CN102495088A - Method for quantifying analyzed result of electronic probe line/plane - Google Patents
Method for quantifying analyzed result of electronic probe line/plane Download PDFInfo
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- CN102495088A CN102495088A CN201110402411XA CN201110402411A CN102495088A CN 102495088 A CN102495088 A CN 102495088A CN 201110402411X A CN201110402411X A CN 201110402411XA CN 201110402411 A CN201110402411 A CN 201110402411A CN 102495088 A CN102495088 A CN 102495088A
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Abstract
The invention discloses a method for quantifying an analyzed result of an electronic probe line/plane. The method comprises the following steps of: firstly, carrying out line analysis and plane analysis on a segregation region; and combining a working curve to carry out quantification treatment on line and plane analyzed results, so as to obtain a quantitative distribution state of segregation region elements, wherein the accuracy of the results can be compared favorably with quantitative point analysis, the detection efficiency is greatly improved and the influences caused by external reasons on the results are smaller. The analysis method provided by the invention is simple and feasible, can be used as a common analysis skill to be popularized and applied in daily detection, and can provide more direct and accurate reference data.
Description
Technical field
The present invention relates to a kind of electron probe line, surface analysis result's quantitative method, the regional area that is mainly used at sample exists under the situation of element segregation, detects the quantitative distribution of segregation element.
Background technology
Electron probe (Electron Probe Microanalyzer, abbreviation EPMA or EPM), the element that is mainly used in the research material surface is formed and distribution.It is the characteristic X-ray that utilizes in the high-power electron beam excited sample that is focused into 1 μ m, detects the wavelength and the intensity of X ray again with spectrometer, confirms the composition and the content of element in the sample.Line, surface analysis technology are the major functions of electron probe, and promptly the element on analytic sample surface distributes and assemblage characteristic, but line, surface analysis technology belong to qualitative analysis, can not obtain the quantitative result that element distributes.
Simultaneously, quantitative result mainly is to obtain through quantitative point analysis in conventional art, though and quantitatively point analysis can obtain quantitative result accurately, the time of cost is long, workload is bigger, and the result is also than being easier to receive extraneous interference.
Summary of the invention
The objective of the invention is to provides a kind of electron probe line/surface analysis result's quantitative method to the deficiency that exists in the prior art, and its quantitative method through electron probe line, surface analysis result carries out the detection of the quantitative distribution of line of segragation element.
For realizing the foregoing invention purpose, the present invention has adopted following technical scheme:
A kind of electron probe line/surface analysis result's quantitative method is characterized in that this method is:
At first detect the requirement to sample according to electron probe, preparation has the testing sample in spot segregation zone;
Thereafter, with setting testing conditions examination criteria sample, and according to testing result drawing standard working curve;
At last, detect testing sample, and according to the aforesaid standards working curve, line, surface analysis result that detection is obtained carry out the quantification conversion to set testing conditions.
Further, said setting testing conditions comprises accelerating potential and electron beam line, and wherein, said accelerating potential is preferably 10-25KV, and the electron beam line is preferably 0.5 * 10
-7-1.5 * 10
-7A.
In this method line, surface analysis result being carried out the process that quantification transforms is: according to line, surface analysis result; The element that selection will transform; In conjunction with the slope and the intercept of the standard working curve of selected element, thereby obtain line, surface analysis result's quantification spectrogram.
Compared with prior art; The invention has the advantages that: the high efficiency through taking all factors into consideration line, surface analysis and quantitative two factors of accuracy of point analysis; Electron probe is combined with working curve in the line, the surface analysis result that measure the segregation zone, make line, surface analysis quantification as a result, distribute with quantitative form display element; Can compare favourably with quantitative point analysis through the line of above conversion, surface analysis result's accuracy; And significantly improved detection efficiency, the result receives the influence of external cause also smaller, thereby can more visual and accurate reference data be provided for research work.
Description of drawings
Fig. 1 a-1d is the working curve diagram of element M n, Cr, P and Si in the present invention's one preferred embodiment;
Fig. 2 is SWRH82B (Cr) martensitic backscattered electron image in wire rod central area and line analysis position photo in the present invention's one preferred embodiment;
Fig. 3 is the spectrogram as a result of M-region line analysis in the present invention's one preferred embodiment;
Fig. 4 is the spectrogram after the quantification conversion as a result of M-region line analysis in the present invention's one preferred embodiment;
The curve map that Fig. 5 draws for the quantitative point analysis result of M-region multiple spot in the present invention's one preferred embodiment.
Embodiment
Below in conjunction with an accompanying drawing and a preferred embodiment technical scheme of the present invention is further described.
Present embodiment electron probe line/surface analysis result's quantitative method comprises the steps:
The first step, according to the requirement of electron probe to sample, preparation sample SWRH82B (Cr) wire rod;
In second step,, adorn appearance with the dress appearance requirement of the sample for preparing according to electron probe;
The 3rd step was provided with accelerating potential, the analysis condition of a series of drawing curves such as electron beam line, and wherein accelerating potential is made as 15KV, and the electron beam line is made as: 1.0 * 10
-7A carries out the working curve of Mn, Cr, P and Si and draws, and the result sees Fig. 1.
In the 4th step, accelerating potential 15KV, electron beam line 1 * 10 are set
-7A; SWRH82B (Cr) wire rod central area martensite is carried out line, surface analysis test, and the line analysis spectrogram is the spectral line of one dimension, and ordinate is represented the counting rate of element; Qualitatively judge the changes of contents of element according to the fluctuating of curve; The result sees Fig. 3, and the surface analysis spectrogram is the scatter diagram of two dimension, goes up the dense degree of point and the qualitative comparison element changes of contents of counting of corresponding color bar according to figure.
The 5th step, line, surface analysis result's quantification step of converting (Quantitative yield with Mn element among the line analysis result is an example, the quantification conversion of other elements and the like):
(1) adopting day model of island proper Tianjin company production is EPMA-1610 type electron probe system software EPMA SYSTEM (Ver.3.05).
(2) on software EPMA SYSTEM (Ver.3.05) interface, click the Online program by right key; Calibration Curve Analysis (Curve) option below the selection Calibration Curve Analysis; The workmanship of Load institute makes curve file; Select the Make Curve button in the upper right corner, interface, select target Mn element is noted slope c, intercept d and the content range WT% of the Mn element working curve among the Coefficient.
(3) on software EPMA SYSTEM (Ver.3.05) interface, click the Offline program by right key, select Line Analysis-Data Processing, find the destination folder of line analysis result storage; Load line analysis spectrogram; Left mouse button is clicked Mn element spectrogram, clicks the Operate in the Line Analysis-Data Processing upper right corner by right key, selects Calibration Curve function; Point is opened Input Coefficient interface; The content range WT% of Mn element in the corresponding slope c of input Mn element working curve, intercept d and the working curve clicks Apply below Coefficient, can show the line analysis spectrogram after Mn element quantification transforms.
(4) quantification of other elements transforms referring to above-mentioned steps (2), (3) among the line analysis result, and the line analysis spectrogram after quantification transforms is seen Fig. 4.
(5) surface analysis result's quantification transforms the step of converting referring to the line analysis result, and the counting on the surface analysis spectrogram color bar after the conversion is converted into percentage composition, thereby can find out the constituent content scope in segregation zone intuitively.
In the 6th step, go on foot the accuracy after center line analysis result quantification transforms in order to verify the 5th, to the line analysis zone; Carried out the quantitative point analysis of multiple spot; Be depicted as line according to quantitative result then, carry out the comparison of constituent content with the line analysis result, the quantitative point analysis result of multiple spot sees Fig. 5.
In the test, line, the surface analysis result of M-region carried out the quantification conversion, purpose is exactly to distribute for the element that shows the segregation zone with quantitative form.Curve ratio from Fig. 4 and Fig. 5 can find out that because counting of line analysis is more much more than quantitative point analysis, so the variation tendency of curve more relaxes than quantitative distribution curve, details is more obvious.Can compare favourably with quantitative point analysis through the line of above conversion, surface analysis result's accuracy, and significantly improve detection efficiency, the result receives the influence of external cause also smaller.This kind method will provide more directly and reference data accurately for research work.
Claims (3)
1. electron probe line/surface analysis result quantitative method is characterized in that, this method is:
At first, detect the requirement to sample according to electron probe, preparation has the testing sample in spot segregation zone;
Thereafter, with setting testing conditions examination criteria sample, and according to testing result drawing standard working curve;
At last, detect testing sample, and according to the aforesaid standards working curve, line, surface analysis result that detection is obtained carry out the quantification conversion to set testing conditions.
2. electron probe line according to claim 1/surface analysis result's quantitative method is characterized in that said setting testing conditions comprises accelerating potential and electron beam line, and wherein, said accelerating potential is 10-25KV, and the electron beam line is 0.5 * 10
-7-1.5 * 10
-7A.
3. electron probe line according to claim 1/surface analysis result's quantitative method; It is characterized in that, according to line, surface analysis result, the element that selection will transform; In conjunction with the slope and the intercept of the standard working curve of selected element, thereby obtain line, surface analysis result's quantification spectrogram.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323480A (en) * | 2013-07-02 | 2013-09-25 | 首钢总公司 | Evaluation method of composition segregation of low-carbon high-manganese steel continuous casting small square billet |
| CN103363930A (en) * | 2013-07-02 | 2013-10-23 | 首钢总公司 | Method for measuring thickness of galvanized layer on steel plate |
| CN103411990A (en) * | 2013-08-23 | 2013-11-27 | 武汉钢铁(集团)公司 | Detection method for precipitated phases of nitride and oxide in steel-iron material |
| CN103454300A (en) * | 2013-09-06 | 2013-12-18 | 鞍钢股份有限公司 | Electronic probe line analysis quantitative test method of ultra-light element carbon |
| CN103604824A (en) * | 2013-11-28 | 2014-02-26 | 武汉钢铁(集团)公司 | Method for quantitative detection on steel wire rod carbon segregation |
| CN105181727A (en) * | 2015-09-17 | 2015-12-23 | 山东省分析测试中心 | Identification method of axle workpiece fracture failure crack initiation |
| CN105372275A (en) * | 2015-11-16 | 2016-03-02 | 南京钢铁股份有限公司 | Calibration method of martensite-austenite island in steel plate |
| CN105466961A (en) * | 2015-12-26 | 2016-04-06 | 首钢总公司 | Method for evaluating microsegregation of alloy elements of continuous casting billet |
| CN105806867A (en) * | 2016-05-25 | 2016-07-27 | 江苏省沙钢钢铁研究院有限公司 | Analytical method for quantitative evaluation of alloy element segregation in high-temperature alloy |
| CN106596615A (en) * | 2016-12-25 | 2017-04-26 | 首钢总公司 | Quantitative analysis method for continuous casting billet dendritic segregation |
| CN113447512A (en) * | 2021-03-16 | 2021-09-28 | 首钢集团有限公司 | Quantitative evaluation method for hypoeutectoid steel strip-shaped structure |
| CN114002250A (en) * | 2021-11-01 | 2022-02-01 | 江苏省沙钢钢铁研究院有限公司 | Method for removing peak interference of electronic probe line analysis and application thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323480A (en) * | 2013-07-02 | 2013-09-25 | 首钢总公司 | Evaluation method of composition segregation of low-carbon high-manganese steel continuous casting small square billet |
| CN103363930A (en) * | 2013-07-02 | 2013-10-23 | 首钢总公司 | Method for measuring thickness of galvanized layer on steel plate |
| CN103363930B (en) * | 2013-07-02 | 2016-03-30 | 首钢总公司 | A kind of method measuring steel plate galvanized layer thickness |
| CN103411990A (en) * | 2013-08-23 | 2013-11-27 | 武汉钢铁(集团)公司 | Detection method for precipitated phases of nitride and oxide in steel-iron material |
| CN103454300A (en) * | 2013-09-06 | 2013-12-18 | 鞍钢股份有限公司 | Electronic probe line analysis quantitative test method of ultra-light element carbon |
| CN103604824A (en) * | 2013-11-28 | 2014-02-26 | 武汉钢铁(集团)公司 | Method for quantitative detection on steel wire rod carbon segregation |
| CN105181727A (en) * | 2015-09-17 | 2015-12-23 | 山东省分析测试中心 | Identification method of axle workpiece fracture failure crack initiation |
| CN105372275A (en) * | 2015-11-16 | 2016-03-02 | 南京钢铁股份有限公司 | Calibration method of martensite-austenite island in steel plate |
| CN105466961A (en) * | 2015-12-26 | 2016-04-06 | 首钢总公司 | Method for evaluating microsegregation of alloy elements of continuous casting billet |
| CN105806867A (en) * | 2016-05-25 | 2016-07-27 | 江苏省沙钢钢铁研究院有限公司 | Analytical method for quantitative evaluation of alloy element segregation in high-temperature alloy |
| CN105806867B (en) * | 2016-05-25 | 2018-11-06 | 江苏省沙钢钢铁研究院有限公司 | The analysis method of segregation in a kind of quantitative assessment high temperature alloy |
| CN106596615A (en) * | 2016-12-25 | 2017-04-26 | 首钢总公司 | Quantitative analysis method for continuous casting billet dendritic segregation |
| CN113447512A (en) * | 2021-03-16 | 2021-09-28 | 首钢集团有限公司 | Quantitative evaluation method for hypoeutectoid steel strip-shaped structure |
| CN113447512B (en) * | 2021-03-16 | 2024-02-06 | 首钢集团有限公司 | Quantitative assessment method for hypoeutectoid steel strip-shaped structure |
| CN114002250A (en) * | 2021-11-01 | 2022-02-01 | 江苏省沙钢钢铁研究院有限公司 | Method for removing peak interference of electronic probe line analysis and application thereof |
| CN114002250B (en) * | 2021-11-01 | 2024-05-03 | 江苏省沙钢钢铁研究院有限公司 | Method for removing analysis peak interference of electronic probe line and application thereof |
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Application publication date: 20120613 |