Analysis method of electron back scattering diffraction

文档序号:1168711 发布日期:2020-09-18 浏览:39次 中文

阅读说明:本技术 一种电子背散射衍射的分析方法 (Analysis method of electron back scattering diffraction ) 是由 崔桂彬 鞠新华 杨瑞 于 2020-06-09 设计创作,主要内容包括:本发明公开了一种电子背散射衍射的分析方法:根据预设工艺制备标定样品;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;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;对所有的BC值进行单峰拟合,获得BC值的单峰拟合曲线;确定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;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。上述方法能够更加方便、快捷地分析出当前工作参数下EBSD的空间分辨率,基于此提高对待分析样品进行EBSD分析的准确性。(The invention discloses an analysis method of electron back scattering diffraction, which comprises the following steps: preparing a calibration sample according to a preset process; according to preset working parameters, performing Electron Back Scattering Diffraction (EBSD) analysis on the calibration sample under a scanning electron microscope to determine a target grain boundary of the calibration sample; performing line scanning analysis on a target grain boundary by adopting a first scanning step length to obtain pattern quality BC values of the chrysanthemum pool patterns of all sampling points on a line scanning path; performing unimodal fitting on all BC values to obtain a unimodal fitting curve of the BC values; determining the full width at half maximum of the unimodal fitting curve, and determining the full width at half maximum as the spatial resolution of the scanning electron microscope EBSD analysis under the preset working parameters; and determining target analysis parameters when the sample to be analyzed is subjected to EBSD analysis according to the spatial resolution. The method can more conveniently and quickly analyze the spatial resolution of the EBSD under the current working parameters, and improves the accuracy of the EBSD analysis of the sample to be analyzed based on the analysis.)

1. A method of analyzing electron backscatter diffraction, the method comprising:

preparing a calibration sample according to a preset process;

according to preset working parameters, performing Electron Back Scattering Diffraction (EBSD) analysis on the calibration sample under a scanning electron microscope to determine a target grain boundary of the calibration sample;

performing line scanning analysis on the target grain boundary by adopting a first scanning step length to obtain pattern quality BC values of the chrysanthemum pool patterns of all sampling points on a line scanning path; the line scanning path of the line scanning analysis forms a preset angle with the target grain boundary and penetrates through the target grain boundary;

carrying out unimodal fitting on the BC values of all the sampling points to obtain a unimodal fitting curve of the BC values;

calculating the full width at half maximum of the single-peak fitting curve, and determining the full width at half maximum as the spatial resolution of the scanning electron microscope in the EBSD analysis under the preset working parameters;

and determining target analysis parameters when the sample to be analyzed is subjected to EBSD analysis according to the spatial resolution.

2. The analytical method of claim 1, wherein the predetermined angle is 90 °.

3. The analysis method according to claim 1, wherein the first scanning step is 50nm or less.

4. The analysis method according to claim 1, wherein the target analysis parameter comprises a second scanning step or a target operating parameter of the scanning electron microscope.

5. The analysis method of claim 4, wherein the target operating parameter comprises at least one of an acceleration voltage, an electron beam current, a diaphragm aperture, and a working distance.

6. The analysis method according to claim 4, wherein the determining the target analysis parameters for the EBSD analysis of the sample to be analyzed according to the spatial resolution specifically comprises:

and when the sample to be analyzed is subjected to EBSD analysis, adjusting the second scanning step length to enable the second scanning step length to be larger than the spatial resolution.

7. The analysis method according to claim 5, wherein the determining the target analysis parameters for the EBSD analysis of the sample to be analyzed according to the spatial resolution specifically comprises:

and when the sample to be analyzed is subjected to EBSD analysis, adjusting the target working parameters of the scanning electron microscope so as to enable the EBSD spatial resolution under the target working parameters to be smaller than the second scanning step length.

8. The analysis method according to any one of claims 1 to 7, wherein the preparing of the calibration sample according to the predetermined process specifically comprises:

and (3) using the silica sol polishing solution to polish the surface of the selected sample at a low speed, wherein the polishing speed is 100-300 r/min, so as to obtain a calibration sample.

9. The analysis method according to claim 8, wherein the determining the target grain boundary of the calibration sample specifically comprises:

performing EBSD surface scanning on the local area of the calibration sample under a scanning electron microscope to obtain a Juliangchuan pattern quality BC picture;

and determining a clearly imaged grain boundary as a target grain boundary from the Julian style pattern quality BC picture.

10. The analytical method of claim 8, wherein the selected sample is a rectangular specimen having a length of 10mm to 12mm, a width of 5mm to 8mm, and a thickness of 1mm to 2 mm; the upper and lower surfaces of the rectangular sample are parallel to each other.

Technical Field

The application relates to the technical field of metal material detection, in particular to an analysis method of electron back scattering diffraction.

Background

A back scattering electron diffraction analysis device (EBSD) is added in a scanning electron microscope, can be used for analyzing crystallographic information of materials, and is widely applied to the representation of microstructure and texture of metal materials at present. The resolution of EBSD includes spatial resolution, which refers to the size of the smallest grain that EBSD can resolve, and angular resolution, which determines the scan step size that is suitable for EBSD analysis. Generally, the spatial resolution of an EBSD depends mainly on the beam spot size of the incident electron beam, and is smaller if the beam spot size of the electron beam is larger; the spatial resolution of EBSD is also related to the atomic number of the sample, and the smaller the atomic number, the larger the backscattered electron generation range, and the lower the resolution under the same parameter conditions. Therefore, the EBSD detection analysis of the material microstructure can be more accurately carried out by determining the spatial resolution of the scanning electron microscope in the EBSD under the current working condition and determining reasonable analysis parameters based on the spatial resolution.

The current method for determining the spatial resolution of the EBSD comprises the steps of calculating the pixel correlation of diffraction patterns, namely selecting a twin boundary in a material, collecting the diffraction patterns in the areas on two sides of the twin boundary and collecting reference patterns far away from the twin boundary, then calculating a correlation coefficient curve between the diffraction patterns and the reference patterns by adopting a pixel correlation formula, and then calculating the spatial resolution by utilizing the correlation coefficient curve. However, the calculation of spatial resolution using pixel correlation is complicated, involving fourier, gaussian and inverse fourier transforms of the correlation curve; on the other hand, the absence of twin boundaries in the structure of many metallic materials or twin boundaries are not easily found, thus increasing the difficulty of application of this method. Therefore, a simpler and faster quantitative determination method of spatial resolution is needed to guide more accurate analysis of the EBSD microstructure.

Disclosure of Invention

The invention provides an analysis method of electron back scattering diffraction, which aims to solve or partially solve the technical problem that the existing determination method of EBSD spatial resolution is too complex to influence the EBSD analysis accuracy.

In order to solve the above technical problem, the present invention provides an analysis method of electron backscatter diffraction, comprising:

preparing a calibration sample according to a preset process;

according to preset working parameters, performing Electron Back Scattering Diffraction (EBSD) analysis on the calibration sample under a scanning electron microscope to determine a target grain boundary of the calibration sample;

performing line scanning analysis on a target grain boundary by adopting a first scanning step length to obtain pattern quality BC values of the chrysanthemum pool patterns of all sampling points on a line scanning path; the line scanning path of the line scanning analysis forms a preset angle with the target crystal boundary and penetrates through the target crystal boundary;

carrying out unimodal fitting on BC values of all sampling points to obtain a unimodal fitting curve of the BC values;

calculating the half-height width of the single-peak fitting curve, and determining the half-height width as the spatial resolution of the EBSD analysis of the scanning electron microscope under preset working parameters;

and determining target analysis parameters when the sample to be analyzed is subjected to EBSD analysis according to the spatial resolution.

Optionally, the preset angle is 90 °.

Optionally, the first scanning step is less than or equal to 50 nm.

Optionally, the target analysis parameter includes a second scanning step length or a target working parameter of the scanning electron microscope.

Further, the target working parameter includes at least one of an acceleration voltage, an electron beam current, a diaphragm aperture and a working distance.

According to the technical scheme, the method for determining the target analysis parameters in the EBSD analysis of the sample to be analyzed according to the spatial resolution specifically comprises the following steps:

and when the sample to be analyzed is subjected to EBSD analysis, adjusting the second scanning step length to enable the second scanning step length to be larger than the spatial resolution.

Further, determining target analysis parameters when performing EBSD analysis on a sample to be analyzed according to the spatial resolution specifically includes:

and when the sample to be analyzed is subjected to EBSD analysis, adjusting the target working parameters of the scanning electron microscope so as to enable the EBSD spatial resolution under the target working parameters to be smaller than the second scanning step length.

According to the technical scheme, the preparation of the calibration sample according to the preset process specifically comprises the following steps:

and (3) using the silica sol polishing solution to polish the surface of the selected sample at a low speed, wherein the polishing speed is 100-300 r/min, so as to obtain a calibration sample.

Optionally, determining a target grain boundary of the calibration sample specifically includes:

performing EBSD surface scanning on a local area of a calibration sample under a scanning electron microscope to obtain a surface-scanned Juliangchua pattern quality BC picture;

and determining a clearly imaged grain boundary as a target grain boundary from the Juliangchua pattern quality BC picture.

Optionally, the selected sample is a rectangular sample with the length of 10 mm-12 mm, the width of 5 mm-8 mm and the thickness of 1 mm-2 mm; the upper and lower surfaces of the rectangular sample were parallel to each other.

Through one or more technical schemes of the invention, the invention has the following beneficial effects or advantages:

the invention provides an analysis method of electron back scattering diffraction, which comprises the steps of performing line scanning on two sides of a target grain boundary in a calibration sample to obtain pattern quality BC values of Juchi lines of all sampling points on a line scanning path, performing unimodal fitting on all BC values and calculating the full width at half maximum of a fitting peak based on the principle that the minimum distance of the Juchi line patterns without overlapping is the spatial resolution, wherein the full width at half maximum corresponds to the spatial resolution of EBSD under the current working parameters, and correspondingly adjusting analysis parameters of the EBSD according to the full width at half maximum. The analysis method provided by the embodiment utilizes the conventional grain boundary in the material microstructure, quantitatively analyzes the spatial resolution of the EBSD under the current working parameter more conveniently and rapidly, guides the analysis parameter of the EBSD according to the spatial resolution, and improves the accuracy of EBSD analysis on a sample to be analyzed.

The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.

Drawings

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 only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:

FIG. 1 shows a flow diagram of a method of analysis of electron backscatter diffraction in accordance with one embodiment of the invention;

FIG. 2 shows an SEM photograph of the surface topography of a sample with invisible grain boundaries of a calibration sample after slow polishing with silica sol according to one embodiment of the invention;

FIG. 3 shows a graph of the Chrysanthemum pattern quality BC visible to grain boundaries after local surface scanning of a calibration sample surface, according to one embodiment of the present invention;

FIG. 4 shows a curve of BC values obtained by line scanning the grain boundaries within the dashed box of FIG. 2 along their vertical direction, according to one embodiment of the present invention;

FIG. 5 shows a schematic diagram of unimodal fit and full width at half maximum determination for a BC value curve according to one embodiment of the present invention.

Detailed Description

In order to make the present application more clearly understood by those skilled in the art to which the present application pertains, the following detailed description of the present application is made with reference to the accompanying drawings by way of specific embodiments.

Based on the importance of accurately grasping the spatial resolution in the EBSD analysis, in an alternative embodiment, a method for determining the spatial resolution based on the quality of the chrysanthemums flower bud patterns analyzed by the EBSD analysis and performing EBSD analysis based on the determined spatial resolution is provided, and the overall idea is as follows:

a method for analyzing electron backscatter diffraction, as shown in fig. 1, comprising:

s1: preparing a calibration sample according to a preset process;

s2: according to preset working parameters, performing Electron Back Scattering Diffraction (EBSD) analysis on the calibration sample under a scanning electron microscope to determine a target grain boundary of the calibration sample;

s3: performing line scanning analysis on a target grain boundary by adopting a first scanning step length to obtain pattern quality BC values of the chrysanthemum pool patterns of all sampling points on a line scanning path; the line scanning path of the line scanning analysis forms a preset angle with the target crystal boundary and penetrates through the target crystal boundary;

s4: carrying out unimodal fitting on BC values of all sampling points to obtain a unimodal fitting curve of the BC values;

s5: calculating the half-height width of the single-peak fitting curve, and determining the half-height width as the spatial resolution of the EBSD analysis of the scanning electron microscope under preset working parameters;

s6: and determining target analysis parameters when the sample to be analyzed is subjected to EBSD analysis according to the spatial resolution.

Specifically, in the electron backscatter diffraction analysis method provided in this embodiment, a preset working parameter is first used to perform tissue analysis on a calibration sample under EBSD, a chrysanthemum pool pattern quality BC diagram of the calibration sample is obtained through backscatter diffraction imaging of a scanning electron microscope, and then a clearly-imaged target grain boundary is determined from the chrysanthemum pool pattern quality BC diagram; in a scanning electron microscope, common preset working parameters include: accelerating and pressurizing the electron beam to 15kV or 20kV, setting the electron beam to 1-10 nA, setting the working distance WD to 13-15 mm, setting the aperture of the diaphragm to 30 microns, 50 microns, 70 microns, 110 microns and the like; the calibration sample can be selected from a steel test sample, and further, mild steel such as a low-carbon and ultra-low-carbon component system is selected, the mild steel has low carbon content and alloy content, and is easy to prepare and convenient to observe clear grain boundaries in the structure;

next, performing EBSD line scanning analysis on one side of the target grain boundary according to a first scanning step, where line scanning is to determine a scanning line in the quality BC diagram of the daisy chain pattern, and performing sampling analysis at intervals of the first scanning step on a path of the line, where the path of line scanning starts from a crystal grain on one side of the target grain boundary, passes through the target grain boundary at a certain preset angle, and extends into a crystal grain on the other side of the target grain boundary (as shown by a dotted line in fig. 3), and the EBSD analysis outputs the daisy chain pattern of a series of sampling points on the line scanning path and a corresponding quality BC value (or a daisy chain line contrast value) of the daisy chain pattern;

then, using common analysis software with fitting and drawing functions, such as Origin software, the BC values of all sampling points are drawn into a BC value curve, and then the BC value curve is subjected to unimodal fitting to obtain a unimodal fitting curve and calculate the full width at half maximum of the fitting peak, where the full width at half maximum is the value of the spatial resolution of the EBSD under the current operating parameters. In order to be accurate, the target grain boundary can be measured for three times according to the method and then averaged, or other target grain boundaries are selected for analysis and then averaged;

after determining the EBSD spatial resolution under the current working parameters, adaptively determining or adjusting target analysis parameters of the EBSD by combining the material characteristics of the actual sample to be analyzed, such as the main component system and the grain size of the material, and then performing EBSD detection and analysis on the sample to be analyzed according to the target analysis parameters; the method provided by the embodiment improves the accuracy of EBSD analysis, and provides data support for the minimum microscale which can be characterized by EBSD.

It should be noted that the determination of the spatial resolution of S1-S5 is not necessarily performed before each detection of the sample to be analyzed, and the spatial resolution data obtained from one determination can be used to guide multiple EBSD analyses of the same scanning electron microscope.

The principle of determining the spatial resolution using the BC value obtained by EBSD line scanning provided by this embodiment is as follows: research shows that the spatial resolution of the EBSD is equivalent to the minimum distance between two points on a sample corresponding to two Juchi patterns which can be correctly calibrated, and the pattern quality BC value (or Juchi linear contrast value) is the imaging quality for representing the Juchi linear patterns; in the discontinuous region between two grains, i.e. on both sides of the grain boundary, the pattern quality BC of the Jukumi line obtained by line scanning across the target grain boundary is dramatically reduced by the abrupt change due to the orientation difference existing between the grains, because: when the sampling points are gradually close to the grain boundary, because the mutual cross interference is generated between the Jukuai patterns with the sampling points with different orientations at the two sides of the grain boundary, the Jukuai patterns of the sampling points near the grain boundary are more vague than those far away from the grain boundary, and the quality of the Jukuai patterns is obviously reduced and generates mutation; and the current spatial resolution is determined by the time when the Julian style quality BC value of the sampling point on the line scanning path passing through the grain boundary at the preset angle is suddenly generated. The EBSD analysis method provided in this embodiment is based on the mutation principle of the quality BC values of the daisy chain patterns of the sampling points on both sides of the grain boundary, and performs unimodal fitting on the BC values of the daisy chain patterns of the sampling points on the line scanning path to obtain a fitting peak representing the mutation rule of the BC values of the sampling points on both sides of the grain boundary, and then calculates the full width at half maximum of the fitting peak, where the full width at half maximum corresponds to the minimum distance at which the daisy chain patterns of the EBSD under the current working parameter do not overlap, so as to correspondingly determine the spatial resolution of the EBSD.

Optionally, the preset angle is 90 °, that is, the line scanning path is perpendicular to the target grain boundary and extends from the grain on one side of the grain boundary to the grain on the other side of the grain boundary through the grain boundary, so that the accuracy of the spatial resolution can be improved, and unnecessary errors are avoided.

Optionally, the first scanning step length is less than or equal to 50 nanometers and nm to ensure the density of sampling points on the online scanning path and improve the accuracy of the measured spatial resolution, and the preferred first scanning step length is within 20 nm.

The embodiment provides an analysis method of electron backscatter diffraction, which includes performing line scanning on two sides of a target grain boundary in a calibration sample to obtain pattern quality BC values of Juchi lines of all sampling points on a line scanning path, performing unimodal fitting on all BC values and calculating half-height width of a fitting peak based on the principle that the minimum distance of the Juchi line pattern non-overlapping is spatial resolution, wherein the half-height width value corresponds to the spatial resolution of EBSD under the current working parameters, and accordingly, adjusting analysis parameters of the EBSD correspondingly. The analysis method provided by the embodiment utilizes the conventional grain boundary in the material microstructure, quantitatively analyzes the spatial resolution of the EBSD under the current working parameter more conveniently and rapidly, guides the analysis parameter of the EBSD according to the spatial resolution, and improves the accuracy of EBSD analysis on a sample to be analyzed.

After the spatial resolution of the EBSD under the current preset working parameters is accurately known, the target analysis parameters used when performing EBSD analysis on the sample to be analyzed can be guided and determined from two aspects. Based on the same inventive concept of the foregoing embodiment, in another alternative embodiment, the target analysis parameter includes a second scanning step or a target working parameter of the scanning electron microscope. The second scanning step length refers to a scanning step length range which should be adopted when EBSD line scanning or surface scanning is carried out on a sample to be analyzed; the target working parameter refers to a specific range of working parameters which should be set by the scanning electron microscope when the EBSD analysis is performed on a sample to be analyzed. As previously mentioned, the spatial resolution of an EBSD depends primarily on the spot size of the incident electron beam; meanwhile, during the EBSD analysis, the working parameters of the scanning electron microscope, such as the adopted accelerating voltage, the diaphragm aperture, the beam current of the electron beam and the like, also have obvious influence on the spatial resolution of the EBSD. Therefore, the target working parameter comprises at least one of acceleration voltage, electron beam current, diaphragm aperture and working distance.

Optionally, determining target analysis parameters when performing EBSD analysis on a sample to be analyzed according to the spatial resolution specifically includes: and when the sample to be analyzed is subjected to EBSD analysis, adjusting the second scanning step length to enable the second scanning step length to be larger than the spatial resolution. That is, the spatial resolution can be used to guide the minimum scanning step size of line scanning and area scanning in EBSD analysis, and a scanning step size smaller than the current spatial resolution has no detection significance and only increases unnecessary analysis time.

In some cases, a scanning step size smaller than the spatial resolution of the current preset working parameter needs to be adopted, for example, a higher spatial resolution is needed to detect a material sample with a smaller atomic number of a main component element, and at this time, the spatial resolution of the EBSD can be improved by adjusting the working parameter of the EBSD, so that the value of the spatial resolution is reduced to be below the second scanning step size. Optionally, determining target analysis parameters when performing EBSD analysis on a sample to be analyzed according to the spatial resolution specifically includes: and when the sample to be analyzed is subjected to EBSD analysis, adjusting the target working parameters of the scanning electron microscope so as to enable the EBSD spatial resolution under the target working parameters to be smaller than the second scanning step length. For example, the spatial resolution of EBSD can be improved by properly reducing the acceleration voltage, reducing the electron beam current, reducing the aperture of the diaphragm, shortening the working distance, and other working parameters. For example, the spatial resolution of the EBSD is improved by a single mode or a combined mode, such as reducing the acceleration voltage from 15kv to 12kv, reducing the electron beam current from 5nA to 2nA, reducing the diaphragm aperture from 50 micrometers to 30 micrometers, and shortening the working distance from 15mm to 13 mm.

The selection and preparation of calibration samples are very important for accurately determining the spatial resolution, and the grain boundary relief effect of the material is an important factor influencing the accurate determination of the spatial resolution. In order to eliminate the adverse effect of the grain boundary relief effect on the spatial resolution, based on the same inventive concept of the previous embodiment, in a further alternative embodiment, a calibration sample is prepared according to a preset process, specifically including: and (3) using the silica sol polishing solution to polish the surface of the selected sample at a low speed, wherein the polishing speed is 100-300 r/min, so as to obtain a calibration sample.

In the embodiment, the silica sol polishing solution is adopted to polish the selected sample or the sample to be calibrated at a low speed, so that not only can the residual stress of the material be removed, but also more importantly, the surface relief of the grain boundary can be eliminated, the problem that the measurement result of the spatial resolution is larger due to the relief effect is avoided, and the accuracy of the measurement result of the spatial resolution is improved.

Because the silica sol polishing solution is used for slow polishing, the grain boundary of the surface of the calibration sample can not be clearly identified under a scanning electron microscope, and in order to solve the problem, further, the target grain boundary of the calibration sample is determined, which specifically comprises the following steps: performing EBSD surface scanning on a local area of a calibration sample under a scanning electron microscope to obtain a surface-scanned Juliangchua pattern quality BC picture; and determining a clearly imaged grain boundary as a target grain boundary from the Juliangchua pattern quality BC picture.

For the shape specification of the sample, the sample is selected as a rectangular sample with the length of 10 mm-12 mm, the width of 5 mm-8 mm and the thickness of 1 mm-2 mm; the upper and lower surfaces of the rectangular sample were parallel to each other.

In the following embodiment, the scheme in the above embodiment is described in detail with reference to specific data:

in this example, the spatial resolution of EBSD is determined using ultra-low carbon IF steel as a calibration sample, and the following steps are performed:

(1) preparing a calibration sample: the sample size requires 10mm in length, 5mm in width and 1mm in thickness, the upper surface and the lower surface are ensured to be parallel, in order to eliminate the influence of the grain boundary relief effect on the resolution determination result during online scanning, the sample preparation adopts silica sol for slow polishing, the material of the silica sol is water-soluble silica, and the polishing speed is 150 r/m;

(2) determining preset working parameters of a scanning electron microscope: accelerating and pressurizing 15kV, the beam current is 2nA, the working distance WD is 15mm, and the aperture of the diaphragm is 30 mu m;

(3) determining the spatial resolution under the current working parameters: because the grain boundary on the surface of the sample obtained by slow polishing of the silica sol is not clear (see fig. 2), the EBSD surface scanning analysis needs to be performed on a local area to obtain a quality BC diagram of the chrysanthemum pool pattern of the local area (see fig. 3), a suitable grain boundary is found in the obtained backscatter diffraction image as a target grain boundary (located in a dotted line frame in fig. 3), then a line scan is performed on one side of the grain boundary along the vertical direction of the grain boundary (see a black dotted line in fig. 3), the first scanning step of the line scan is 3.5nm, the chrysanthemum pool pattern of each sampling point on the line scan path is obtained by passing through the grain boundary to the other side, a single peak curve is drawn according to the pattern quality (BC value) of the chrysanthemum pool pattern (see fig. 4), then single peak fitting and calculating corresponding half height width (see fig. 5) are performed by using Origin professional software, the half height width is 38nm, the same grain boundary is measured and averaged three times according to the above method, see table 1 below, which is the spatial resolution under the current conditions;

TABLE 1 half-height-width statistics of the same grain boundary measurement three times

(4) Determining target analysis parameters for 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, the second scanning step length of the surface scanning and the line scanning needs to be controlled to be more than 52nm when EBSD is carried out on a sample to be analyzed subsequently; if a scanning step size of less than 50nm, for example, about 40nm, is required for a certain analysis sample, the working parameters of the electron microscope should be adjusted to improve the spatial resolution of EBSD, so that the value of the spatial resolution is reduced to less than 40 nm.

Through one or more embodiments of the present invention, the present invention has the following advantageous effects or advantages:

the invention provides an analysis method of electron back scattering diffraction, which comprises the steps of performing line scanning on two sides of a target grain boundary in a calibration sample to obtain pattern quality BC values of Juchi lines of all sampling points on a line scanning path, performing unimodal fitting on all BC values and calculating the full width at half maximum of a fitting peak based on the principle that the minimum distance of the Juchi line patterns without overlapping is the spatial resolution, wherein the full width at half maximum corresponds to the spatial resolution of EBSD under the current working parameters, and correspondingly adjusting analysis parameters of the EBSD according to the full width at half maximum. The analysis method provided by the embodiment utilizes the conventional grain boundary in the material microstructure, quantitatively analyzes the spatial resolution of the EBSD under the current working parameter more conveniently and rapidly, guides the analysis parameter of the EBSD according to the spatial resolution, and improves the accuracy of EBSD analysis on a sample to be analyzed.

While the preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all alterations and modifications as fall within the scope of the application.

It will be apparent to those skilled in the art that various changes and modifications may be made in the present application without departing from the spirit and scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application is intended to include such modifications and variations as well.

12页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:一种脉冲磁场处理对金属零件微观组织影响的分析方法

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!

技术分类