their surface topography using atomic force microscopy and their mechanical properties with nano-hardness measurements by the Berkovich method. The tests showed that the hardness of multilayers was substantially influenced by the thickness ratio of Cu and Ni sublayers and by surface roughness. The highest hardness and, at the same time, the lowest roughness was exhibited by a multilayer structure with a Cu-to-Ni sublayer thickness ratio of 2:1.5.     

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     

Effect of substrate temperature on the magnetic properties and internal stresses of CoPt/AlN multilayer deposited by dc magnetron sputtering

Magnetic properties and internal stresses of AlN(20 nm)/[CoPt(2 nm)/AlN(20 nm)]₅ multilayer structure deposited at different substrate temperatures by dc magnetron sputtering have been studied. It is found that with increasing the substrate temperature from room temperature to 400 °C, in-plane magnetic anisotropy field of the film becomes smaller, and the out-of-plane magnetization becomes stronger. Especially when the film is deposited at substrate temperature of 400 °C, the out-of-plane magnetization becomes as strong as the in-plane magnetization. On the other hand, the total in-plane residual stress of the film changes gradually from compressive to tensile. The compressive intrinsic stress is generated during deposition process and decreases with increasing the substrate temperature. After annealing at high temperatures, the films show strong perpendicular magnetic anisotropy. With increasing the annealing temperature, the in-plane thermal stress also increases and becomes dominant, which is considered to result in the perpendicular magnetic anisotropy of the films.     

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.     

Change of surface properties of high-chromium cast iron under conditions of laser treatment and wear in a pellet stream

We investigate the influence of laser treatment on the formation of residual stresses relative to the changing structure-phase composition in the surface layers of high-chromium cast iron with 16% chromium. We show that appreciable tensile stresses are produced in the region of the laser action and that their distribution depends on whether the laser treatment was or was not accompanied by surface melting. The produced residual stresses are responsible for the formation of a large number of cracks. Preheating to 400°C lowers the level of the tensile residual stresses and prevents crack formation. A pellet stream acting on the surface produces cold-work hardening layers in which the tensile stresses change into compressive ones. The depth, hardness, and magnitude of the compressive residual stresses depend on the method used to work harden the cast iron and on the angle of attack of the pellet as it acts on the surface.Translation of Preprint No. 195, Lebedev Institute of Physics, Academy of Sciences of the USSR.     

Microstructure, hardness and stress in melted zone of 42CrMo steel by wide-band laser surface melting

Using laser surface melting (LSM) of a roller, to obtain the desired distribution of the microstructure, hardness and residual stresses with minimum distortion, is essential in order to improve machining efficiency and to achieve reliable service performance. In this study, a 3D finite element model has been developed to simulate the wide-band LSM process and predict the thermal and mechanical properties in the melted zone. The microstructure evolution, hardness distribution and stress field in the melted zone with different laser power were simulated. With the increase of the laser power from 3000 to 3800 W, the width and the depth of the laser melted layer increase, while the laser power has a little effect on the martensite contents, which exceed 90% in the melt-hardened zone. It greatly affects the mechanical properties in the melt-hardened zone with its volumetric expansion effect and the hardness increases by 2-3 times. The residual stress distributed within the melt-hardened zone is always of the compressive type. The amplitude of compressive stress exists in the transition region, and the amplitude of von Mises stress within the heat affected-zone (HAZ) decreases with the increase in laser power. The accuracy of the developed finite element simulation strategy is validated for phase proportion and hardness distributions through the wide-band LSM on roller steel with proper instrumentation for data measurement. This agreement is encouraging.     

Effects on the evolution of microstructure and properties of low-silicon cast aluminum alloys in service

ABSTRACT

The microstructure evolution and property change of four kinds of low silicon cast aluminum alloy exposed to heat for 0–50?h at 200°C were studied by means of Brinell hardness test, tensile property test, friction and wear property test and XRD analysis. The results show that with increasing thermal exposure time, the tensile strength of each group of samples decreased and the amount of wear increased. The tensile strength of samples with more Si content decreased slowly. When the time increased to 50?h, the increase of wear loss was the largest. The hardness of samples after thermal exposure increases compared with that before thermal exposure. The residual stress of (311) diffraction crystal surface of AlSi3.5Mg0.66 under different thermal exposure time was measured. The type of residual stress changed from residual tensile stress to residual compressive stress after thermal exposure. There is an abnormal phenomenon that the hardness of the sample increased and the amount of wear increased, and it is evident that the distribution of residual stress was inhomogeneous after thermal exposure. It is found that with increasing thermal exposure time to 50?h, the average lattice distortion ε of the low-index crystal plane and the high-index crystal plane in the aluminum alloys gradually increased.     

Stress analysis of ZrO2/SiO2 multilayers deposited on different substrates with different thickness periods

The effects of repeating thickness periods on stress are studied in ZrO2/SiO2 multilayers deposited by electron-beam evaporation on BK7 glass and fused-silica substrates. The results show that the residual stress is compressive and decreases with an increase of the periods of repeating thickness in the ZrO2/SiO2 multilayers. At the same time, the residual stress in multilayers deposited on BK7 glass is less than that of samples deposited on fused silica. The variation of the microstructure examined by x-ray diffraction shows that microscopic deformation does not correspond to macroscopic stress, which may be due to variation of the interface stress.     

一种在线测量微机械薄膜残余应力的新结构

提出了一种利用临界屈曲法在线测量微机械薄膜残余应力的新结构，并采用表面微加工技术制作了两种测试样品.搭建了在线观测实验装置来实时监控释放过程中结构出现的临界屈曲变形模态，由此判断出结构内部的应力状态，同时在测得临界刻蚀深度的情况下，采用有限元方法计算出残余应力大小.借助有限元方法，先研究了多个参数对临界屈曲应力的影响，然后利用这种新结构对薄膜残余应力进行了实际测量，所得结果与微旋转结构的应力测量结果基本吻合.分析及实验表明，新结构在测量薄膜残余应力方面有许多优点，具有较高的实用价值，不仅能满足大量程的应力检测要求，而且只用一个结构就可以同时测量压应力和拉应力，从而极大提高了器件版图空间的利用率.     

Analysis by speckle interferometry of the dependency of yield stress on residual stress

We used electronic speckle pattern interferometry (ESPI) to measure in situ displacement fields nondestructively and with high resolution (10⁻² μm) by using the interferometry principle and the phase-shift technique. We measured the depth profile of the residual stress in steel pipe manufactured by thermomechanically controlled processing using a quantitative model, which explains the relationship between residual stress and displacement measured by ESPI in chemical etching. We analyzed the variation of yield stresses measured by the indentation technique and the residual stresses at various depths. The relationship between the residual stresses and the yield stresses was consistent with simulated results and can be used for indirect evaluation of the residual stresses from the yield stresses.     

ZrO2／SiO2多层膜中膜厚组合周期数及基底材料对残余应力的影响

ZrO₂／SiO₂多层膜由相同沉积条件下的电子束蒸发方法制备而成， 通过改变多层膜中高(ZrO₂)、低(SiO₂)折射率材料膜厚组合周期数的方法，研究了沉积 在熔石英和BK7玻璃 基底上多层膜中残余应力的变化. 用ZYGO光学干涉仪测量了基底镀膜前后曲率半径的变化， 并确定了薄膜中的残余应力. 结果发现，该多层膜中的残余应力为压应力，随着薄膜中膜厚 组合周期数的增加，压应力值逐渐减小. 而且在相同条件下，石英基底上所沉积多层膜中的 压应力值要小于BK7玻璃基底上所沉积多层膜中的压应力值. 用x射线衍射技术测量分析了膜 厚组合周期数不同的ZrO₂／SiO₂多层膜微结构，发现随着周期数增 加，多层膜的结晶程 度增强. 同时多层膜的微结构应变表现出了与所测应力不一致的变化趋势，这主要是由多层 膜中，膜层界面之间复杂的相互作用引起的. 关键词： 2／SiO₂多层膜')" href="#">ZrO₂／SiO₂多层膜 残余应力 膜厚组合周期数     

连续梯度的功能层对燃料电池在初始还原过程中曲率及残余应力的影响

连续梯度的电极由于其相对于多层梯度电极能更加有效地缓解电极和电解质的热失配及改善界面黏接而受到特别的关注. 本文通过建立含连续梯度的阳极功能层的阳极支撑固体氧化物燃料电池的力学模型, 研究了连续梯度的阳极功能层对阳极支撑固体氧化物燃料电池半电池在初始还原过程中曲率及残余应力的影响. 结果表明电池的曲率在初始还原过程中随还原程度的增大而逐渐增大. 连续梯度的阳极功能层的引入不能同时改善电池的曲率和残余应力, 即连续梯度的阳极功能层在缓解应力的同时会导致曲率的增大, 反之亦然. 含有连续梯度的阳极功能层的电池在部分还原状态下, 梯度层/阳极支撑界面处具有最大的拉应力容易导致电池受损, 实际中应保证电池被完全还原.     

Effect of pulsed bias on the properties of ZrN/TiZrN films deposited by a cathodic vacuum arc

ZrN/TiZrN multilayers are deposited by using the cathodic vacuum arc method with different substrate bias(from 0 to 800 V),using Ti and Zr plasma flows in residual N 2 atmosphere,combined with ion bombardment of sample surfaces.The effect of pulsed bias on the structure and properties of films is investigated.Microstructure of the coating is analyzed by X-ray diffraction(XRD),and scanning electron microscopy(SEM).In addition,nanohardness,Young’s modulus,and scratch tests are performed.The experimental results show that the films exhibit a nanoscale multilayer structure consisting of TiZrN and ZrN phases.Solid solutions are formed for component TiZrN films.The dominant preferred orientation of TiZrN films is(111) and(220).At a pulsed bias of 200 V,the nanohardness and the adhesion strength of the ZrN/TiZrN multilayer reach a maximum of 38 GPa,and 78 N,respectively.The ZrN/TiZrN multilayer demonstrates an enhanced nanohardness compared with binary TiN and ZrN films deposited under equivalent conditions.     

Structure and mechanical properties of Al/AlN multilayer with different AlN layer thickness

Nanometer scale Al/AlN multilayers have been prepared by dc magnetron sputtering technique with a columnar target. A set of Al/AlN multilayers with the Al layer thickness of 2.9 nm and the AlN layer thickness variation from 1.13 to 6.81 nm were determined. Low angle X-ray diffraction (LAXRD) was used to analyze the layered structure of multilayers. The phase structure of the coatings was investigated with grazing angle XRD (GAXRD). Mechanical properties of these multilayers were thoroughly studied using a nanoindentation and ball-on-disk micro-tribometer. It was found that the multilayer hardness and reduced modulus showed no strong dependence on the AlN layer thickness. Al2.9 nm/AlN1.13 nm multilayer had more excellent tribological properties than single layers and other proportion multilayers with a lowest friction coefficient of 0.15. And the tribological properties of all the multilayers are superior to the AlN single layer.     

Control of the structure and stress state of thin films and coatings in the process of their preparation by ion-plasma methods

A system analysis of the influence of the substrate temperature during deposition on two main factors (nanodimensionality of structural aggregates and high stresses) responsible for the nonequilibrium state of the materials of ion-plasma-deposited films and coatings has been performed. It has been shown that an increase in the temperature during deposition leads to a preferred growth of nanocrystallites in the direction of incidence of film-forming particles, which, in turn, results in the formation of an anisometric crystal structure. The main causes of the generation of high elastic stresses in ion-plasma condensates are the ion/atom bombardment in the process of deposition (which stimulates the development of compressive stresses) and the difference in the thermal expansion coefficients of the condensate and substrate materials (which initiates the development of thermal stresses; the sign is determined by the difference between the thermal expansion coefficients of the condensate and substrate materials). An increase in the temperature during deposition results in the relaxation of compressive stresses stimulated by the ion/atom bombardment and in an enhancement of the influence of thermal stresses on the state of the ion-plasma condensate. This makes it possible to control the stress state of ion-plasma films and coatings by purposefully varying the substrate temperature during deposition.