CN114088502A - Electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample - Google Patents
Electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample Download PDFInfo
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- CN114088502A CN114088502A CN202111220995.9A CN202111220995A CN114088502A CN 114088502 A CN114088502 A CN 114088502A CN 202111220995 A CN202111220995 A CN 202111220995A CN 114088502 A CN114088502 A CN 114088502A
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- 238000005498 polishing Methods 0.000 title claims abstract description 63
- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract description 32
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 12
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 11
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 56
- 239000003792 electrolyte Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- KFSUNTUMPUWCMW-UHFFFAOYSA-N ethanol;perchloric acid Chemical compound CCO.OCl(=O)(=O)=O KFSUNTUMPUWCMW-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000007943 implant Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 description 9
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses an electrolytic polishing sample preparation method for a sample for cold-rolled oriented silicon steel EBSD, which comprises the following steps: s1, mechanical polishing, namely cutting 10 mm-10 mm specification samples, cleaning the samples by using an ultrasonic instrument, pre-grinding the samples on sand paper with different particle sizes, and polishing the samples on a metallographic sample polishing machine to a mirror surface; s2, performing electrolytic polishing, namely performing electrolytic polishing on the mechanically polished sample by using a strulerselectropol-5 type electrolytic polishing machine; and S3, detecting the EBSD. The method mainly solves the problem of how to obtain high-quality EBSD detection technical samples under the technical conditions of the existing equipment, is suitable for preparing large-batch EBSD samples of cold-rolled oriented silicon steel, and has the advantages of simple and quick experimental process after the method is used, and the experimental time and the cost are saved.
Description
Technical Field
The invention relates to the technical field of sample preparation and detection, in particular to an electrolytic polishing sample preparation method for a sample for cold-rolled oriented silicon steel EBSD.
Background
For researchers in material science, it has become an important hotspot in the field of material science research to analyze and research the micro-crystallography structure of materials by using an EBSD analysis testing technology and improve the material performance through grain boundary control and design. However, all applications are based on obtaining high quality EBSD results, and thus the preparation of high quality EBSD samples is a prerequisite for obtaining high quality EBSD results.
At present, the preparation methods of samples for EBSD analysis include mechanical polishing, chemical polishing, electrolytic polishing, ion thinning and the like. The ion thinning method is expensive and not suitable for processing steel samples in large scale. The mechanical polishing method is simple, but the mechanical polishing alone cannot effectively remove the deformation layer of the processed surface and cannot obtain the Kikuchi diffraction pattern. The chemical polishing has no ideal effect on steel materials. The method of electrolytic corrosion after mechanical polishing is a method with simple, rapid and low-cost operation for steel materials.
However, the requirements of the high-quality EBSD sample on the parameters of the electrolytic polishing sample preparation process of the steel materials with different carbon contents and chemical compositions are very different, and especially for low-carbon steel materials, the success or failure of the electrolytic polishing method is closely related to the electrolyte and the polishing parameters (polishing time, voltage, electrolyte flow rate, temperature and the like). Based on the current situation, an electrolytic polishing sample preparation method for preparing a cold-rolled oriented silicon steel EBSD sample is provided.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide an electrolytic polishing sample preparation method for samples for cold-rolled oriented silicon steel EBSD, mainly solving the problem of how to obtain high-quality EBSD detection technical samples under the technical conditions of the existing equipment, being suitable for preparing large-batch EBSD samples of cold-rolled oriented silicon steel, and being simple and rapid in experimental process after the method is used, and saving experimental time and cost.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to an electrolytic polishing sample preparation method for a sample for cold-rolled oriented silicon steel EBSD, which comprises the following steps:
s1, mechanical polishing, namely cutting 10 mm-10 mm specification samples, cleaning the samples by using an ultrasonic instrument, pre-grinding the samples on sand paper with different particle sizes, and polishing the samples on a metallographic sample polishing machine to a mirror surface;
s2, performing electrolytic polishing, namely performing electrolytic polishing on the mechanically polished sample by using a strulerselectropol-5 type electrolytic polishing machine;
s2.1, preparing two matching containers with the specification of 500ml, adding 500ml of deionized water into one matching container, adding 500ml of 5% perchloric acid ethanol electrolyte into the other matching container, and placing the container added with the deionized water into a container groove of an electrolytic polishing machine;
s2.2, opening an equipment switch, entering an operation main interface, and starting a program to clean a polishing device in contact with the electrolyte after selecting a changeelectrolyte interface in a manufuntations interface;
s2.3, after the cleaning procedure is finished, replacing the container with a 5% perchloric acid ethanol electrolyte container, and putting a sample mold with the aperture of 1cm2 on a sample table;
s2.4 choose the usermethods interface to implant a blank interface for programming: selecting a polishing corrosion program, wherein the polishing area is 1cm2, the electrolyte temperature is 22 ℃, the voltage is 40V, the flow speed is 17, and the program is stored after the polishing time is 20S;
s2.5, starting a preset program, quickly taking out the sample by using a sample clamp after the electrolytic polishing is finished, and washing and drying the sample by using an absolute ethyl alcohol solution;
s3, EBSD detection, namely adhering the prepared sample on a 70-degree sample table by using a conductive adhesive, putting the sample table into a scanning electron microscope, vacuumizing to 5 × 10-9mpa, starting high voltage, and selecting HDBSD signal debugging equipment parameters until clear sample morphology is observed;
and (3) closing the high pressure, inserting the EBSD probe, opening the high pressure debugging EBSD parameter after the probe is inserted, collecting the appearance of the detection area of the sample, and clicking any micro area of the sample in the detection area to observe a high-quality Juchi pattern image.
Compared with the prior art, the invention has the beneficial technical effects that:
the sample preparation method for selecting steel materials with different chemical components influences the quality of the EBSD sample, the implementation of the method effectively solves the difference, the sample preparation method suitable for the EBSD detection of the cold-rolled oriented silicon steel is found, the polishing damage caused in the traditional mechanical polishing process can be observed to be removed, the surface is smooth, the EBSD pattern image with higher quality is obtained, the working efficiency is improved, and the experimental cost for purchasing electrolytes with different components is saved.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is a high-quality Kikuchi flower pattern image observed in any micro-area of a sample.
Detailed Description
The following description of the embodiments of the present invention is made with reference to the drawings:
electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample
Firstly, mechanical polishing, namely cutting 10mm by 10mm specification samples, cleaning the samples by using an ultrasonic instrument, pre-grinding the samples on sand paper with different particle sizes, and polishing the samples on a metallographic sample polishing machine to a mirror surface;
step two, electrolytic polishing, namely performing electrolytic polishing on the mechanically polished sample by using a Struers optropol-5 type electrolytic polishing machine;
firstly, preparing two matching containers with the specification of 500ml, adding 500ml of deionized water into one matching container, adding 500ml of 5% perchloric acid ethanol electrolyte into the other matching container, and placing the container added with the deionized water into a container tank of an electrolytic polishing machine;
further, opening an equipment switch, entering an operation main interface, selecting a change electrolyte interface in the manual fuels interface, and starting a program to clean polishing device devices such as an anode arm, a stirring coil and the like which are in contact with the electrolyte;
further, after the cleaning procedure is finished, the container is replaced by a 5% perchloric acid ethanol electrolyte container, and a sample mold with the aperture of 1cm2 is placed on a sample table;
further, a blank interface is implanted into the user methods interface for programming: selecting a polishing corrosion program, wherein the polishing area is 1cm2, the electrolyte temperature is 22 ℃, the voltage is 40V, the flow speed is 17, and the program is stored after the polishing time is 20S;
further, starting a preset program, quickly taking out the sample by using a sample clamp after the electrolytic polishing is finished, and washing and drying the sample by using an absolute ethyl alcohol solution;
thirdly, performing EBSD detection, namely adhering the prepared sample on a 70-degree sample table by using a conductive adhesive, putting the sample table into a scanning electron microscope, vacuumizing to 5 × 10-9mpa, starting high voltage, and selecting HDBSD signal debugging equipment parameters until clear sample morphology is observed;
further, the EBSD probe is inserted after the high pressure is closed, the high pressure debugging EBSD parameters are started after the probe is inserted, the appearance of the detection area of the sample is collected, and the high-quality Juchi pattern image can be observed by clicking any micro area of the sample in the detection area.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (1)
1. An electrolytic polishing sample preparation method for a sample for cold-rolled oriented silicon steel EBSD is characterized by comprising the following steps:
s1, mechanical polishing, namely cutting 10 mm-10 mm specification samples, cleaning the samples by using an ultrasonic instrument, pre-grinding the samples on sand paper with different particle sizes, and polishing the samples on a metallographic sample polishing machine to a mirror surface;
s2, performing electrolytic polishing, namely performing electrolytic polishing on the mechanically polished sample by using a strulerselectropol-5 type electrolytic polishing machine;
s2.1, preparing two matching containers with the specification of 500ml, adding 500ml of deionized water into one matching container, adding 500ml of 5% perchloric acid ethanol electrolyte into the other matching container, and placing the container added with the deionized water into a container groove of an electrolytic polishing machine;
s2.2, opening an equipment switch, entering an operation main interface, and starting a program to clean a polishing device in contact with the electrolyte after selecting a changeelectrolyte interface in a manufuntations interface;
s2.3, after the cleaning procedure is finished, replacing the container with a 5% perchloric acid ethanol electrolyte container, and putting a sample mold with the aperture of 1cm2 on a sample table;
s2.4 choose the usermethods interface to implant a blank interface for programming: selecting a polishing corrosion program, wherein the polishing area is 1cm2, the electrolyte temperature is 22 ℃, the voltage is 40V, the flow speed is 17, and the program is stored after the polishing time is 20S;
s2.5, starting a preset program, quickly taking out the sample by using a sample clamp after the electrolytic polishing is finished, and washing and drying the sample by using an absolute ethyl alcohol solution;
s3, EBSD detection, namely adhering the prepared sample on a 70-degree sample table by using a conductive adhesive, putting the sample table into a scanning electron microscope, vacuumizing to 5 × 10-9mpa, starting high voltage, and selecting HDBSD signal debugging equipment parameters until clear sample morphology is observed;
and (3) closing the high pressure, inserting the EBSD probe, opening the high pressure debugging EBSD parameter after the probe is inserted, collecting the appearance of the detection area of the sample, and clicking any micro area of the sample in the detection area to observe a high-quality Juchi pattern image.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111220995.9A CN114088502A (en) | 2021-10-20 | 2021-10-20 | Electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample |
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| CN202111220995.9A CN114088502A (en) | 2021-10-20 | 2021-10-20 | Electrolytic polishing sample preparation method for cold-rolled oriented silicon steel EBSD sample |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117233188A (en) * | 2023-11-08 | 2023-12-15 | 包头市威丰稀土电磁材料股份有限公司 | Preparation method of silicon steel EBSD large-size spliced sample |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051666A (en) * | 2010-12-20 | 2011-05-11 | 北京工业大学 | Electrolytic polishing method for EBSD analysis of cold-rolled NiW alloy baseband |
| CN103900889A (en) * | 2014-03-21 | 2014-07-02 | 李岩 | Chemical polishing method for electrical silicon steel EBSD (electron back-scattered diffraction) sample |
| WO2020019400A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Preparation method for iron-based alloy powder ebsd test sample |
| CN112858357A (en) * | 2021-02-04 | 2021-05-28 | 包头钢铁（集团）有限责任公司 | Sample preparation method for oriented silicon steel micro-texture EBSD sample |
-
2021
- 2021-10-20 CN CN202111220995.9A patent/CN114088502A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051666A (en) * | 2010-12-20 | 2011-05-11 | 北京工业大学 | Electrolytic polishing method for EBSD analysis of cold-rolled NiW alloy baseband |
| CN103900889A (en) * | 2014-03-21 | 2014-07-02 | 李岩 | Chemical polishing method for electrical silicon steel EBSD (electron back-scattered diffraction) sample |
| WO2020019400A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Preparation method for iron-based alloy powder ebsd test sample |
| CN112858357A (en) * | 2021-02-04 | 2021-05-28 | 包头钢铁（集团）有限责任公司 | Sample preparation method for oriented silicon steel micro-texture EBSD sample |
Non-Patent Citations (1)
| Title |
|---|
| 王春芳;王毛球;: "钢铁材料EBSD样品电解抛光制备方法", 物理测试, no. 06, 15 November 2011 (2011-11-15) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117233188A (en) * | 2023-11-08 | 2023-12-15 | 包头市威丰稀土电磁材料股份有限公司 | Preparation method of silicon steel EBSD large-size spliced sample |
| CN117233188B (en) * | 2023-11-08 | 2024-01-30 | 包头市威丰稀土电磁材料股份有限公司 | Preparation method of silicon steel EBSD large-size spliced sample |
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