CN111678932B - Analysis method of electron back scattering diffraction - Google Patents
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Abstract
Description
技术领域Technical field
本申请涉及金属材料检测技术领域，尤其涉及电子背散射衍射的分析方法。The present application relates to the technical field of metal material detection, and in particular to the analysis method of electron backscattered diffraction.
背景技术Background technique
在扫描电镜中加入背散射电子衍射分析装置(EBSD)，可以用于分析材料的晶体学信息，目前已在金属材料微观组织及织构表征中得到了广泛应用。EBSD的分辨率包括空间分辨率和角度分辨率，其中的空间分辨率是指EBSD可以分辨的最小晶粒的尺寸，决定了在EBSD分析时适用的扫描步长。一般来说，EBSD的空间分辨率主要取决于入射电子束的束斑尺寸，若电子束束斑的尺寸越大，则空间分辨率越小；另外，EBSD的空间分辨率还与样品的原子序数有关，原子序数越小，背散射电子产生范围越大，同等参数条件下其分辨率会降低。故而，明确扫描电镜在当前工况下的EBSD的空间分辨率，基于此确定合理的分析参数，可以更准确的进行材料显微组织的EBSD检测分析。Adding a backscattered electron diffraction analysis device (EBSD) to the scanning electron microscope can be used to analyze the crystallographic information of the material. It has been widely used in the microstructure and texture characterization of metal materials. The resolution of EBSD includes spatial resolution and angular resolution. The spatial resolution refers to the size of the smallest grain that EBSD can resolve, which determines the scanning step size applicable in EBSD analysis. Generally speaking, the spatial resolution of EBSD mainly depends on the beam spot size of the incident electron beam. If the size of the electron beam spot is larger, the spatial resolution will be smaller. In addition, the spatial resolution of EBSD is also related to the atomic number of the sample. Relevantly, the smaller the atomic number is, the wider the range of backscattered electrons will be, and its resolution will be reduced under the same parameter conditions. Therefore, by clarifying the spatial resolution of EBSD of the scanning electron microscope under the current working conditions, and determining reasonable analysis parameters based on this, we can more accurately conduct EBSD detection and analysis of the material microstructure.
目前EBSD的空间分辨率的确定方法是计算衍射花样的像素相关性，即选取材料中的孪晶界，在孪晶界两侧区域采集衍射花样和在远离孪晶界处采集参比花样，然后采用像素相关公式计算衍射花样与参比花样之间的相关系数曲线，再利用相关系数曲线计算出空间分辨率。然而，利用像素相关性计算空间分辨率比较复杂，涉及到对相关性曲线进行傅里叶变换、高斯滤波和反傅里叶变换；另一方面，许多金属材料的组织中并不存在孪晶界或孪晶界不易找到，故而增加了此方法的应用难度。故而，需要一种更加简单、快捷的空间分辨率的定量确定方法，并以此指导进行更准确的EBSD显微组织分析。The current method to determine the spatial resolution of EBSD is to calculate the pixel correlation of the diffraction pattern, that is, select the twin boundary in the material, collect the diffraction pattern on both sides of the twin boundary and collect the reference pattern far away from the twin boundary, and then The pixel correlation formula is used to calculate the correlation coefficient curve between the diffraction pattern and the reference pattern, and then the spatial resolution is calculated using the correlation coefficient curve. However, calculating spatial resolution using pixel correlation is more complicated, involving Fourier transform, Gaussian filtering and inverse Fourier transform of the correlation curve; on the other hand, twin boundaries do not exist in the structure of many metallic materials. Or the twin boundaries are difficult to find, which increases the difficulty of applying this method. Therefore, a simpler and faster quantitative determination method of spatial resolution is needed to guide more accurate EBSD microstructural analysis.
发明内容Contents of the invention
本发明提供了一种电子背散射衍射的分析方法，以解决或者部分解决现有的EBSD空间分辨率的确定方法过于复杂以至于影响EBSD分析准确性的技术问题。The present invention provides an electron backscattered diffraction analysis method to solve or partially solve the technical problem that the existing method for determining the spatial resolution of EBSD is too complicated and affects the accuracy of EBSD analysis.
为解决上述技术问题，本发明提供了一种电子背散射衍射的分析方法，包括：In order to solve the above technical problems, the present invention provides an analysis method of electron backscattered diffraction, including:
根据预设工艺制备标定样品；Prepare calibration samples according to the preset process;
根据预设工作参数，在扫描电镜下对标定样品进行电子背散射衍射EBSD分析，确定标定样品的目标晶界；According to the preset working parameters, conduct electron backscatter diffraction EBSD analysis on the calibration sample under a scanning electron microscope to determine the target grain boundary of the calibration sample;
采用第一扫描步长对目标晶界进行线扫描分析，获取在线扫描路径上的全部采样点的菊池花样的花样质量BC值；其中，线扫描分析的线扫描路径与目标晶界呈预设角度并穿过目标晶界；Use the first scan step to perform line scan analysis on the target grain boundary, and obtain the pattern quality BC value of the Kikuchi pattern at all sampling points on the line scan path; where the line scan path of the line scan analysis is at a preset angle with the target grain boundary. and cross the target grain boundary;
对全部采样点的BC值进行单峰拟合，获得BC值的单峰拟合曲线；Perform unimodal fitting on the BC values of all sampling points to obtain a unimodal fitting curve of BC values;
计算单峰拟合曲线的半高宽，将半高宽确定为扫描电镜在预设工作参数下的EBSD分析的空间分辨率；Calculate the half-maximum width of the single-peak fitting curve, and determine the half-maximum width as the spatial resolution of EBSD analysis under the scanning electron microscope under preset working parameters;
根据空间分辨率，确定对待分析样品进行EBSD分析时的目标分析参数。According to the spatial resolution, the target analysis parameters for EBSD analysis of the sample to be analyzed are determined.
可选的，预设角度为90°。Optional, the default angle is 90°.
可选的，第一扫描步长小于等于50纳米。Optionally, the first scanning step size is less than or equal to 50 nanometers.
可选的，目标分析参数包括第二扫描步长或扫描电镜的目标工作参数。Optionally, the target analysis parameters include the second scanning step or the target working parameters of the scanning electron microscope.
进一步的，目标工作参数包括加速电压、电子束流、光阑孔径、工作距离中的至少一种。Further, the target operating parameters include at least one of accelerating voltage, electron beam current, aperture aperture, and working distance.
如上述的技术方案，根据空间分辨率，确定对待分析样品进行EBSD分析时的目标分析参数，具体包括：As in the above technical solution, according to the spatial resolution, the target analysis parameters for EBSD analysis of the samples to be analyzed are determined, specifically including:
在对待分析样品进行EBSD分析时，调整第二扫描步长，以使第二扫描步长大于空间分辨率。When performing EBSD analysis on the sample to be analyzed, the second scan step size is adjusted so that the second scan step size is greater than the spatial resolution.
进一步的，根据空间分辨率，确定对待分析样品进行EBSD分析时的目标分析参数，具体包括：Further, based on the spatial resolution, the target analysis parameters for EBSD analysis of the sample to be analyzed are determined, including:
在对待分析样品进行EBSD分析时，调整扫描电镜的目标工作参数，以使在目标工作参数下的EBSD空间分辨率小于第二扫描步长。When performing EBSD analysis on the sample to be analyzed, the target working parameters of the scanning electron microscope are adjusted so that the EBSD spatial resolution under the target working parameters is smaller than the second scanning step.
如上述的技术方案，根据预设工艺制备标定样品，具体包括：As in the above technical solution, calibration samples are prepared according to the preset process, specifically including:
使用硅溶胶抛光液对选定样品的表面进行慢速抛光，抛光速度为100～300转/分，获得标定样品。Use silica sol polishing liquid to slowly polish the surface of the selected sample at a polishing speed of 100 to 300 rpm to obtain a calibration sample.
可选的，确定标定样品的目标晶界，具体包括：Optionally, determine the target grain boundaries of the calibration sample, including:
在扫描电镜下对标定样品的局部区域进行EBSD面扫描，获得面扫描的菊池花样质量BC图；Perform EBSD surface scanning on a local area of the calibration sample under a scanning electron microscope to obtain a surface scanning Kikuchi pattern quality BC chart;
从菊池花样质量BC图中确定一条成像清晰的晶界作为目标晶界。Determine a clearly imaged grain boundary from the Kikuchi pattern mass BC map as the target grain boundary.
可选的，选定样品为长度10mm～12mm，宽度5mm～8mm，厚度1mm～2mm的矩形试样；矩形试样的上下表面相互平行。Optional, the selected sample is a rectangular specimen with a length of 10mm~12mm, a width of 5mm~8mm, and a thickness of 1mm~2mm; the upper and lower surfaces of the rectangular specimen are parallel to each other.
通过本发明的一个或者多个技术方案，本发明具有以下有益效果或者优点：Through one or more technical solutions of the present invention, the present invention has the following beneficial effects or advantages:
本发明提供了一种电子背散射衍射的分析方法，通过对标定样品中的目标晶界的两侧进行线扫描，获得线扫描路径上所有采样点的菊池线的花样质量BC值，基于菊池线花样不重叠的最小距离为空间分辨率的原理，对所有BC值进行单峰拟合并计算拟合峰的半高宽，此半高宽的值即对应于当前工作参数下的EBSD的空间分辨率，并依此为据对应调整EBSD的分析参数。本实施例提供的分析方法利用材料显微组织中的常规晶界，更加方便、快捷的定量分析出当前工作参数下EBSD的空间分辨率，并以此为据对EBSD的分析参数进行指导，提高对待分析样品进行EBSD分析的准确性。The present invention provides an analysis method for electron backscattered diffraction. By performing a line scan on both sides of the target grain boundary in the calibration sample, the pattern quality BC value of the Kikuchi line of all sampling points on the line scan path is obtained. Based on the Kikuchi line The minimum distance at which patterns do not overlap is the principle of spatial resolution. Perform single-peak fitting on all BC values and calculate the half-maximum width of the fitted peak. The value of this half-maximum width corresponds to the spatial resolution of EBSD under the current working parameters. rate, and adjust the EBSD analysis parameters accordingly. The analysis method provided in this embodiment uses the conventional grain boundaries in the material microstructure to quantitatively analyze the spatial resolution of EBSD under the current working parameters more conveniently and quickly, and uses this as a basis to guide the analysis parameters of EBSD and improve Accuracy of EBSD analysis on samples to be analyzed.
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，而可依照说明书的内容予以实施，并且为了让本发明的上述和其它目的、特征和优点能够更明显易懂，以下特举本发明的具体实施方式。The above description is only an overview of the technical solution of the present invention. In order to have a clearer understanding of the technical means of the present invention, it can be implemented according to the content of the description, and in order to make the above and other objects, features and advantages of the present invention more obvious and understandable. , the specific embodiments of the present invention are listed below.
附图说明Description of the drawings
通过阅读下文优选实施方式的详细描述，各种其他的优点和益处对于本领域普通技术人员将变得清楚明了。附图仅用于示出优选实施方式的目的，而并不认为是对本发明的限制。而且在整个附图中，用相同的参考符号表示相同的部件。在附图中：Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are for the purpose of illustrating preferred embodiments only and are not to be construed as limiting the invention. Also throughout the drawings, the same reference characters are used to designate the same components. In the attached picture:
图1示出了根据本发明一个实施例的电子背散射衍射的分析方法的流程图；Figure 1 shows a flow chart of an analysis method for electron backscattered diffraction according to one embodiment of the present invention;
图2示出了根据本发明一个实施例的标定样品在采用硅溶胶慢速抛光后晶界不可见的样品表面形貌SEM照片；Figure 2 shows an SEM photo of the surface morphology of the calibration sample with invisible grain boundaries after slow polishing using silica sol according to an embodiment of the present invention;
图3示出了根据本发明一个实施例的对标定样品表面进行局部面扫描后的晶界可见的菊池花样质量BC图；Figure 3 shows a Kikuchi pattern quality BC diagram with visible grain boundaries after partial surface scanning of the calibration sample surface according to one embodiment of the present invention;
图4示出了根据本发明一个实施例的对图2的虚线框内的晶界沿着其垂直方向做线扫描获得的BC值曲线；Figure 4 shows a BC value curve obtained by line scanning along the vertical direction of the grain boundary in the dotted frame of Figure 2 according to one embodiment of the present invention;
图5示出了根据本发明一个实施例的对BC值曲线进行单峰拟合和半高宽确定的示意图。FIG. 5 shows a schematic diagram of single-peak fitting and half-maximum width determination of a BC value curve according to an embodiment of the present invention.
具体实施方式Detailed ways
为了使本申请所属技术领域中的技术人员更清楚地理解本申请，下面结合附图，通过具体实施例对本申请技术方案作详细描述。In order to enable those skilled in the technical field to which this application belongs to understand this application more clearly, the technical solutions of this application will be described in detail through specific embodiments in conjunction with the accompanying drawings.
基于在EBSD分析中准确掌握空间分辨率的重要性，在一个可选的实施例中，提出了一种基于EBSD分析的菊池花样质量确定空间分辨率并据此进行EBSD分析的方法，其整体思路如下：Based on the importance of accurately grasping the spatial resolution in EBSD analysis, in an optional embodiment, a method of determining the spatial resolution based on the Kikuchi pattern quality of EBSD analysis and performing EBSD analysis accordingly is proposed. The overall idea is as follows:
一种电子背散射衍射的分析方法，如附图1所示，包括：An analysis method for electron backscattered diffraction, as shown in Figure 1, includes:
S1：根据预设工艺制备标定样品；S1: Prepare calibration samples according to the preset process;
S2：根据预设工作参数，在扫描电镜下对标定样品进行电子背散射衍射EBSD分析，确定标定样品的目标晶界；S2: According to the preset working parameters, conduct electron backscatter diffraction EBSD analysis on the calibration sample under a scanning electron microscope to determine the target grain boundary of the calibration sample;
S3：采用第一扫描步长对目标晶界进行线扫描分析，获取在线扫描路径上的全部采样点的菊池花样的花样质量BC值；其中，线扫描分析的线扫描路径与目标晶界呈预设角度并穿过目标晶界；S3: Use the first scan step to perform line scan analysis on the target grain boundary, and obtain the pattern quality BC value of the Kikuchi pattern at all sampling points on the line scan path; among which, the line scan path of the line scan analysis is in predetermined relationship with the target grain boundary. Set the angle and cross the target grain boundary;
S4：对全部采样点的BC值进行单峰拟合，获得BC值的单峰拟合曲线；S4: Perform unimodal fitting on the BC values of all sampling points to obtain a unimodal fitting curve of BC values;
S5：计算单峰拟合曲线的半高宽，将半高宽确定为扫描电镜在预设工作参数下的EBSD分析的空间分辨率；S5: Calculate the half-maximum width of the single-peak fitting curve, and determine the half-maximum width as the spatial resolution of EBSD analysis under the scanning electron microscope under preset working parameters;
S6：根据空间分辨率，确定对待分析样品进行EBSD分析时的目标分析参数。S6: Based on the spatial resolution, determine the target analysis parameters for EBSD analysis of the sample to be analyzed.
具体的，本实施例中提供的电子背散射衍射分析方法，首先是在EBSD下采用预设工作参数对标定样品进行组织分析，通过扫描电镜的背散射衍射成像，获得标定样品的菊池花样质量BC图，然后从菊池花样质量BC图中确定出一条成像清晰的目标晶界；在扫描电镜中，常见的预设工作参数包括：电子束的加速加压为15kV或20kV，电子束流为1～10nA，工作距离WD为13～15mm、光阑孔径设置值为30μm、50μm、70μm和110μm等；标定样品可以选择钢铁试样，进一步的，选择如低碳、超低碳成分体系的软钢，这种软钢碳含量和合金含量低，容易制备并方便观察到组织中的清晰晶界；Specifically, the electron backscattered diffraction analysis method provided in this embodiment first uses preset working parameters to perform tissue analysis on the calibration sample under EBSD, and obtains the Kikuchi pattern quality BC of the calibration sample through backscattered diffraction imaging with a scanning electron microscope. Figure, and then determine a clearly imaged target grain boundary from the Kikuchi pattern mass BC map; in the scanning electron microscope, common preset working parameters include: the acceleration and pressure of the electron beam is 15kV or 20kV, and the electron beam current is 1~ 10nA, the working distance WD is 13~15mm, and the diaphragm aperture setting values are 30μm, 50μm, 70μm and 110μm, etc.; the calibration sample can choose steel samples, and further, choose mild steel with low carbon and ultra-low carbon composition systems. This kind of mild steel has low carbon and alloy content, is easy to prepare and facilitates observation of clear grain boundaries in the structure;
接下来，在目标晶界的一侧按第一扫描步长进行EBSD线扫描分析，线扫描是在菊池花样质量BC图中确定一条扫描线，在这条线的路径上以第一扫描步长为间隔进行采样分析，线扫描的路径开始于目标晶界一侧的晶粒，呈一定的预设角度穿过目标晶界，并向目标晶界另一侧的晶粒中延伸(如图3虚线所示)，EBSD分析并输出线扫描路径上的一系列采样点的菊池花样和对应的菊池花样质量BC值(或菊池线衬度值)；Next, perform EBSD line scan analysis with the first scan step on one side of the target grain boundary. The line scan is to determine a scan line in the Kikuchi pattern mass BC chart, and use the first scan step on the path of this line. For interval sampling analysis, the line scan path starts from the grain on one side of the target grain boundary, passes through the target grain boundary at a certain preset angle, and extends to the grain on the other side of the target grain boundary (Figure 3 (shown by the dotted line), EBSD analyzes and outputs the Kikuchi pattern and the corresponding Kikuchi pattern quality BC value (or Kikuchi line contrast value) of a series of sampling points on the line scan path;
接着，可以使用常见的带有拟合和绘图功能的分析软件，如Origin软件，先将所有采样点的BC值绘制成BC值曲线，在对所述BC值曲线进行单峰拟合，获得单峰拟合曲线并计算出拟合峰的半高宽，所述半高宽即为当前工作参数下的EBSD的空间分辨率的值。为了准确，可以根据上述方法对目标晶界测量三次取平均值，或者再选取其他的目标晶界进行分析再取平均值；Then, you can use common analysis software with fitting and drawing functions, such as Origin software, to first draw the BC values of all sampling points into a BC value curve, and then perform single-peak fitting on the BC value curve to obtain a single peak. The peak fitting curve is calculated and the half-width of the fitted peak is calculated. The half-width is the value of the spatial resolution of EBSD under the current working parameters. For accuracy, you can measure the target grain boundary three times and take the average according to the above method, or select other target grain boundaries for analysis and take the average;
在确定了当前工作参数下的EBSD空间分辨率后，即可结合实际待分析的样品的材料特性，如材料的主要成分体系、晶粒大小等，适应性的确定或调整EBSD的目标分析参数，然后根据目标分析参数，对待分析样品进行EBSD的检测分析；本实施例中提供的方法提高了EBSD分析的准确性，同时也为EBSD所能表征的最小微观尺度提供数据支撑。After determining the EBSD spatial resolution under the current working parameters, the target analysis parameters of EBSD can be adaptively determined or adjusted based on the material characteristics of the actual sample to be analyzed, such as the main component system of the material, grain size, etc. Then, based on the target analysis parameters, EBSD detection and analysis is performed on the sample to be analyzed; the method provided in this embodiment improves the accuracy of EBSD analysis, and also provides data support for the smallest microscopic scale that EBSD can characterize.
需要说明的是，不必在每次检测待分析样品之前都要进行S1～S5的空间分辨率的确定，一次确定得到的空间分辨率数据可用于指导同一台扫描电镜的多次EBSD分析。It should be noted that it is not necessary to determine the spatial resolution of S1 to S5 before each detection of the sample to be analyzed. The spatial resolution data obtained once determined can be used to guide multiple EBSD analyzes of the same scanning electron microscope.
本实施例提供的利用EBSD线扫描获得的BC值确定空间分辨率的原理如下：研究表明，EBSD的空间分辨率等效于能够正确标定的两个菊池花样所对应在样品上两个点之间的最小距离，而花样质量BC值(或菊池线衬度值)是表征菊池线花样的成像质量；在两个晶粒之间的不连续区域，也就是晶界两侧，由于晶粒之间存在的取向差异，穿过目标晶界的线扫描获得的菊池线的花样质量BC值产生突变显著降低，原因在于：当采样点逐渐靠近晶界时，由于晶界两侧具有不同取向采样点的菊池花样之间产生相互交叉干扰，导致晶界附近采样点的菊池花样与远离晶界处的相比变得更为模糊不清，进而导致菊池花样质量显著降低产生突变；而沿着预设角度穿过晶界的线扫描路径上采样点的菊池花样质量BC值突变产生的早晚决定了当前空间分辨率的大小。而本实施例提供的EBSD的分析方法基于上述晶界两侧采样点的菊池花样质量BC值的突变原理，通过对线扫描路径上的采样点的菊池花样BC值进行单峰拟合，获得表征晶界两侧采样点的BC值突变规律的拟合峰，然后计算出所述拟合峰的半高宽，所述半高宽的值即对应于EBSD在当前的工作参数下的菊池线花样不重叠的最小距离，从而对应的确定出EBSD的空间分辨率。The principle of determining spatial resolution using BC values obtained by EBSD line scanning provided in this embodiment is as follows: Research shows that the spatial resolution of EBSD is equivalent to the distance between two points on the sample corresponding to two Kikuchi patterns that can be correctly calibrated. The minimum distance, and the pattern quality BC value (or Kikuchi line contrast value) is the imaging quality that characterizes the Kikuchi line pattern; in the discontinuous area between two grains, that is, on both sides of the grain boundary, due to the Due to the existing orientation differences, the pattern quality BC value of the Kikuchi line obtained by line scanning through the target grain boundary suddenly decreases significantly. The reason is that when the sampling point gradually approaches the grain boundary, due to the different orientation sampling points on both sides of the grain boundary. Cross-interference occurs between Kikuchi patterns, causing the Kikuchi patterns at sampling points near the grain boundaries to become more blurry than those far away from the grain boundaries, which in turn leads to a significant reduction in the quality of the Kikuchi patterns and a mutation; while along the preset angle The sooner or later the Kikuchi pattern mass BC value mutation occurs at the sampling point on the line scan path passing through the grain boundary determines the size of the current spatial resolution. The EBSD analysis method provided in this embodiment is based on the mutation principle of the Kikuchi pattern mass BC values of the sampling points on both sides of the grain boundary. The characterization is obtained by performing single-peak fitting on the Kikuchi pattern BC values of the sampling points on the line scan path. The fitting peak of the BC value mutation pattern of the sampling points on both sides of the grain boundary is then calculated, and the half-width of the fitting peak is calculated. The value of the half-width corresponds to the Kikuchi line pattern of EBSD under the current working parameters. The minimum distance without overlap, thus correspondingly determining the spatial resolution of EBSD.
可选的，预设角度为90°，即线扫描的路径与目标晶界垂直，并从晶界的一侧的晶粒穿过晶界延伸至晶界另一侧的晶粒中，如此可以提高空间分辨率的准确性，避免引入不必要的误差。Optionally, the preset angle is 90°, that is, the line scan path is perpendicular to the target grain boundary and extends from the grains on one side of the grain boundary through the grain boundary to the grains on the other side of the grain boundary, so that Improve the accuracy of spatial resolution and avoid introducing unnecessary errors.
可选的，第一扫描步长小于等于50纳米，nm，以保证在线扫描路径上的采样点密度，提高测定的空间分辨率的准确性，优选的第一扫描步长在20nm以内。Optionally, the first scanning step size is less than or equal to 50 nanometers, nm, to ensure the density of sampling points on the online scanning path and improve the accuracy of the spatial resolution of the measurement. The preferred first scanning step size is within 20 nm.
本实施例提供了一种电子背散射衍射的分析方法，通过对标定样品中的目标晶界的两侧进行线扫描，获得线扫描路径上所有采样点的菊池线的花样质量BC值，基于菊池线花样不重叠的最小距离为空间分辨率的原理，对所有BC值进行单峰拟合并计算拟合峰的半高宽，此半高宽的值即对应于当前工作参数下的EBSD的空间分辨率，并依此为据对应调整EBSD的分析参数。本实施例提供的分析方法利用材料显微组织中的常规晶界，更加方便、快捷的定量分析出当前工作参数下EBSD的空间分辨率，并以此为据对EBSD的分析参数进行指导，提高对待分析样品进行EBSD分析的准确性。This embodiment provides an analysis method of electron backscattered diffraction. By performing a line scan on both sides of the target grain boundary in the calibration sample, the pattern quality BC value of the Kikuchi line of all sampling points on the line scan path is obtained. Based on Kikuchi The minimum distance at which line patterns do not overlap is the principle of spatial resolution. Perform single-peak fitting on all BC values and calculate the half-width of the fitted peak. The value of this half-width corresponds to the space of EBSD under the current working parameters. resolution, and adjust the EBSD analysis parameters accordingly. The analysis method provided in this embodiment uses the conventional grain boundaries in the material microstructure to quantitatively analyze the spatial resolution of EBSD under the current working parameters more conveniently and quickly, and uses this as a basis to guide the analysis parameters of EBSD and improve Accuracy of EBSD analysis on samples to be analyzed.
在准确获知了EBSD在当前预设工作参数下的空间分辨率后，可以从两方面指导并确定对待分析样品进行EBSD分析时所采用的目标分析参数。基于前述实施例相同的发明构思，在另一个可选的实施例中，目标分析参数包括第二扫描步长或扫描电镜的目标工作参数。第二扫描步长是指在对待分析样品进行EBSD线扫描或面扫描时应当采用的扫描步长范围；目标工作参数是指在对待分析样品进行EBSD分析时，扫描电镜应当设定的工作参数具体范围。如前所述，EBSD的空间分辨率主要取决于入射电子束的束斑尺寸；同时，EBSD分析时扫描电镜的工作参数，如采用的加速电压、光阑孔径和电子束的束流等同样对EBSD的空间分辨率产生显著的影响。故而，目标工作参数包括加速电压、电子束流、光阑孔径、工作距离中的至少一种。After accurately knowing the spatial resolution of EBSD under the current preset working parameters, we can guide and determine the target analysis parameters used in EBSD analysis of the samples to be analyzed from two aspects. Based on the same inventive concept of the foregoing embodiment, in another optional embodiment, the target analysis parameter includes a second scanning step or a target working parameter of the scanning electron microscope. The second scan step refers to the scan step range that should be used when performing EBSD line scan or surface scan on the sample to be analyzed; the target working parameters refer to the specific working parameters that should be set by the scanning electron microscope when performing EBSD analysis on the sample to be analyzed. scope. As mentioned before, the spatial resolution of EBSD mainly depends on the beam spot size of the incident electron beam; at the same time, the working parameters of the scanning electron microscope during EBSD analysis, such as the accelerating voltage, aperture aperture and beam current of the electron beam, etc. also affect The spatial resolution of EBSD has a significant impact. Therefore, the target operating parameters include at least one of accelerating voltage, electron beam current, aperture aperture, and working distance.
可选的，根据空间分辨率，确定对待分析样品进行EBSD分析时的目标分析参数，具体包括：在对待分析样品进行EBSD分析时，调整第二扫描步长，以使第二扫描步长大于空间分辨率。即，空间分辨率可以用于指导在EBSD分析时线扫描和面扫描的最小扫描步长，小于当前空间分辨率的扫描步长没有检测意义，只会增加不必要的分析时间。Optionally, according to the spatial resolution, determine the target analysis parameters when performing EBSD analysis on the sample to be analyzed, specifically including: when performing EBSD analysis on the sample to be analyzed, adjust the second scan step so that the second scan step is larger than the space resolution. That is, the spatial resolution can be used to guide the minimum scan step size for line scans and surface scans during EBSD analysis. Scan step sizes smaller than the current spatial resolution have no detection significance and will only increase unnecessary analysis time.
在一些情况下，需要采用比当前预设工作参数下的空间分辨率更小的扫描步长，如检测主成分元素的原子序数较小的材料样品，需要更高的空间分辨率，此时，可以通过调整EBSD的工作参数，提高EBSD的空间分辨率，使空间分辨率的数值降到第二扫描步长以下。可选的，根据空间分辨率，确定对待分析样品进行EBSD分析时的目标分析参数，具体包括：在对待分析样品进行EBSD分析时，调整扫描电镜的目标工作参数，以使在目标工作参数下的EBSD空间分辨率小于第二扫描步长。例如，可以采用适当降低加速电压，降低电子束流，减小光阑孔径，缩短工作距离等工作参数的合理搭配，提高EBSD的空间分辨率。例如，将加速电压从15kv降低到12kv，电子束流从5nA降低到2nA，光阑孔径从50微米减小至30微米，工作距离从15mm缩短到13mm等单一或组合的方式，提高EBSD的空间分辨率。In some cases, it is necessary to adopt a scanning step size smaller than the spatial resolution under the current preset working parameters. For example, to detect material samples with smaller atomic numbers of the main component elements, a higher spatial resolution is required. In this case, The spatial resolution of EBSD can be improved by adjusting the working parameters of EBSD, so that the spatial resolution value drops below the second scanning step. Optionally, according to the spatial resolution, determine the target analysis parameters when performing EBSD analysis on the sample to be analyzed, which specifically includes: adjusting the target working parameters of the scanning electron microscope when performing EBSD analysis on the sample to be analyzed, so that the target working parameters are adjusted under the target working parameters. The EBSD spatial resolution is smaller than the second scan step size. For example, a reasonable combination of working parameters such as appropriately reducing the accelerating voltage, reducing the electron beam current, reducing the aperture aperture, shortening the working distance, etc. can be used to improve the spatial resolution of EBSD. For example, reducing the accelerating voltage from 15kv to 12kv, reducing the electron beam current from 5nA to 2nA, reducing the aperture aperture from 50 microns to 30 microns, shortening the working distance from 15mm to 13mm, etc., single or combined methods can improve the space of EBSD. resolution.
标定样品的选取和制备对准确的确定空间分辨率非常重要，材料的晶界浮凸效应是影响准确测定空间分辨率的一个重要因素。为了消除晶界浮凸效应对空间分辨率的不利影响，基于前述实施例相同的发明构思，在又一个可选的实施例中，根据预设工艺制备标定样品，具体包括：使用硅溶胶抛光液对选定样品的表面进行慢速抛光，抛光速度为100～300转/分，获得标定样品。The selection and preparation of calibration samples are very important for accurately determining spatial resolution. The grain boundary relief effect of materials is an important factor affecting the accurate determination of spatial resolution. In order to eliminate the adverse impact of the grain boundary relief effect on spatial resolution, based on the same inventive concept of the previous embodiment, in yet another optional embodiment, a calibration sample is prepared according to a preset process, which specifically includes: using silica sol polishing liquid The surface of the selected sample is slowly polished at a polishing speed of 100 to 300 rpm to obtain a calibration sample.
常规的样品抛光方法和抛光液无法消除材料晶界附近的浮凸，本实施例中采用硅溶胶抛光液对选定样品或待标定的样品进行慢速抛光，不仅可以去除材料的残留应力，更重要的是可以消除晶界的表面浮凸，避免浮凸效应导致空间分辨率的测定结果偏大，提高了空间分辨率测定结果的准确性。Conventional sample polishing methods and polishing fluids cannot eliminate the relief near the material grain boundaries. In this embodiment, silica sol polishing fluid is used to slowly polish the selected sample or the sample to be calibrated, which can not only remove the residual stress of the material, but also The important thing is to eliminate the surface embossment at the grain boundary, avoid the embossment effect causing the spatial resolution measurement results to be larger, and improve the accuracy of the spatial resolution measurement results.
由于使用了硅溶胶抛光液进行慢速抛光，很可能导致标定样品的表面在扫描电镜下无法清楚的辨识出晶界，为了解决这个问题，进一步的，确定标定样品的目标晶界，具体包括：在扫描电镜下对标定样品的局部区域进行EBSD面扫描，获得面扫描的菊池花样质量BC图；从菊池花样质量BC图中确定一条成像清晰的晶界作为目标晶界。Due to the use of silica sol polishing liquid for slow polishing, it is likely that the grain boundaries of the calibration sample cannot be clearly identified under the scanning electron microscope. In order to solve this problem, further determine the target grain boundaries of the calibration sample, including: Perform EBSD surface scanning on a local area of the calibration sample under a scanning electron microscope to obtain a surface-scanned Kikuchi pattern quality BC chart; determine a clearly imaged grain boundary from the Kikuchi pattern quality BC chart as the target grain boundary.
对于样品的形状规格，可选的，选定样品为长度10mm～12mm，宽度5mm～8mm，厚度1mm～2mm的矩形试样；矩形试样的上下表面相互平行。Regarding the shape specification of the sample, optionally, the selected sample is a rectangular sample with a length of 10mm~12mm, a width of 5mm~8mm, and a thickness of 1mm~2mm; the upper and lower surfaces of the rectangular sample are parallel to each other.
在接下来的一个实施例中，结合具体数据，对上述实施例中的方案进行详细说明：In the following embodiment, the solution in the above embodiment will be described in detail in combination with specific data:
本实施例以超低碳IF钢为标定样品，测定EBSD的空间分辨率，步骤如下：In this example, ultra-low carbon IF steel is used as the calibration sample to measure the spatial resolution of EBSD. The steps are as follows:
(1)标定样品制备：样品尺寸要求长度10mm，宽度5mm，厚度1mm，保证上下表面平行，为了在线扫描时消除晶界浮凸效应对分辨率测定结果的影响，样品制备采用硅溶胶慢速抛光，硅溶胶材质为水溶性二氧化硅，抛光速率150转/分；(1) Calibration sample preparation: The sample size requires a length of 10mm, a width of 5mm, and a thickness of 1mm, ensuring that the upper and lower surfaces are parallel. In order to eliminate the impact of the grain boundary relief effect on the resolution measurement results during online scanning, the sample preparation uses silica sol slow polishing. , the silica sol material is water-soluble silica, and the polishing rate is 150 rpm;
(2)确定扫描电镜的预设工作参数：加速加压15kV，束流2nA，工作距离WD为15mm、光阑孔径为30μm；(2) Determine the preset working parameters of the scanning electron microscope: accelerated pressure 15kV, beam current 2nA, working distance WD 15mm, aperture aperture 30μm;
(3)确定当前工作参数下的空间分辨率：由于硅溶胶慢速抛光获得的样品表面晶界并不清晰(见图2)，因此需要先对局部区域进行EBSD面扫描分析，获得该局部区域的菊池花样质量BC图(见图3)，在获得的背散射衍射图像中找到一条合适的晶界作为目标晶界(位于图3虚线框内)，然后在该晶界的一侧沿着晶界的垂直方向做线扫描(见图3中的黑色虚线)，线扫描的第一扫描步长为3.5nm，穿过晶界到另一侧，获得该线扫描路径上各个采样点的菊池花样，再根据菊池花样的花样质量(BC值)绘制单峰曲线(见图4)，然后利用Origin专业软件进行单峰拟合并计算出相应的半高宽(见图5)，经计算半高宽为38nm，根据上述方法对同一条晶界测量三次取平均值，见下表1，该值即为当前条件下的空间分辨率；(3) Determine the spatial resolution under the current working parameters: Since the grain boundaries on the surface of the sample obtained by slow polishing of silica sol are not clear (see Figure 2), it is necessary to first perform EBSD surface scanning analysis on the local area to obtain the local area. Kikuchi pattern mass BC diagram (see Figure 3), find a suitable grain boundary in the obtained backscattered diffraction image as the target grain boundary (located in the dotted line box in Figure 3), and then trace the grain boundary along one side of the grain boundary. Do a line scan in the vertical direction of the boundary (see the black dotted line in Figure 3). The first scan step of the line scan is 3.5nm. Go through the grain boundary to the other side and obtain the Kikuchi pattern of each sampling point on the line scan path. , and then draw a unimodal curve according to the pattern quality (BC value) of the Kikuchi pattern (see Figure 4), and then use Origin professional software to perform unimodal fitting and calculate the corresponding half-height width (see Figure 5). After calculating the half-height The width is 38nm. According to the above method, the same grain boundary is measured three times and the average is taken. See Table 1 below. This value is the spatial resolution under the current conditions;
表1同一条晶界测量三次的半高宽统计Table 1 Statistics of the half-maximum width measured three times on the same grain boundary
(4)确定EBSD的目标分析参数：在确定了当前工作参数下的EBSD空间分辨率为51.7nm后，若不更改扫描电镜的工作参数，则在后续对待分析样品进行EBSD时，面扫描和线扫描的第二扫描步长需要控制在52nm以上；若对某分析样品必须采用50nm以下，如40nm左右的扫描步长，此时应当调整电镜的工作参数，提高EBSD的空间分辨率，使其空间分辨率的数值降低到40nm以下。(4) Determine the target analysis parameters of EBSD: After determining that the EBSD spatial resolution under the current working parameters is 51.7nm, if the working parameters of the scanning electron microscope are not changed, when the subsequent EBSD is performed on the sample to be analyzed, the surface scanning and line scanning The second scanning step of the scan needs to be controlled above 52nm; if a certain analysis sample must use a scanning step below 50nm, such as about 40nm, the working parameters of the electron microscope should be adjusted at this time to improve the spatial resolution of EBSD to make it spatially The resolution value is reduced to below 40nm.
通过本发明的一个或者多个实施例，本发明具有以下有益效果或者优点：Through one or more embodiments of the present invention, the present invention has the following beneficial effects or advantages:
本发明提供了一种电子背散射衍射的分析方法，通过对标定样品中的目标晶界的两侧进行线扫描，获得线扫描路径上所有采样点的菊池线的花样质量BC值，基于菊池线花样不重叠的最小距离为空间分辨率的原理，对所有BC值进行单峰拟合并计算拟合峰的半高宽，此半高宽的值即对应于当前工作参数下的EBSD的空间分辨率，并依此为据对应调整EBSD的分析参数。本实施例提供的分析方法利用材料显微组织中的常规晶界，更加方便、快捷的定量分析出当前工作参数下EBSD的空间分辨率，并以此为据对EBSD的分析参数进行指导，提高对待分析样品进行EBSD分析的准确性。The present invention provides an analysis method for electron backscattered diffraction. By performing a line scan on both sides of the target grain boundary in the calibration sample, the pattern quality BC value of the Kikuchi line of all sampling points on the line scan path is obtained. Based on the Kikuchi line The minimum distance at which patterns do not overlap is the principle of spatial resolution. Perform single-peak fitting on all BC values and calculate the half-maximum width of the fitted peak. The value of this half-maximum width corresponds to the spatial resolution of EBSD under the current working parameters. rate, and adjust the EBSD analysis parameters accordingly. The analysis method provided in this embodiment uses the conventional grain boundaries in the material microstructure to quantitatively analyze the spatial resolution of EBSD under the current working parameters more conveniently and quickly, and uses this as a basis to guide the analysis parameters of EBSD and improve Accuracy of EBSD analysis on samples to be analyzed.
尽管已描述了本申请的优选实施例，但本领域内的普通技术人员一旦得知了基本创造性概念，则可对这些实施例作出另外的变更和修改。所以，所附权利要求意欲解释为包括优选实施例以及落入本申请范围的所有变更和修改。Although the preferred embodiments of the present application have been described, those skilled in the art will be able to make additional changes and modifications to these embodiments once the basic inventive concepts are understood. Therefore, it is intended that the appended claims be construed to include the preferred embodiments and all changes and modifications that fall within the scope of this application.
显然，本领域的技术人员可以对本申请进行各种改动和变型而不脱离本申请的精神和范围。这样，倘若本申请的这些修改和变型属于本申请权利要求及其等同技术的范围之内，则本申请也意图包含这些改动和变型在内。Obviously, those skilled in the art can make various changes and modifications to the present application without departing from the spirit and scope of the present application. In this way, if these modifications and variations of the present application fall within the scope of the claims of the present application and equivalent technologies, the present application is also intended to include these modifications and variations.
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