CN103472082A - Quantitative line scanning method for curved surface sample electronic probe - Google Patents
Quantitative line scanning method for curved surface sample electronic probe Download PDFInfo
- Publication number
- CN103472082A CN103472082A CN2013104032929A CN201310403292A CN103472082A CN 103472082 A CN103472082 A CN 103472082A CN 2013104032929 A CN2013104032929 A CN 2013104032929A CN 201310403292 A CN201310403292 A CN 201310403292A CN 103472082 A CN103472082 A CN 103472082A
- Authority
- CN
- China
- Prior art keywords
- sample
- quantitative
- curved surface
- scanning
- coordinate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000523 sample Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 238000005259 measurement Methods 0.000 claims abstract description 3
- 238000013507 mapping Methods 0.000 claims description 11
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000010183 spectrum analysis Methods 0.000 claims description 3
- 238000007689 inspection Methods 0.000 abstract 2
- 238000002083 X-ray spectrum Methods 0.000 abstract 1
- 230000001133 acceleration Effects 0.000 abstract 1
- 238000010586 diagram Methods 0.000 abstract 1
- 238000010894 electron beam technology Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Images
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a quantitative line scanning method for an electronic probe of a curved surface sample, which comprises the steps of finding a sample analysis area by using a back-scattered electron image, setting electron microscope acceleration voltage, electron beam current, beam spot size, minimum moving step length of a surface distribution diagram and a grid data dot matrix, reading the coordinate position of a current point, moving the next point and reading the coordinate of the point until all grid point coordinate positions are completely read; obtaining an element intensity surface scanning image of an analysis area by utilizing element characteristic X-ray spectrum analysis, testing the X-ray intensity of a standard sample of the analyzed element, and converting the X-ray intensity of an original counting surface scanning result into concentration content to obtain a quantitative surface distribution map; and obtaining a quantitative line scanning curve of the curved surface sample by using line scanning. The invention can correct the measurement error generated by the concave-convex surface of the sample, improve the inspection efficiency and the inspection precision, effectively solve the problem that the electronic probe can only analyze flat samples, and enlarge the sample range of the electronic probe analysis.
Description
Technical field
The invention belongs to metallurgical analysis check field, be specifically related to a kind of quantitative line sweep method of electron probe for the curved surface sample.
Background technology
The linescan of electron probe can qualitative, quantitative ground be described the segregation rate of certain composition in sample, can understand the rate of propagation of certain element and measure thickness of diffusion layer, can judge in sample the element degree etc. that is evenly distributed, so the line scanning of electron probe is the extremely useful analysis means of steel products.
But not all samples can adopt electron probe to carry out line scanning, because electron probe requires sample to reach the smooth degree of minute surface, otherwise can produce great measuring error, the analysis result that must make mistake.For example, certain sample is distributed components originally, and line scanning but draws element segregation rate 80%, and this analysis result is exactly because this sample surfaces is smooth not, is revised again and the wrong conclusion that draws.
Sample, because the reasons such as use, processing often can produce torsional deformation, makes sample to be analyzed smooth not, but urgent hope is understood the distribution situation of element on this type of sample to solve a research and production difficult problem.Therefore, be necessary to invent a kind of quantitative line sweep method that is applicable to the curved surface sample.
Summary of the invention
The present invention is intended to solve the problem that electron probe can only be analyzed flat sample, thereby providing a kind of can revise due to concavo-convex the produced measuring error of sample, enlarge electron probe sample analysis scope, improve the quantitative line sweep method of curved surface sample electron probe of checkability and precision.
For this reason, the solution that the present invention takes is:
A kind of quantitative line sweep method of curved surface sample electron probe, its concrete steps are:
1, determine analyzed area
Clean analytic sample is put into to the EPMA-1610 of Shimadzu company electron probe sample chamber, by backscattered electron image, find sample analysis area.
2, parameter setting
The Electronic Speculum parameter: during measurement, accelerating potential is 15-25kV, and electronic beam current is 20-200nA, and beam spot size is 1;
The mapping parameter arranges: selecting scan mode in menu is sample stage scanning, minimum moving step length 1.0, coordinate manual positioning;
The sample stage sweep parameter arranges: the scanning residence time is greater than 30ms, and moving step length is greater than 1.0 * 1.0;
Trace Map parameter arranges: the grid data dot matrix is greater than 9 * 9, reads current point coordinate position, moves to next point, and Manual focusing reads this point coordinate again, repeats above-mentioned steps until the coordinate position of the interior all net points of analyzed area all reads complete; Above-mentioned coordinate is calculated to rear preservation result of calculation.
3, obtain original face scanning distribution plan, utilize the Spectrum Analysis of elemental characteristic X ray to obtain analyzed area element X ray intensity face scintigram.
4, be converted to quantitative mapping, the standard sample X ray intensity at same test condition test institute analytical element, become concentration content by the X ray intensity conversion in original counting face scanning result, obtains quantitative mapping.
5, Line Profile line sweep
Quantitatively in mapping, applying Line Profile line sweep, obtain the quantitative linescan of the curved surface sample through revising.
Beneficial effect of the present invention is:
The present invention can revise concavo-convex the produced measuring error of sample surfaces, greatly improves checkability and testing accuracy, effectively solves the problem that electron probe can only be analyzed flat sample, and the sample scope of electron probing analysis is further enlarged.Especially not minute surface flat sample and the curved surface sample that distortion is arranged for specimen surface, through revising, can obtain accurately quantitatively line sweep result yet.
The accompanying drawing explanation
Fig. 1 is Comparative Examples linescan figure;
Fig. 2 is linescan figure after correction of the present invention.
Embodiment
Embodiment adopts the quantitative line sweep method of curved surface sample of the present invention, and uneven sample is carried out to line scanning.Its step is as follows:
1. clean analytic sample is put into to the electron probe sample chamber, by backscattered electron image, find sample analysis area.
2., while measuring, select the Electronic Speculum running parameter, accelerating potential 15kV, electronic beam current is selected 100nA, beam spot size 1.The mapping parameter is selected: scan mode is sample stage scanning, minimum moving step length 1.0, and the coordinate manual positioning, Trace Map selects YES.Sample stage scanning residence time 30ms, moving step length 6.0 X 6.0.The corrected parameter of curved surface sample is set to 9 * 9 grids, after reading current point coordinate, moves to next point coordinate, and Manual focusing reads this point coordinate again, repeats above-mentioned steps until the coordinate position of interior all 81 points of analyzed area all reads complete.Above-mentioned coordinate is calculated to rear preservation result of calculation.
3. obtain the original face scanning result.Utilize the Spectrum Analysis of the characteristic X-ray of element to carry out the scanning of ferro element X ray intensity face to analyzed area.
4. the original face distribution plan is converted to quantitative mapping.Under same test condition, the standard sample X ray intensity of test institute analytical element, become concentration content by the X ray intensity conversion in original counting face scanning result.
5.Line Profile line sweep.Quantitatively in mapping, applying the quantitative linescan that line sweep Line Profile obtains the curved surface sample through revising.
Fig. 1 is Comparative Examples linescan figure, ferro element average content 62.26%; Fig. 2 is linescan figure after correction of the present invention, ferro element average content 97.74%.From Fig. 1, Fig. 2, can find out, for same sample, under identical test condition, the present invention has successfully repaired the huge measuring error that the concavo-convex difference due to sample produces.
Claims (1)
1. the quantitative line sweep method of curved surface sample electron probe, is characterized in that, concrete steps are:
(1), determine analyzed area
Clean analytic sample is put into to the electron probe sample chamber, by backscattered electron image, find sample analysis area;
(2), parameter setting
The Electronic Speculum parameter: during measurement, accelerating potential is 15-25kV, and electronic beam current is 20-200nA, and beam spot size is 1;
The mapping parameter arranges: selecting scan mode in menu is sample stage scanning, minimum moving step length 1.0, coordinate manual positioning;
The sample stage sweep parameter arranges: the scanning residence time is greater than 30ms, and moving step length is greater than 1.0 * 1.0;
Trace Map parameter arranges: the grid data dot matrix is greater than 9 * 9, reads current point coordinate position, moves to next point, and Manual focusing reads this point coordinate again, repeats above-mentioned steps until the coordinate position of the interior all net points of analyzed area all reads complete; Above-mentioned coordinate is calculated to rear preservation result of calculation;
(3), obtain original face scanning distribution plan, utilize the Spectrum Analysis of elemental characteristic X ray to obtain analyzed area element X ray intensity face scintigram;
(4), be converted to quantitative mapping, the standard sample X ray intensity at same test condition test institute analytical element, become concentration content by the X ray intensity conversion in original counting face scanning result, obtains quantitative mapping;
(5), Line Profile line sweep
Quantitatively in mapping, applying Line Profile line sweep, obtain the quantitative linescan of the curved surface sample through revising.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013104032929A CN103472082A (en) | 2013-09-07 | 2013-09-07 | Quantitative line scanning method for curved surface sample electronic probe |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013104032929A CN103472082A (en) | 2013-09-07 | 2013-09-07 | Quantitative line scanning method for curved surface sample electronic probe |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103472082A true CN103472082A (en) | 2013-12-25 |
Family
ID=49797021
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013104032929A Pending CN103472082A (en) | 2013-09-07 | 2013-09-07 | Quantitative line scanning method for curved surface sample electronic probe |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103472082A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113009324A (en) * | 2021-05-24 | 2021-06-22 | 中国电子科技集团公司第二十九研究所 | Curved surface multi-probe test fixture |
| CN114739342A (en) * | 2022-04-08 | 2022-07-12 | 河北光兴半导体技术有限公司 | Method for measuring thickness of ultrathin glass stress layer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1661363B (en) * | 1998-11-10 | 2011-03-23 | 株式会社岛津制作所 | Electro-probe micro analyzer |
| JP2012078234A (en) * | 2010-10-04 | 2012-04-19 | Jeol Ltd | X-ray analysis method and apparatus |
| CN102954976A (en) * | 2011-08-19 | 2013-03-06 | 鞍钢股份有限公司 | Quantitative detection method for center segregation of wire rod |
-
2013
- 2013-09-07 CN CN2013104032929A patent/CN103472082A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1661363B (en) * | 1998-11-10 | 2011-03-23 | 株式会社岛津制作所 | Electro-probe micro analyzer |
| JP2012078234A (en) * | 2010-10-04 | 2012-04-19 | Jeol Ltd | X-ray analysis method and apparatus |
| CN102954976A (en) * | 2011-08-19 | 2013-03-06 | 鞍钢股份有限公司 | Quantitative detection method for center segregation of wire rod |
Non-Patent Citations (3)
| Title |
|---|
| 张文兰等: "电子探针面分析与相分析技术及其应用", 《电子显微学报》 * |
| 杨勇，陈能松: "电子探针线扫描分析技术", 《电子显微学报》 * |
| 潘清林: "《材料现代分析测试实验教程》", 31 August 2011, 冶金工业出版社，北京大学出版社，国防工业出版社，哈尔滨工业大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113009324A (en) * | 2021-05-24 | 2021-06-22 | 中国电子科技集团公司第二十九研究所 | Curved surface multi-probe test fixture |
| CN114739342A (en) * | 2022-04-08 | 2022-07-12 | 河北光兴半导体技术有限公司 | Method for measuring thickness of ultrathin glass stress layer |
| CN114739342B (en) * | 2022-04-08 | 2023-08-11 | 河北光兴半导体技术有限公司 | Method for measuring thickness of ultrathin glass stress layer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sobel et al. | Influence of etching conditions on apatite fission-track etch pit diameter | |
| Hwang et al. | Three-dimensional imaging of individual dopant atoms in SrTiO 3 | |
| CN103558237B (en) | Three-dimensional precision measurement and calibration method for industrial CT (computed tomography) | |
| US9129353B2 (en) | Charged particle beam device, and image analysis device | |
| CN103454300A (en) | Electronic probe line analysis quantitative detection method for ultra-light element carbon | |
| JPWO2019059011A1 (en) | Teacher data creation method and equipment and defect inspection method and equipment | |
| WO2010029700A1 (en) | Charged particle beam device | |
| CN105510362B (en) | Rice tillering character damage-free measuring apparatus and its measurement method based on minitype CT | |
| CN103604824A (en) | Method for quantitative detection on steel wire rod carbon segregation | |
| CN102636488A (en) | Quantitative measurement method for sorbite content in high-carbon steel rod | |
| CN102426119A (en) | Preparation method of structure section sample of small-sized wafer sample for observation | |
| Gong et al. | Comparison of simultaneous signals obtained from a dual-field-of-view lidar and its application to noise reduction based on empirical mode decomposition | |
| JP2007183231A (en) | Method for processing eddy current flaw detection signal | |
| CN108008000A (en) | A kind of method for measuring the brannerite age | |
| CN109030462A (en) | Different type inclusion area and the quantitatively characterizing method of content in a kind of steel | |
| CN104215489A (en) | Preparation method of retained austenite standard sample of high-carbon chromium bearing steel | |
| CN106098518A (en) | Use the adaptive scanning of the particle size of directional beam signal analysis | |
| CN105093166B (en) | A kind of field test method of electronic electric energy meter | |
| CN103472082A (en) | Quantitative line scanning method for curved surface sample electronic probe | |
| JP5187810B2 (en) | Film thickness measuring method and sample preparation method, film thickness measuring apparatus and sample preparation apparatus | |
| CN109884180A (en) | A kind of sparse current vortex fast imaging detection method of conductive structure defect and system | |
| US20150012229A1 (en) | Sample analysis apparatus, non-transitory computer-readable recording medium and sample analysis method | |
| Jenson et al. | A Bayesian approach for the determination of POD curves from empirical data merged with simulation results | |
| CN111579572A (en) | Hierarchical quantitative analysis method for material surface topological structure and application | |
| CN109668862B (en) | Aluminum electrolyte molecular ratio detection method based on laser-induced breakdown spectroscopy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131225 |