高强双相钢氩离子抛光EBSD制备研究

利用Gatan公司的685型多功能氩离子抛光镀膜仪对铁素体-马氏体高强双相钢EBSD样品进行制备。采用正交法研究了氩离子加速电压、抛光时间以及入射角度对高强双相钢EBSD衍射花样标定率的影响。结果表明,随着加速电压、抛光时间及氩离子入射角度的增加,可有效地降低砂纸打磨痕迹对EBSD衍射花样标定的影响,且花样标定率明显提高,试样表面平整度增加。

Analysis of Orange Peel Defect in St14 Steel Sheet by Electron Backscattered Diffraction (EBSD)

In this paper, the orange peel defect in the surface range of the st14 steel sheet has been investigated using the electron backscattered diffraction (EBSD) technique. It has been found that the orange peel defect in the st14 steel sheet was resulted from the local coarse grains which were produced during hot-rolling due to the critical deformation in dual-phase zone. During deep drawing, the coarse grains with {100}<001> microtexture can slip on the {112}<111> slip system to form bulging and yields orange peel defects, while the coarse grains with {112}<110> orientation do not form the defect as the Schmid factor of {112}<111> slip system in it equals zero.

Analysis of surface orange peel of aluminum-alloy automobile sheet by using of EBSD and X-ray diffraction

The formation cause of orange peel of aluminum-alloy automotive sheet after tensile deformation was analysed by using X-ray diffraction and electron back-scattered diffraction(EBSD).The test results showed that formation cause of surface orange peel after tensile deformation related to product texture and nonuniform deformation during the tensile process.The grain size has significant effect on deformation uniform and texture formation.Coarse grains were easy to produce nonuniform deformation and texture,which would produce surface orange peel after tensile deformation.

电解铜箔截面微观组织的EBSD分析

目的通过树脂包埋结合离子截面抛光的制备方法,实现铜箔样品的截面EBSD分析,进而利用截面EBSD分析方法探究电流密度对铜箔组织性能的影响。方法通过使用热固性树脂对铜箔进行包埋,使用加热平台使胶体凝固,对得到的包埋好的铜箔试样在砂纸上进行截面打磨,放入截面离子抛光仪中进行离子切割,样品制备完成后,将样品取下。使用电子背散射(EBSD)作为电镜附件,进行晶体学取向的表征。结果结合截面微观组织的EBSD分析方法,分析了电流密度对铜箔组织性能的影响,结果表明,随着电流密度的增大,电解铜箔的晶粒尺寸呈现出先减小后增大的趋势,孪晶密度和位错密度呈现出先增大后减小的趋势,抗拉强度在45 A/dm^(2)时达到最大547.05 MPa。结论该方法可以利用EBSD分析软件自动分析铜箔截面的晶粒粒度分布、孪晶密度等,并将这些微观结构特征与力学性能结果进行详细对比分析,验证了电流密度对铜箔组织和性能的显著影响。

Application of EBSD technique to ultrafine grained and nanostructured materials processed by severe plastic deformation:Sample preparation, parameters optimization and analysis

With the help of FESEM, high resolution electron backscatter diffraction can investigate the grains/subgrains as small as a few tens of nanometers with a good angular resolution （~0.5°）. Fast development of EBSD speed （up to 1100 patterns per second） contributes that the number of published articles related to EBSD has been increasing sharply year by year. This paper reviews the sample preparation, parameters optimization and analysis of EBSD technique, emphasizing on the investigation of ultrafine grained and nanostructured materials processed by severe plastic deformation （SPD）. Detailed and practical parameters of the electropolishing, silica polishing and ion milling have been summarized. It is shown that ion milling is a real universal and promising polishing method for EBSD preparation of almost all materials. There exists a maximum value of indexed points as a function of step size. The optimum step size depends on the magnification and the board resolution/electronic step size. Grains/subgrains and texture, and grain boundary structure are readily obtained by EBSD. Strain and stored energy may be analyzed by EBSD.

MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTI-TATIVE X-RAY DIFFRACTION PHASE ANALYSIS

A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

AN EXTERNAL STANDARD METHOD OF QUANTITATIVE PHASE ANALYSIS OF THE SAMPLE CONTAINING AN AMORPHOUS PHASE BY X—RAY DIFFRACTION

A new method of the quantitative phase analysis of the sample containing an amorphous phase or a standardless phase by X-ray diffraction is proposed in the paper. The addtion of a reference phase or some analytical phase to the analyzed sample is not required in this method and the experimental results are satisfactory.

X-ray diffraction analysis of cold-worked Cu-Ni-Si and Cu-Ni-Si-Cr alloys by Rietveld method

Cold worked and annealed supersaturated Cu-2.65Ni-0.6Si and Cu-2.35Ni-0.6Si-0.6Cr alloys were studied. The microstructural parameters evolution, including crystallite size, root mean square strain and dislocation density was analyzed using Materials Analysis Using Diffraction software （MAUD）. The parameters for both alloys have typical values of cold deformed and subsequently annealed copper based alloy. A net change of the crystallite size, root mean square strain and dislocation density values of the alloys aged at 450 °C for 2.5-3 h seems corresponding to the recovery and recrystallization processes. Addition of Cr as quaternary element did not lead to any drastic changes of post deformation or ageing microstructural parameters and hence of recovery-recrystallization kinetics.

AN INCREMENTAL METHOD OF X-RAY DIFFRACTION QUANTITATIVE PHASE ANALYSIS OF SAMPLESCONTAINING AMORPHOUS MATERIAL

A new method for quantitative X-ray diffraction phase analysis of a powder misture has been developed according to Popovic's doping method. The weight fraction of amorphous material in the analysed sample is obtained. For a multicomponent system in which (n-2) pure phases are added into an n-phase compnent sample and theweight fractions of all n phases can be determined by the method. The test results of confirmation agree well with the theory.

Influence of X-ray Powder Diffraction Instrument Error on Crystalline Structure Analysis

Standard mica was used to correct the X-ray powder diffraction instrument error and mathematic methods were employed to find the correction equation. By analyzing mullite sample and comparing the corrected and uncorrected analysis results we found the former is obviously more reasonable. So the conclusion is that the X-ray powder diffraction instrument error greatly affects the crystalline structure analysis, and the above method is convenient and effective for the correction of instrument error.

A SOLUTION OF MINIMUM NORM FOR QUANTITATIVE PHASE ANALYSIS BY STANDARDLESS X-RAY DIFFRACTION

A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus,The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.

A SOLUTION OF MINIMUM NORM FOR QUANTITATIVE PHASE ANALYSIS BY STANDARDLESS X-RAY DIFFRACTION

A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus.The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.

An Analysis of Interference as a Source for Diffraction

An analysis is made of interference of two plane waves which in turn give rise to subsequent diffraction phenomena. This is done using two different approaches. One of them is straight forward but is difficult to interpret. The second is less conventional but more intuitive thus giving more insight into the process. The geometry is kept very simple to focus on the process itself. Both approaches give rise to the same results thus offering a choice in tackling such prob-lems.

Analysis of Freely Swimming C. elegans Using Laser Diffraction

Soil and aquatic multicellular microorganisms play a critical role in the nutrient-cycling and organismal ecology of soil and aquatic ecosystems. These organisms live and behave in a complex three-dimensional environment. Most studies of microorganismal behavior, in contrast, have been conducted using microscope-based approaches, which limit the movement and behavior to a narrow, nearly two-dimensional focal field. We report on a novel analytical approach that provides real-time analysis of freely swimming C elegans without dependence on microscope-based equipment. This approach consists of tracking the temporal periodicity of diffraction patterns generated by directing laser light onto nematodes in a cuvette. We measured oscillation frequencies for freely swimming nematodes in cuvettes of different sizes to provide different physical constraints on their swimming. We compared these frequencies with those obtained for nematodes swimming within a small droplet of water on a microscope slide, a strategy used by microscope-based locomotion analysis systems. We collected data from diffraction patterns using two methods: video analysis and real time data acquisition using a fast photodiode. Swimming frequencies of nematodes in a droplet of ionic solution on a microscope slide was confirmed to be 2.00 Hz with a variance of 0.05 Hz for the video analysis method and 0.03 Hz for the real time data acquisition using a photodiode;this result agrees with previously published estimates using microscope-based analytical techniques. We find the swimming frequency of unconstrained worms within larger cuvettes to be 2.37 Hz with a variance of 0.02 Hz. As the cuvette size decreased, so did the oscillation frequency, indicating a change in locomotion when physical constraints are introduced.

Investigation of Changes in the Fine Structure of Graphitizing Carbon Materials during Heat Treatment by X-Ray Diffraction Analysis

The properties of synthetic graphite materials, widely used in advanced fields, are determined by their structure, which is formed in the process of high-temperature (~2500°C) heat treatment. The fine structure of a graphitizing carbon material based on petroleum coke containing 1.3 wt% S at various stages of graphitization was studied by X-ray diffraction analysis. Some of the samples contained the addition of dispersed Fe2O3. It is shown that the heat-treated material in the range 1200°C - 2600°C is heterogeneous, its component composition is determined by the processing temperature and the presence of Fe2O3 additive. The observed dependence of the component composition on the heat treatment temperature suggests that the process of graphitization of the carbon material, apparently, develops through a number of metastable states.

THE DEGREE OF CRYSTALLINITY OF MULTICOMPONENT POLYMERS BY X-RAY DIFFRACTION ANALYSIS

Based on the X-ray scattering intensity theory,the correction factors of the degree of crystallinity formulae of the multicomponent polymers have been clearly defined.The formula of degree of erystallinity of the multicomponent polymers was derived in terms of the WAXD theory ahd improved graphic multipeak resolution methods.The results calculated are compatible with the density measurement.

Simulation of X-ray Diffraction Line Broadening Caused by Stress Gradients and Determination of Stress Distribution by Fourier Analysis

Different physical, mechanical and chemical processes, such as： ion implantation, oxidation, nitridation and others create on the surface of materials residual stress state, characterized by high level and strong gradient. X-ray diffraction method widely used for stress measurements has some difficulties in interpretation of experimental data, when the depth of X-ray penetration is compared with thickness of surface layer where inhomogeneous stress distribution is localized. Early it has been shown by authors that diffraction line broadening occurs when analyzed surface is characterized by strong gradient. The interest to study the diffraction line broadening is connected to the possibility of obtaining information about parameters of surface stress distribution. In the present paper the convolution and deconvolution concepts of Fourier analysis were applied to study X ray diffraction line broadening caused by surface stress gradients. Developed methodology allows determining of stress distribution in superficial layers of materials.

西准噶尔达尔布特断裂南东缘红山岩体“拖尾”构造的成因探究——基于石英EBSD组构的分析

通过地质填图厘清了达尔布特断裂为形成于晚石炭世晚期的左行走滑断裂,红山岩体侵入于晚石炭世早期,前者左行错移改造红山岩体形成了“拖尾”构造。采用野外观察达尔布特断裂伴生构造和红山岩体中发育的剪切构造特征,与基于岩体碱长花岗岩石英EBSD组构测试分析相结合的方式对红山岩体“拖尾”构造的成因进行探究。探究结果表明,红山岩体“拖尾”变形构造是达尔布特断裂左行走滑脆性剪切错移红山岩体所致。

HR3C奥氏体耐热钢晶界蠕变损伤的电子背散射衍射分析

对不同条件下的HR3C奥氏体耐热钢蠕变试样进行性能测试和微观结构观察,研究奥氏体耐热不锈钢蠕变沿晶破坏行为和损伤特征。电子背散射衍射(EBSD)分析结果表明,不同蠕变速度下材料的晶粒尺寸基本不变,未产生择优取向,但高蠕变速度条件下部分孪晶界演变成一般晶界,而低蠕变速度下原始孪晶结构基本保持不变。EBSD分析结果清楚地反映了微观蠕变应变的不均匀性。沿晶微裂纹和蠕变空洞的产生和扩展是最显著的损伤特征,这些损伤现象与不同蠕变速度下的蠕变机制及晶界性质密切相关。

基于X射线荧光光谱-X射线衍射技术的泥土物证分析与区域分类鉴别研究

在法庭科学鉴定领域,土壤、岩石等地球化学相关材料是重要的物证来源。在实际案情分析中,物证材料所提供的信息往往指向未知区域,在没有明确犯罪现场位置的情况下,预测物证的来源是一项极具挑战性的工作。针对地球化学物证信息的未知性,通过建立包含矿物组成、元素含量、地理位置等理化性质和地理信息的数据集,比对案发现场样本信息,快速确定物证样本来源,为案情调查提供有力的技术支持和证据支持。本文采集辽宁沈阳市城市内表层泥土样品(0~10cm),应用X射线荧光光谱法(XRF)和X射线粉晶衍射法(XRD)对泥土物证样本中15种元素(SiO_(2)、Al_(2)O_(3)、CaO、Cu、Zn和Pb等)和矿物成分进行测试分析;借助MapGIS软件绘制元素含量分布图,探讨研究区元素分布特点及影响因素,利用主成分分析法(PCA)对三个研究区域泥土样本进行分类鉴别。结果表明:①通过城市地质填图可以获得准确直观的元素含量分布图,法庭工作者可以比对泥土样本的元素特征,追溯物证来源。②沈阳市泥土物证样本主要由石英、长石、蒙脱石和伊利石组成(88.0%~98.0%),XRD条形热图便于法庭工作者进行大量数据比对分析。③基于主成分分析法对三个研究区域15种元素进行降维分析,在95%的置信区间内实现显著的区域鉴别(第1组F_(1)<0,F_(2)<0;第2组F_(1)>0,F_(2)>0;第三组F_(1)>0,F_(2)<0)。④三个研究区域泥土样本中绿泥石、透闪石、高岭石、方解石和白云石存在显著差异,进一步佐证PCA分析分类的准确性。XRF与XRD的联合应用能够有效地区分城市内不同区域的泥土物证样本,为泥土物证溯源调查提供指向性研究区域,并为缩小调查范围提供重要线索。