A new methodology for the near-surface strain measurement on Pd-Ag-Sn alloy

With the development of modern synchrotron sources, high-energy X-ray diffraction plays an important role in the residual stresses analysis of materials. This paper deals with the development of a new high-energy synchrotron X-ray diffraction (HESXRD) stress evaluation method for improving the near-surface strain measurement. For this purpose a new Monte Carlo simulation program has been developed to modelize any synchrotron radiation instrument. Futhermore conventional X-ray diffraction measurements have also been carried out after chemical etching, to define the surface and in-depth stresses of the sample, thus giving a reference to test the synchrotron radiation measurements. It has been shown that the reliability of this method is better than 5 μm. This method has been applied to a machined palladium alloy (Pd-Ag-Sn) plate substrate.     

Residual stresses and white layer in electric discharge machining (EDM)

The effect of dielectric liquid and electrode type on white layer structure in electric discharge machined surfaces has been studied in terms of retained austenite and residual stresses using X-ray diffraction method. The machining tests were conducted by using two different tool electrodes (copper and graphite) and dielectric liquid (kerosene and de-ionized water) under same operational conditions. The present work suggests that the surface is saturated with carbon irrespective of the tool electrode material when machining with kerosene dielectric liquid. But, retained austenite is formed on the surface due to carbon uptake from graphite tool electrode when machining with de-ionized water dielectric liquid. On the other hand, even though surface residual stresses increase with structural non-homogeneities in the white layer, no clear consequences have been observed in residual stress distribution beneath the white layer.     

Microstructure of ferroelectric domains in BaTiO3 observed via x-ray microdiffraction

X-ray microdiffraction utilizing Fresnel zone plate focusing optics has been used to study microstructural properties of individual 90 degree ferroelectric domains in BaTiO3. Diffraction measurements at a microfocused spot resolution of 0.3 microm over domain widths of approximately 10 microm unambiguously reveal features of lattice buckling, rotation, and strain near domain boundaries. Our results may be understood within the context of bound residual strain due to lattice mismatch and elastic interactions between neighboring domains.     

工艺参数对PC光学制品残余应力的影响

先通过光弹实验测量残余应力的分布形态,然后通过应力—光学定律计算出相应的残余应力值,最后把该数值做了数值模拟分析。研究表明:对于同一工艺参数,残余应力的数值从浇口附近至流动末端逐渐减小;对于不同工艺参数,对残余应力的影响程度从大到小的顺序为熔体温度、模具温度、注射压力、冷却时间。     

Stress anisotropy in circular planar magnetron sputter deposited molybdenum films and its annealing effect

As part of the program to develop a free-standing thin-film filter for soft X-ray optics application, stress anisotropy in the molybdenum films deposited by dc circular planar magnetron sputtering were studied by X-ray diffraction (XRD) as a function of sputtering argon gas pressure over a range of 0.8–1.5 Pa. Surface morphology of the films has been investigated by optical microscopy and scanning tunneling microscopy (STM). It is found that, for the film deposited at 0.8 Pa pressure, the stresses are more compressive in the tangential than in the radial direction; the highest compressive stress exists in the center area. The film deposited at 1.5 Pa pressure has the highest stress anisotropy, and the stresses are less tensile in the tangential than in the radial direction. Annealing in vacuum is more effective in reducing tensile stress and stress anisotropy in the tensile stressed film than in the compressively stressed film. Received: 14 September 2001 / Accepted: 21 January 2002 / Published online: 5 July 2002 RID="*" ID="*"Corresponding author. Fax: +86-21/6598-6323, E-mail: ygwu@mail.tongji.edu.cn     

Development of Hard X-ray Focusing Optics at Diamond Light Source

The short wavelength of X-rays makes them an excellent choice for probing materials on the nanometer scale and for crystallography of sub-micrometer crystallites. The objective of nanofocusing optics is to produce a small, focused beam size in order to obtain the highest X-ray flux on a small sample or as a fine spatial probe. Achieving nanometer-scale focused X-ray beam sizes puts great demands on the optical elements in an X-ray beamline—the optics must balance the requirements to de-magnify the electron beam X-ray source, to reduce the diffraction-limited focus size, and to minimize the contribution to the focus of aberrations in the optics while collecting the maximum X-ray flux into the focused beam. These requirements dictate that an extreme demagnifying geometry should be employed and that high-specification optical elements must be used. Nanofocusing optics has often been added as an upgrade to existing beamlines at Diamond, extending the range of science that can be carried out. Extreme nanofocusing also forms the basis of new beamlines at Diamond, such as the nanoprobe beamline (I14), which aims to provide sub-30-nm-dimension focused X-ray beams for mapping samples at high spatial resolution. The demand for nanometer-scale diffraction-limited X-ray beams is expected to grow at Diamond and requires corresponding advances in X-ray optics to exploit the present source and future lower emittance storage ring sources; for example, the proposed Diamond II upgrade, projected to give a factor 20 emittance reduction.     

退火参数对熔石英透射波前和损伤阈值的影响

 采用高温退火技术去除熔石英元件表面由于CO2激光修复带来的残余应力,研究了退火环境对元件的表面污染,分析了不同退火温度（600～900 ℃）和保温时间（3～10 h）对于元件残余应力、透射波前、表面粗糙度和激光损伤阈值的影响。结果表明:在800 ℃以下,高温退火10 h可有效去除CO₂激光修复带来的残余应力,对元件的透射波前和表面粗糙度无明显影响;石英保护盒能有效减少退火环境对元件表面产生的污染,但仍有X射线光电子能谱检测不到的表面污染物存在;在退火后采用质量分数为1%的HF刻蚀15 min,激光损伤阈值可恢复,同时元件透射波前和表面粗糙度并无明显的增加。     

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.     

Thermal evolution of residual stress in IN718 alloy subjected to laser peening

The thermal relaxation behaviors of residual stresses induced by laser peening (LP) in IN718 alloy were investigated using an integrated numerical simulation and experimental approach. LP and heat treatments (HT) were carried out after which the X-ray diffraction (XRD) technique was employed in measuring the residual stresses. Micro-structures were observed using an optic microscope (OM) and transmission electron microscope (TEM). Dislocations induced by LP were also observed by TEM and characterized using the XRD technique. The effects of the applied temperature and the exposure time on residual stress and micro-structures were investigated. The results show that the extent of the residual stresses relaxation increased accordingly with the increase in the applied temperature. The relaxation rate was initially high and tended to stabilize for a longer exposure time. Grain size evolution during the process was subsequently discussed. Furthermore, a conceivable mechanism of residual stresses thermal relaxation behavior was obtained.     

激光冲击诱导弹簧钢丝残余应力状态分析

利用高功率Nd:YAG激光对不同工艺处理的SWOSC-V弹簧钢丝进行单点冲击处理,用X射线应力分析仪测量弹簧内外侧、侧表面的残余应力并计算出残余主应力,建立了激光冲击SWOSC-V弹簧钢丝表面残余应力的产生模型,并利用该模型分析了弹簧钢丝表面残余应力产生的原因。结果表明:弹簧钢丝在经激光冲击处理的表面强化区产生残余压应力,钢丝退火后直接激光冲击处理与经喷丸强化的钢丝激光冲击处理的表面残余应力变化不同,喷丸强化所引起的材料硬化是激光冲击处理弹簧钢丝残余应力变化不同的原因。     

一种毛细管聚焦的便携式微束X射线荧光谱仪

基于毛细管X光透镜技术的便携式能量色散X射线荧光分析因其无损分析等优点成为分析文物样品的有利工具。但由于文物样品的表面不平整或弧度以及毛细管X光透镜聚焦X射线的特点，导致在测量过程中样品测量点与毛细管X光透镜出端之间的距离产生变化，引起照射样品的X射线束斑大小发生改变，从而影响测量结果的准确性和元素区域扫描的分辨率。介绍了本实验室自行研发的一种新型便携式微束X射线荧光谱仪，此谱仪主要是由SDD X射线探测器、30 W低功率X射线管、毛细管X光透镜、CCD和一个新型闭环控制系统构成。该闭环控制系统是在激光位移传感器能够精确控制样品测量点到毛细管X光透镜出端距离的基础上，结合LabVIEW语言环境下开发的计算机控制程序以及步进电机、样品台等器件组成。基于此系统，该实验室研发的便携式微束X射线荧光谱仪在测量过程中可以时刻保证照射样品的X射线光斑大小固定不变。同时，该谱仪还可以通过调整样品测量点到透镜出端的距离来选择不同尺寸的X射线照射光斑。为了验证设备的可行性，使用该便携式微束X射线荧光谱仪在激活激光位移传感器和关闭激光位移传感器两种情况下测量了一块表面不平整古陶瓷样品釉彩层中K，Ca，Zn和Fe等元素的含量及分布，并将测量结果进行了对比。结果显示，在激活激光位移传感器的情况下测得的样品微区元素含量与真实值较接近，扫描区域元素分布图的分辨率更好，表明本谱仪基于激光位移传感器开发的自动调整样品测量点到透镜出口端距离的闭环控制系统能有效的减少由于样品表面不平整或弧度带来的测量误差，弥补了现有微束X射线荧光谱仪在此方面的不足。因此，本便携式微束X射线荧光谱仪在无损分析检测文物方面具有潜在的应用前景。     

Fabrication of nested elliptical KB mirrors using profile coating for synchrotron radiation X-ray focusing

This paper describes fabrication methods used to demonstrate the advantages of nested or Montel optics for micro/nanofocusing of synchrotron X-ray beams. A standard Kirkpatrick-Baez (KB) mirror system uses two separated elliptical mirrors at glancing angles to the X-ray beam and sequentially arranged at 90° to each other to focus X-rays successively in the vertical and horizontal directions. A nested KB mirror system has the two mirrors positioned perpendicular and side-by-side to each other. Compared to a standard KB mirror system, Montel optics can focus a larger divergence and the mirrors can have a shorter focal length. As a result, nested mirrors can be fabricated with improved demagnification factor and ultimately smaller focal spot, than with a standard KB arrangement. The nested system is also more compact with an increased working distance, and is more stable, with reduced complexity of mirror stages. However, although Montel optics is commercially available for laboratory X-ray sources, due to technical difficulties they have not been used to microfocus synchrotron radiation X-rays, where ultra-precise mirror surfaces are essential. The main challenge in adapting nested optics for synchrotron microfocusing is to fabricate mirrors with a precise elliptical surface profile at the very edge where the two mirrors meet and where X-rays scatter. For example, in our application to achieve a sub-micron focus with high efficiency, a surface figure root-mean-square (rms) error on the order of 1 nm is required in the useable area along the X-ray footprint with a ∼0.1 mm-diameter cross section. In this paper we describe promising ways to fabricate precise nested KB mirrors using our profile coating technique and inexpensive flat Si substrates.     

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.     

X-ray topographic identification and measurement of plastic strains and elastic stresses in single crystallites of polycrystalline diamond layers

The well-known phenomenon of asterism is used as the basis for the development of an X-ray topographic method to identify and measure plastic strains and residual elastic stresses in single crystallites more than 3 μm in size in polycrystalline diamond layers. The amount of asterism is used as a quantitative measure of plastic strains in crystallites. The distribution of crystallites over the amount of asterism in 40-to 670-μm-thick microwave-plasma-deposited polycrystalline diamond layers is obtained. Shear plastic strains, which cause a misorientation from 0.4′ to 1.5° between different areas of a crystallite, are observed for the first time. The residual elastic stresses calculated in plastically strained crystallites vary between 2.7 kPa and 0.84 GPa.     

自适应光学对大气扰动波前的补偿效果研究：I.理论推导

在采用冻结湍流假设和几何光学近似的条件下，得到了经自适应光学系统校正后的剩余波前相位扰动的结构函数，进而根据剩余相位结构函数与系统Ｓｔｒｅｈｌ比的关系，求出自适应光学系统的补偿效果受系统的时空传递函数，大气湍流，光波传播路径上的横向风，观察目标的旋转角速度以及系统时间延迟影响情况的解析表达式。     

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 laser surface hardening on the microstructure, hardness and residual stresses of austempered ductile iron grades

A study of the laser surface hardening process of two austempered ductile iron grades, with different austempering treatments has been carried out. Hardening was performed with an infrared continuous wave Nd:YAG laser in cylindrical specimens. The microstructure of the laser hardened samples was investigated using an optical microscope, microhardness profiles were measured and surface and radial residual stresses were studied by an X-ray diffractometer. Similar results were achieved for both materials. A coarse martensite with retained austenite structure was found in the treated area, resulting in a wear resistant effective layer of 0.6 mm to 1 mm with a microhardness between 650 HV and 800 HV. Compressive residual stresses have been found at the hardened area being in agreement with the microhardness and microstructural variations observed. The achieved results point out that the laser surface hardening is a suitable method for improving the mechanical properties of austempered ductile irons.     

High energy X-ray micro-optics

A tremendous progress in X-ray optics development was made in the past decade. Progress has been driven by the unique properties of X-ray beams produced by third generation synchrotron sources. The very low emittance coupled with high brilliance allows one to develop efficient focusing devices for new X-ray microscopy techniques. This article provides an overview of the state-of-the-art in micro-focusing optics and methods for hard X-rays. The main emphasis is put on those methods which aim to produce submicron and nanometer resolution. These methods fall into three broad categories: reflective, refractive and diffractive optics.The basic principles and recent achievements are discussed for all optical devices. To cite this article: A. Snigirev, I. Snigireva, C. R. Physique 9 (2008).     

High efficiency antireflection coating in MWIR region (3.6–4.9 μm) simultaneously effective for Germanium and Silicon optics

Antireflection coatings have critical importance in thermal imaging system working in MWIR region (3–5 μm) since optics of high refractive index materials are used. Germanium (Ge) and Silicon (Si) optics are used extensively in the MWIR thermal systems. In this paper a study has been carried out on the design and fabrication of multi-substrate antireflection coating effective for Germanium and Silicon optics in MWIR (3.6–4.9 μm) region. The wave band 3.6–4.9 μm is chosen for the reported work because detector system used in MWIR region has a band selection filter effective in the same wavelength region and atmospheric transmission window in MWIR region is effective in 3–5 μm spectral band. Comprehensive search method was used to design the multilayer stack on the substrate. The coating materials used in the design were Germanium (Ge), Hafnium oxide (HfO₂) and Y-Ba-Fluoride (IR-F625). The fabrication of coating was made in a coating plant fitted with Cryo pump system and residual gas analyzer (RGA). The evaporation was carried out at high vacuum (2–6 × 10^?6 mbar) with the help of electron beam gun system and layer thicknesses were measured with crystal monitor. The result achieved for the antireflection coating was 98.5% average transmission in 3.6–4.9 μm band for Germanium and Silicon optics. This work will be helpful in reducing the plant operation time, material and power consumption, as two different kinds of optics are simultaneously coated in a single coating cycle.     

Effect of Young's modulus evolution on residual stress measurement of thermal barrier coatings by X-ray diffraction

Subjected to thermal cycling, the apparent Young's modulus of air plasma-sprayed (APS) 8 wt.% Y₂O₃-stabilized ZrO₂ (8YSZ) thermal barrier coatings (TBCs) was measured by nanoindentation. Owing to the effects of sintering and porous microstructure, the apparent Young's modulus follows a Weibull distribution and changes from 50 to 93 GPa with an increase of thermal cycling. The evolution of residual stresses in the top coating of an 8YSZ TBC system was determined by X-ray diffraction (XRD). The residual stresses derived from the XRD data are well consistent with that obtained by the Vickers indention. It is shown that the evolution of Young's modulus plays an important role in improving the measurement precision of residual stresses in TBCs by XRD.