CN103900889A - Chemical polishing method for electrical silicon steel EBSD (electron back-scattered diffraction) sample - Google Patents
Chemical polishing method for electrical silicon steel EBSD (electron back-scattered diffraction) sample Download PDFInfo
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Abstract
The invention discloses a chemical polishing method for an electrical silicon steel EBSD (electron back-scattered diffraction) sample. The chemical polishing method comprises the following operating steps of (1) embedding; (2) mechanical polishing; (3) chemical polishing; and (4) removal of corrosive products. The chemical polishing method for the electrical silicon steel EBSD sample has the advantages of simplicity, quickness, low cost, good polishing effect, repeated use of polishing liquid and no need of special electrolytic polishing equipment, and the polished sample meets an EBSD analysis requirement.
Description
Technical field
The present invention relates to electrical steel EBSD sample preparation technology field, specifically a kind of electrical steel EBSD sample chemical finishing method.
Background technology
The grain orientation of electrical steel distributes and microstructure state is the key factor that affects its electromagnetic performance, EBSD is the important means of studying now electrical steel grain orientation and microstructure, and the preparation quality of analytic sample has determined the correctness of EBSD analysis result to a great extent.
Electron Back-Scattered Diffraction (EBSD) is that one is based upon on crystallographic analysis basis, carrys out the technology of research material micromechanism by scanning electron microscope.EBSD, except providing absolute crystal orientation information, can also be used for texture and the misorientation analysis of material; Crystallite dimension and morphological analysis; Crystal boundary, subgrain and twin property analysis; The identification of phases and compare calculating; Strain measurement; All many-sides such as fracture mechanism, failure mechanism.EBSD has several large advantages: 1. will between microstructure and crystallography, contact directly; 2. can obtain fast and exactly the bulk information of crystal space constituent element; 3. can select any visual field with scope more widely.All this kind, EBSD technology more and more welcomed by the people.Existing many reports aspect electrical steel research and development.
EBSD using near sample surfaces as analytic target, only occur near the lattice (depth rangees of 5～50 nm) on the extremely shallow top layer of sample, so very responsive to sample surfaces state, require sample surfaces not residual process strained layer, need level and smooth, No oxided film, without continuous etch pit.Sample wide-angle tilt (is generally 70
o) also need sample to keep best surface state (try one's best few uneven) to avoid the generation of shade, to this means that how important sample preparation is to collecting EBSD information accurately.
The preparation of EBSD metal sample is generally first to use sand paper pre-grinding, then arrives minute surface with diamond polishing, then does final polishing by electrolytic process and eliminate surface strain layer.Also have only mechanical buffing, but sample finished surface deformation layer can not be effectively removed in mechanical buffing, obtain high-quality EBSD, must adopt electropolishing (being so at least at present).Sample surfaces through electropolishing is smooth, bright and clean, without deformation layer, but obtain suitable polishing fluid and technological parameter more difficult, need to carry out a large amount of tests and grope.Also have and adopt ion milling method to do final polishing, but affect the many factors of sample ions attenuated polishing quality, as, ion beam voltage, electric current, incident angle, vacuum tightness; Sample type, microstructure features, initial surface condition, thickness etc., need repeatedly to grope, and preparation time is very long in operation.
At present, electrical steel EBSD sample adopts the preparation of mechanical buffing+electrolytic polishing method mostly, and mechanical buffing is relatively simple, and electropolishing is cumbersome.First to there is special electrolysis unit; In addition, electrical steel is thinner, generally, between 0.2 ㎜～0.5 ㎜, before electropolishing, also will inlay and manage conduction sample, makes it and form closed-loop path as anode in electrolytic solution and between the negative electrode of insoluble petal composition.While having electric current to flow through when switching on power between anode and cathode, thereby the microscopic protrusions part generation selective dissolution that anode is polished sample surfaces forms smooth surface, makes sample surfaces become smooth, and final acquisition is applicable to the sample surfaces that EBSD analyzes.
Summary of the invention
The object of this invention is to provide a kind of easy, quick, cost is low, polishing effect good, polishing fluid can repeatedly use, and can replace the electrical steel EBSD sample chemical finishing method of electrolytic polishing method.
A kind of electrical steel EBSD sample chemical finishing method provided by the invention, its step is as follows:
(1) inlay: electrical steel sample is put into silica gel and inlays in mould, cold inlay liquid is poured into and inlayed in mould, after inlay sclerosis in 10 minutes, the described electrical steel EBSD sample of having inlayed can be taken out;
(2) mechanical buffing: by the described electrical steel of having inlayed 180Cw, 600Cw for sample, 1000Cw carborundum paper order water mill, finally use diamond polishing, emery granularity is less than 2.5 μ m, and described mechanical buffing and traditional metallographic sample preparation are basic identical;
(3) chemical polishing: put into chemical brightening solution 8～12 seconds after the described electrical steel sample wash after mechanical buffing is clean, carry out chemical polishing, then take out that described electrical steel sample deionized water fully rinses, ethanol dehydration dries up, polishing completes.
(4) corrosion removal product: after the polishing of described electrical steel sample completes, if electrical steel sample surfaces has corrosion product, can drip a little 1% nital, wipe corrosion product with absorbent cotton.
Described cold inlay is acryl resin inlay, also can use the cold inlay of CMR type metallographic or epoxide resin type metallic phase mounting panel.
Described chemical brightening solution is made up of oxalic acid, hydrogen peroxide, hydrofluorite.Described chemical brightening solution proportioning is: oxalic acid is 3.5-3.8g, and hydrogen peroxide is 100ml, hydrofluorite 5-7.5ml, and chemical brightening solution serviceability temperature is 25 ℃.
Described oxalic acid, hydrogen peroxide, hydrofluorite are analytical reagent.
The advantage of a kind of electrical steel EBSD sample chemical finishing method provided by the invention is: easy, quick, cost is low, polishing effect good, polishing fluid can Reusability, do not need electrolysis special polissoir.Samples met EBSD after polishing analyzes requirement.
Accompanying drawing explanation
Fig. 1 is the sample surfaces figure before chemical polishing in electrical steel EBSD sample chemical finishing method of the present invention.
Fig. 2 is the sample surfaces figure after chemical polishing in electrical steel EBSD sample chemical finishing method of the present invention.
Embodiment
The invention provides a kind of electrical steel EBSD sample chemical finishing method, its operation steps is as follows:
(1) inlay: electrical steel sample is put into silica gel and inlays in mould, cold inlay liquid is poured into and inlayed in mould, within 10 minutes, treat that inlay sclerosis can take out the electrical steel EBSD sample of having inlayed;
In the present embodiment, inlay preferred acrylic resins inlay or the cold inlay of CMR type metallographic or epoxide resin type metallic phase mounting panel.Acryl resin inlay is easy to use, without heating, pressurization, can harden rapidly at normal temperatures, and filling capacity is good, corrosion-resistant, is convenient to sample and preserves for a long time.
(2) mechanical buffing: by the described electrical steel of having inlayed 180Cw, 600Cw for sample, 1000Cw carborundum paper order water mill, finally use diamond polishing, emery granularity is less than 2.5 μ m;
In the present embodiment, mechanical buffing and traditional metallographic sample preparation are basic identical.
(3) chemical polishing: downward the electrical steel sample surfaces of rinsing well, put into chemical brightening solution 8～12 seconds, putting into the time of chemical brightening solution can suitably adjust according to environment temperature, carry out chemical polishing, after taking-up with deionized water fully rinse, ethanol dehydration dries up, the polishing of electrical steel sample completes.
In the present embodiment, chemical brightening solution is made up of oxalic acid, hydrogen peroxide, hydrofluorite.Chemical brightening solution proportioning is: oxalic acid is 3.5-3.8g, and hydrogen peroxide is 100ml, hydrofluorite 5-7.5ml.Polishing fluid serviceability temperature is advisable with 25 ℃.Oxalic acid, hydrogen peroxide, the preferred commercially available analytical reagent of hydrofluorite.
(4) corrosion removal product: after polishing completes, if electrical steel sample surfaces has corrosion product, can drip a little 1% nital, then wipe corrosion product with absorbent cotton.
Claims (4)
1. an electrical steel EBSD sample chemical finishing method, is characterized in that: its operation steps is as follows:
(1) inlay: electrical steel sample is put into silica gel and inlays in mould, cold inlay liquid is poured into and inlayed in mould, within 10 minutes, treat that inlay sclerosis can take out the electrical steel EBSD sample of having inlayed;
(2) mechanical buffing: by the described electrical steel of having inlayed 180Cw, 600Cw for sample, 1000Cw carborundum paper order water mill, finally use diamond polishing, emery granularity is less than 2.5 μ m, and described mechanical buffing and traditional metallographic sample preparation are basic identical;
(3) chemical polishing: downward the electrical steel sample surfaces of rinsing well, put into chemical brightening solution 8～12 seconds, carry out chemical polishing, after taking-up with deionized water fully rinse, ethanol dehydration dries up, the polishing of electrical steel sample completes;
(4) corrosion removal product; After the polishing of described electrical steel sample completes, if electrical steel sample surfaces has corrosion product, can drip a little 1% nital, then wipe corrosion product with absorbent cotton.
2. a kind of electrical steel EBSD sample chemical finishing method as claimed in claim 1, is characterized in that, described cold inlay is acryl resin or the cold inlay of CMR type metallographic or epoxide resin type metallic phase mounting panel.
3. a kind of electrical steel EBSD sample chemical finishing method as claimed in claim 1, it is characterized in that, described chemical brightening solution is made up of oxalic acid, hydrogen peroxide, hydrofluorite, described chemical brightening solution proportioning is: oxalic acid is 3.5-3.8g, hydrogen peroxide is 100ml, hydrofluorite 5-7.5ml, polishing fluid serviceability temperature is 25 ℃.
4. a kind of electrical steel EBSD sample chemical finishing method as claimed in claim 3, is characterized in that described oxalic acid, hydrogen peroxide, hydrofluorite Optimization Analysis pure reagent.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458374A (en) * | 2014-12-03 | 2015-03-25 | 湖南江滨机器（集团）有限责任公司 | Preparation method of aluminum-silicon alloy testing sample with low-magnification grain size |
| CN105063739A (en) * | 2015-09-19 | 2015-11-18 | 太原理工大学 | Preparation method of magnesium alloy electron back-scattered diffraction (EBSD) sample and special electrolytic polishing solution thereof |
| CN106245031A (en) * | 2016-09-06 | 2016-12-21 | 国网天津市电力公司 | A kind of chemical polishing agent being applicable to the polishing of tower material and using method |
| CN106350821A (en) * | 2016-09-06 | 2017-01-25 | 国网天津市电力公司 | Polishing agent applicable to boiler equipment and pipelines of power plants and utilization method of polishing agent |
| CN107063786A (en) * | 2016-12-06 | 2017-08-18 | 重庆大学 | A kind of preparation method of nanometer gradient structural material top layer EBSD samples |
| CN109760324A (en) * | 2019-01-09 | 2019-05-17 | 苏州大学 | Molten bath processing method based on laser transmission welding plastic |
| CN110318092A (en) * | 2019-06-27 | 2019-10-11 | 江苏省沙钢钢铁研究院有限公司 | Auxiliary device for electrolytic polishing and using method thereof |
| CN110389129A (en) * | 2019-08-01 | 2019-10-29 | 四川轻化工大学 | Corrosive agent for displaying 690 nickel-based alloy deposited metal grain boundary and etching method thereof |
| CN111487268A (en) * | 2020-04-27 | 2020-08-04 | 宁波江丰电子材料股份有限公司 | Surface treatment method for tantalum material EBSD sample |
| JP2021099273A (en) * | 2019-12-23 | 2021-07-01 | 信越半導体株式会社 | Standard sample and manufacturing method for the same, and managing method for ebsd measurement device |
| CN114088502A (en) * | 2021-10-20 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample |
| CN114184628A (en) * | 2021-12-21 | 2022-03-15 | 成都大学 | Method for rapidly preparing bulk ceramic EBSD sample |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458374A (en) * | 2014-12-03 | 2015-03-25 | 湖南江滨机器（集团）有限责任公司 | Preparation method of aluminum-silicon alloy testing sample with low-magnification grain size |
| CN105063739A (en) * | 2015-09-19 | 2015-11-18 | 太原理工大学 | Preparation method of magnesium alloy electron back-scattered diffraction (EBSD) sample and special electrolytic polishing solution thereof |
| CN106245031A (en) * | 2016-09-06 | 2016-12-21 | 国网天津市电力公司 | A kind of chemical polishing agent being applicable to the polishing of tower material and using method |
| CN106350821A (en) * | 2016-09-06 | 2017-01-25 | 国网天津市电力公司 | Polishing agent applicable to boiler equipment and pipelines of power plants and utilization method of polishing agent |
| CN107063786A (en) * | 2016-12-06 | 2017-08-18 | 重庆大学 | A kind of preparation method of nanometer gradient structural material top layer EBSD samples |
| CN109760324A (en) * | 2019-01-09 | 2019-05-17 | 苏州大学 | Molten bath processing method based on laser transmission welding plastic |
| CN109760324B (en) * | 2019-01-09 | 2021-02-09 | 苏州大学 | Molten pool treatment method based on laser transmission welding plastics |
| CN110318092A (en) * | 2019-06-27 | 2019-10-11 | 江苏省沙钢钢铁研究院有限公司 | Auxiliary device for electrolytic polishing and using method thereof |
| CN110389129B (en) * | 2019-08-01 | 2022-04-22 | 四川轻化工大学 | Corrosive agent for displaying 690 nickel-based alloy deposited metal grain boundary and etching method thereof |
| CN110389129A (en) * | 2019-08-01 | 2019-10-29 | 四川轻化工大学 | Corrosive agent for displaying 690 nickel-based alloy deposited metal grain boundary and etching method thereof |
| JP2021099273A (en) * | 2019-12-23 | 2021-07-01 | 信越半導体株式会社 | Standard sample and manufacturing method for the same, and managing method for ebsd measurement device |
| JP7188377B2 (en) | 2019-12-23 | 2022-12-13 | 信越半導体株式会社 | Standard sample and its preparation method, and management method of EBSD measuring device |
| CN111487268A (en) * | 2020-04-27 | 2020-08-04 | 宁波江丰电子材料股份有限公司 | Surface treatment method for tantalum material EBSD sample |
| CN114088502A (en) * | 2021-10-20 | 2022-02-25 | 包头钢铁（集团）有限责任公司 | Electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample |
| CN114184628A (en) * | 2021-12-21 | 2022-03-15 | 成都大学 | Method for rapidly preparing bulk ceramic EBSD sample |
| CN114184628B (en) * | 2021-12-21 | 2024-03-19 | 成都大学 | Method for rapidly preparing massive ceramic EBSD sample |
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Application publication date: 20140702 |