CN107290199A - A kind of method that utilization electron probe quickly characterizes bearing steel segregation - Google Patents
A kind of method that utilization electron probe quickly characterizes bearing steel segregation Download PDFInfo
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- CN107290199A CN107290199A CN201710680896.6A CN201710680896A CN107290199A CN 107290199 A CN107290199 A CN 107290199A CN 201710680896 A CN201710680896 A CN 201710680896A CN 107290199 A CN107290199 A CN 107290199A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of method that utilization electron probe quickly characterizes steel segregation, tested using electron microprobe examination, segregation element species in steel is determined using spectrometer point analysis function, carry out being scanned whole specimen surface by spectrometer Surface scan function, the segregation of sample is intuitively characterized using colouring discrimination, is easy to the degree of segregation of apparent observation steel.This method, which has broken electron probe, can only carry out the limitation of micro-zone analysis, can carry out big regional segregation and be particularly that the sign of strand segregation can be carried out.The inventive method is few by interference from human factor, and it can quickly carry out the phenetic analysis of large area element segregation degree in steel, efficiently solve electron probe prior art can only micro-zone analysis element segregation the problem of, there is important reference significance to steel grades and process modification.
Description
Technical field
The invention belongs to detection technique field, more particularly to a kind of utilization electron probe quickly characterizes the side of bearing steel segregation
Method.
Background technology
High-carbon-chromium bearing steel has the higher performance characteristics of intensity, and this feature requires that its continuous casting billet must have well
Solidification Quality, it is to avoid center segregation occur, the defect such as loose and crackle.Macroscopical carbon segregation is used as the common quality of high carbon bearing steel
Problem, fairly obvious to the aging effects of bearing steel, the solidification structure of its formation mechenism and high-carbon Continuous Casting Bloom of Bearing Steel is close
Cut is closed.Strand is changed in operation of rolling tissue, but the distribution of carbon segregation and form are still remained, simply segregation
Degree has obtained a certain degree of improvement, it can be seen that carbon segregation has heredity, and stocking carbon segregation is hereditary from continuous casting billet.Cause
This, accurately evaluate sign segregation has good directive significance to the performance improvement and process modification of bearing steel, at present, evaluates
Bearing steel segregation is mainly carried out by low power experiment, but low power experiment is by extent of corrosion and the factor shadow such as artificially defined
Ring, there is certain error.And segregation sign is carried out using ESEM and electron probing analysis, and will because being prepared to sample
Ask comparison high, and the phenetic analysis time is long and limited.
The content of the invention
The present invention is intended to provide one kind can reduce interference caused by subjective factors, while it is inclined accurately can quickly to characterize bearing steel again
The method of analysis, mainly uses electron probe surface analysis function, to carrying out quick Surface scan point in bearing steel strand or stocking
Analysis, it is ensured that the accuracy and rapidity of analysis.
Adopt this method and carry out the quick segregation problems for characterizing bearing steel, change what subjective factor in former method was caused
Error is big, can accurately demarcate bearing steel degree of segregation, compensate for the deficiency of former method, to steel grades and process modification
With important reference significance.
Therefore, the inventive method is adopted the technical scheme that：
First, it is ensured that the flatness and smoothness of sample, to ensure the accuracy of result of the test；Secondly the detection faces of sample are determined
Product rower of going forward side by side is determined, and detection range is comparative in favor of result from sheet material edge to center portion；Furthermore ensuring in scanning process
It is scanned on the premise of accuracy with most rapid rate, efficiency is improved with this.Electron microprobe examination test vacuum is 10- 4Pa, Surface scan is carried out using spectrometer to bearing steel；Scanning beam is scanned along selected detection range, analytical element
For C, Cr, segregated zone is determined by the change of C element and Cr element count rate intensity, intuitively reaction is face to the intensity of counting rate
The change of color, color is more black to represent that intensity is higher, as segregated zone, and vice versa.
The spectroscopic signal drift value of the spectrometer is less than 1 μm, and the accelerating potential of scanning beam is 15kV.
Specifically, the quick method for characterizing bearing steel segregation of the present invention, the successively polishing step including sample, polishing is walked
Suddenly, corrosion step, scanning area demarcating steps and phenetic analysis step；It is characterized in that the phenetic analysis step is specifically included
Following steps：
1）The sample being scanned through after region labeling processing is solid together with the standard sample provisioned in electron microprobe examination
It is scheduled on professional sample stage, professional sample stage is placed into the test sample pallet of electron microprobe examination, then by specialty
Sample stage is evacuated to vacuum and is not more than 10-4Pa；
2）Professional sample stage is moved to the position of standard sample, sympodium is carried out to electron beam, regulation electron gun filament is heated to electricity
Beamlet stream saturation point；
3）The position of electron microprobe examination is adjusted, professional sample stage is moved to testing sample position from the position of standard sample
Put；Regulation light microscope makes optical imagery clear, and adjustment electronic beam current causes secondary electron image clear；Choose heater current
And beam spot size, to determine analytical element as C and Cr；
4）In step 3）Determine after analytical element, spectrometer, which is proceeded by, searches peak；
5）Determine Surface scan scope, it is ensured that scanning range covers the edge and center portion of sample, i.e., the region progress face of demarcation is swept
Analysis is retouched, and confirmation is scanned to detection range using Trace Point methods；
6）Scan mode is defined as Stage Scan, and Pitch is to ensure sweep time as 30 ~ 40min for adjustment scanning, spectrometer
Electron beam is with perpendicular to the sightingpiston of bearing steel curved beam progress Surface scan and record data；
7）Data are handled after the end of scan, the change of Surface scan result intensity is analyzed, determines the segregation situation of bearing steel.
Beneficial effects of the present invention are：
The inventive method is simple and easy to apply, few by interference from human factor, is remarkably improved the accuracy of bearing steel segregation sign, solves
The problem of test result that prior art is present is inaccurate, to further investigate the formation mechenism of bearing steel segregation and its to steel plate
Structure property influence provides data basis.
Brief description of the drawings
Fig. 1 is the secondary electron image in bearing steel segregation electron probing analysis process scanning region；
Fig. 2 is C element segregation status schematic diagram；
Fig. 3 is Cr element segregation views.
Embodiment
Below, by embodiment, the present invention will be further described.
Instrument in embodiment：
Electron microprobe examination：
SHIMADZU EPMA-1720 types electron microprobe examinations and its supporting spectrometer（WDS）.
(1) sample preparation：Steel plate is cut, the sample that section is 25 × 17mm is made, specimen length includes steel plate edge
And center portion, the longitudinal section by sample along rolling direction（That is the cross section in thickness of slab direction）Successively through 180#, 600#, 800#, 1000#
Waterproof abrasive paper is polished, and is then polished with polishing agent, is corroded with 4% nitric acid alcohol（It is defined so that tissue can be distinguished）, it is aobvious by metallographic
The region for carrying out phenetic analysis is bound by micro mirror, and is demarcated the region defined with microhardness instrument, then again will
Sample is ground polishing, it is ensured that the microhardness marking it is observed that.Ensure absolute smooth, 0.04 μm of the finish of sightingpiston.
(2) analysis and calculating of sample：
The sample prepared is fixed on professional sample stage together with the professional standard sample provisioned in electron microprobe examination
On, professional sample stage is placed into the test sample pallet of electron microprobe examination, vacuumized, the vacuum of test request is reached
Degree 10-4After Pa, sample stage is moved into standard sample position, sympodium is carried out to electron beam according to operational procedure, filament saturation point is adjusted,
After condition to be tested is all met, tested.
Electron microprobe examination position is adjusted, professional sample stage is moved to testing sample position from standard sample position,
Regulation light microscope makes optical imagery clear, and selection appropriate electronic line makes secondary electron image clear, regulation contrast, bright
Degree, accelerating potential is 15kV, chooses suitable heater current and beam spot size, and it is C and Cr to determine analytical element, and element is first after determining
First carry out searching peak, then choose correct position from left to right, from top to bottom carry out Surface scan, scanning area is 22 × 15mm, choosing
Set and Trace Point methods are utilized after scanning range, choose 5 × 5 and be scanned region labeling, to ensure visual field during scanning
Definition and the degree of accuracy, scanning range is defined by the edge and center portion for covering whole sample.Scan mode is Stage Scan,
Pitch is to ensure sweep time as 30 ~ 40min for adjustment scanning, and the electron beam of spectrometer is with perpendicular to the progress of the sightingpiston of sample
Surface scan and record data.After the end of scan as needed carry out data processing, scanning color change and intensity change with partially
The corresponding relation of analysis, meets steel plate edge color based on light color, in the absence of segregation, close to center portion, and color is gradually become by light color
It is changed into black, center portion is clearly present the ribbon tissue of black, there is segregation.
The result of the bearing steel segregation measured using the present invention is accurate.
Using the segregation of electron microprobe examination and spectrometer phenetic analysis bearing steel, Fig. 1 is the secondary electricity of scanning area
Subgraph, is from left to right from sample edge to center portion so not observing segregation status for polishing state image.Fig. 2 is C members
Plain segregation status, color is deeper, and explanation C content is higher, can be shown from figure, and sample edge does not have segregation, and center portion has C members
Plain segregation, and into ribbon, i.e. center portion black ribbon region be C element segregated zone.Fig. 3 is Cr element segregation states, and color is got over
Deep explanation Cr constituent contents are higher, can be shown from figure, sample edge does not have Cr segregations, and center portion has Cr element segregations, i.e.,
Center portion black ribbon region is Cr element segregation bands.Fig. 2 and Fig. 3 results show that Cr element segregations band is kissed with C element segregated zone
Close, be close to sample center portion region.As illustrated, color change and segregation result fit like a glove.
Claims (10)
1. a kind of method of quick sign bearing steel segregation, successively the polishing step including sample, polishing step, corrosion step,
Scanning area demarcating steps and phenetic analysis step；It is characterized in that the phenetic analysis step specifically includes following step
Suddenly：
1）The sample being scanned through after region labeling processing is solid together with the standard sample provisioned in electron microprobe examination
It is scheduled on professional sample stage, professional sample stage is placed into the test sample pallet of electron microprobe examination, then by specialty
Sample stage is evacuated to vacuum and is not more than 10-4Pa；
2）Professional sample stage is moved to the position of standard sample, sympodium is carried out to electron beam, regulation electron gun filament is heated to electricity
Beamlet stream saturation point；
3）The position of electron microprobe examination is adjusted, professional sample stage is moved to testing sample position from the position of standard sample
Put；Regulation light microscope makes optical imagery clear, and adjustment electronic beam current causes secondary electron image clear；Choose heater current
And beam spot size, to determine analytical element as C and Cr；
4）In step 3）Determine after analytical element, spectrometer, which is proceeded by, searches peak；
5）Determine Surface scan scope, it is ensured that scanning range covers the edge and center portion of sample, i.e., the region progress face of demarcation is swept
Analysis is retouched, and confirmation is scanned to detection range using Trace Point methods；
6）Scan mode is defined as Stage Scan, and Pitch is to ensure sweep time as 30 ~ 40min for adjustment scanning, spectrometer
Electron beam is with perpendicular to the sightingpiston of bearing steel curved beam progress Surface scan and record data；
7）Data are handled after the end of scan, the change of Surface scan result intensity is analyzed, determines the segregation situation of bearing steel.
2. quick sign bearing steel segregation method according to claim 1, it is characterised in that：In polishing step, by sample
Cross section of the product along thickness of slab direction is polished step by step through 180#, 600#, 800# and 1000# waterproof abrasive paper successively.
3. the method for quick sign bearing steel segregation according to claim 1, it is characterised in that：In the corrosion step
In, the sample after sanding and polishing is corroded with 3% ~ 4% nitric acid alcohol.
4. the method for quick sign bearing steel segregation according to claim 1, it is characterised in that：In the scanning area mark
Determine in step, be first bound the region for carrying out phenetic analysis by metallographic microscope, and will be defined with microhardness instrument
Region demarcated, sample is then ground polishing again, it is ensured that the microhardness marking it is observed that.
5. the method for quick sign bearing steel segregation according to claim 4, it is characterised in that：Grinding and polishing ensures sample
Sightingpiston is smooth, and finish is 0.04 μm.
6. quick sign bearing steel segregation method according to claim 1, it is characterised in that：In step 3）In, the electricity
The spectroscopic signal drift value of sub- probe analyzer is less than 1 μm, and the accelerating potential of scanning beam is 15kV.
7. the method for quick sign bearing steel segregation according to claim 1, it is characterised in that：The electron probing analysis
Instrument environment temperature is 20 ~ 25 DEG C, relative humidity 50 ~ 70%, and supply voltage and frequency are respectively 220V ± 10%, 50Hz ± 1Hz.
8. quick sign bearing steel segregation method according to claim 1, it is characterised in that：In step 7）In, spectrometer
During Surface scan, from left to right, from top to bottom it is scanned.
9. quick sign bearing steel segregation method according to claim 1, it is characterised in that：In step 1）In, it is described special
The vacuum of industry sample stage is 10-4 Pa。
10. steel according to claim 1 quickly characterizes bearing steel segregation method, it is characterised in that：The electron probe point
Analyzer model SHIMADZU EPMA-1720 types, its supporting spectrometer WDS.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109959671A (en) * | 2019-03-27 | 2019-07-02 | 南京钢铁股份有限公司 | A kind of method of quantitative analysis plate segregation |
| CN110031347A (en) * | 2019-04-02 | 2019-07-19 | 鞍钢股份有限公司 | Method for measuring segregation of spring steel wire rod |
| CN110470687A (en) * | 2019-07-22 | 2019-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Properties of Heavy Rail Steel microsegregation quickly positions evaluation method |
| CN111215592A (en) * | 2020-02-21 | 2020-06-02 | 东北大学 | Heavy rail steel continuous casting billet segregation defect inheritance research method and application thereof |
| CN113655079A (en) * | 2021-07-30 | 2021-11-16 | 宁波锦越新材料有限公司 | Method for detecting 6061 aluminum alloy precipitate |
| CN114518376A (en) * | 2022-02-18 | 2022-05-20 | 中国核动力研究设计院 | Electronic probe shielding sample seat of radioactive sample |
| CN115266795A (en) * | 2022-07-29 | 2022-11-01 | 中国核动力研究设计院 | Method for representing diffusion behavior of fission gas product of strong radioactive fuel element |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104596901A (en) * | 2015-01-09 | 2015-05-06 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring austenite grain size |
| 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 |
| CN105445306A (en) * | 2015-11-16 | 2016-03-30 | 南京钢铁股份有限公司 | Method for evaluating element segregation degree in steel |
-
2017
- 2017-08-10 CN CN201710680896.6A patent/CN107290199A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104596901A (en) * | 2015-01-09 | 2015-05-06 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring austenite grain size |
| 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 |
| CN105445306A (en) * | 2015-11-16 | 2016-03-30 | 南京钢铁股份有限公司 | Method for evaluating element segregation degree in steel |
Non-Patent Citations (1)
| Title |
|---|
| 吴园园等: "电子探针分析方法及在材料研究领域的应用", 《电子显微学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109959671A (en) * | 2019-03-27 | 2019-07-02 | 南京钢铁股份有限公司 | A kind of method of quantitative analysis plate segregation |
| CN110031347A (en) * | 2019-04-02 | 2019-07-19 | 鞍钢股份有限公司 | Method for measuring segregation of spring steel wire rod |
| CN110470687A (en) * | 2019-07-22 | 2019-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Properties of Heavy Rail Steel microsegregation quickly positions evaluation method |
| CN111215592A (en) * | 2020-02-21 | 2020-06-02 | 东北大学 | Heavy rail steel continuous casting billet segregation defect inheritance research method and application thereof |
| CN111215592B (en) * | 2020-02-21 | 2020-11-17 | 东北大学 | Heavy rail steel continuous casting billet segregation defect inheritance research method and application thereof |
| CN113655079A (en) * | 2021-07-30 | 2021-11-16 | 宁波锦越新材料有限公司 | Method for detecting 6061 aluminum alloy precipitate |
| CN114518376A (en) * | 2022-02-18 | 2022-05-20 | 中国核动力研究设计院 | Electronic probe shielding sample seat of radioactive sample |
| CN114518376B (en) * | 2022-02-18 | 2024-08-23 | 中国核动力研究设计院 | Electron probe shielding sample seat for radioactive sample |
| CN115266795A (en) * | 2022-07-29 | 2022-11-01 | 中国核动力研究设计院 | Method for representing diffusion behavior of fission gas product of strong radioactive fuel element |
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Application publication date: 20171024 |