CN112858357A - Sample preparation method for oriented silicon steel micro-texture EBSD sample - Google Patents
Sample preparation method for oriented silicon steel micro-texture EBSD sample Download PDFInfo
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- CN112858357A CN112858357A CN202110166669.8A CN202110166669A CN112858357A CN 112858357 A CN112858357 A CN 112858357A CN 202110166669 A CN202110166669 A CN 202110166669A CN 112858357 A CN112858357 A CN 112858357A
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- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 50
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 10
- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract 6
- 238000005498 polishing Methods 0.000 claims abstract description 68
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 31
- 238000000227 grinding Methods 0.000 claims abstract description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005070 sampling Methods 0.000 claims abstract description 9
- 238000000861 blow drying Methods 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000007796 conventional method Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 6
- 239000010432 diamond Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 7
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000007517 polishing process Methods 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a sample preparation method of an EBSD sample with an oriented silicon steel micro-texture, which comprises the following steps: 1) sampling, namely, adopting a linear cutting machine to machine an oriented silicon steel sample; 2) preparing a sample, namely inlaying an oriented silicon steel sample by using a hot inlaying machine, and performing coarse grinding, fine grinding, polishing, cleaning and blow-drying according to a conventional method; carrying out primary polishing treatment on the sample by adopting 240-mesh, 400-mesh, 600-mesh, 800-mesh, 1000-mesh and 2000-mesh alumina sand paper in sequence; polishing the sample by using a 5.0um high-efficiency diamond polishing agent; 3) and (4) performing electrolytic polishing, namely performing electrolytic polishing on the oriented silicon steel sample after mechanical polishing.
Description
Technical Field
The invention relates to the technical field of metal material detection, in particular to a sample preparation method for an EBSD sample with an oriented silicon steel micro texture.
Background
Oriented silicon steel belongs to ferrite steel, is an important soft magnetic material applied to the manufacture of transformer cores, and is widely applied to the electronic and electric power industry. The market has been increasingly demanding in recent years, and its quality is also increasingly demanding. The high-quality oriented silicon steel is mainly characterized by excellent magnetic performance, in particular to two performance parameters of iron loss and magnetic induction intensity. Therefore, the ability to produce oriented silicon steels with lower core loss and higher magnetic induction is a hot spot of interest to the industry.
In the production process of the oriented silicon steel, particularly in the rolling process and the annealing process, the microstructure of the oriented silicon steel is obviously changed and has characteristics, and the magnetic performance of the oriented silicon steel is closely and inseparably related to the phenomena of grains, textures and recrystallization. Therefore, the microstructure of the oriented silicon steel has important significance.
Disclosure of Invention
The invention aims to provide a sample preparation method for an oriented silicon steel micro-texture EBSD sample, the surface cleanliness of the oriented silicon steel EBSD sample prepared by the method provided by the invention meets the requirement of Electron Back Scattering Diffraction (EBSD) on the sample, and more reliable conditions are provided for accurately measuring the oriented silicon steel micro-texture.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a sample preparation method of an EBSD sample with an oriented silicon steel micro texture, which comprises the following steps:
1) sampling
Adopting a linear cutting machine to machine an oriented silicon steel sample;
2) sample preparation
Inlaying an oriented silicon steel sample by using a hot inlaying machine, and performing coarse grinding, fine grinding, polishing, cleaning and blow-drying according to a conventional method;
carrying out primary polishing treatment on the sample by adopting 240-mesh aluminum oxide sand paper;
carrying out secondary polishing treatment on the sample by using 400-mesh alumina sand paper;
carrying out third polishing treatment on the sample by using 600-mesh alumina sand paper;
carrying out fourth grinding treatment on the sample by adopting 800-mesh aluminum oxide sand paper;
carrying out fifth polishing treatment on the sample by adopting 1000-mesh alumina sand paper;
carrying out sixth grinding treatment on the sample by adopting 2000-mesh alumina sand paper;
polishing the sample by using a 5.0um high-efficiency diamond polishing agent;
3) electrolytic polishing
And performing electrolytic polishing after the oriented silicon steel sample is mechanically polished.
Further, the sample size was 8mm × 10mm (roll direction).
Further, the electrolytic solution used in the electrolytic polishing process is a 10% perchloric acid alcohol solution, the electrolytic polishing voltage is 15-18V, and the electrolytic time is 20-60 s.
Further, after polishing, the polished wafer is immediately washed by clean water, then washed by alcohol and dried.
Compared with the prior art, the invention has the beneficial technical effects that:
the surface cleanliness of the oriented silicon steel EBSD sample prepared by the method provided by the invention meets the requirements of Electron Back Scattering Diffraction (EBSD) on the sample, and more reliable conditions are provided for accurately measuring the microscopic texture of the oriented silicon steel.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1(a) is the EBSD microtexture of oriented silicon steel of example 1;
FIG. 1(b) shows the EBSD microtexture of the oriented silicon steel of example 2;
fig. 1(c) shows the EBSD microtexture of the oriented silicon steel of example 3 of the present invention.
Detailed Description
Example 1
The invention provides a sample preparation method of an EBSD sample with an oriented silicon steel micro texture, which comprises the following main processes: sampling → sample preparation → electrolytic polishing → scanning electron microscope EBSD analysis;
1) sampling
The silicon steel sample is oriented by adopting a linear cutting machine, and the size of the sample is 8mm multiplied by 10mm (rolling direction).
2) Sample preparation
And inlaying the oriented silicon steel sample by using a hot inlaying machine, and performing coarse grinding, fine grinding, polishing, cleaning and blow-drying according to a conventional method.
a) Carrying out primary polishing treatment on the sample by adopting 240-mesh aluminum oxide sand paper;
b) carrying out secondary polishing treatment on the sample by using 400-mesh alumina sand paper;
c) carrying out third polishing treatment on the sample by using 600-mesh alumina sand paper;
d) carrying out fourth grinding treatment on the sample by adopting 800-mesh aluminum oxide sand paper;
e) carrying out fifth polishing treatment on the sample by adopting 1000-mesh alumina sand paper;
f) carrying out sixth grinding treatment on the sample by adopting 2000-mesh alumina sand paper;
g) and polishing the sample by using a 5.0um high-efficiency diamond polishing agent.
3) Electrolytic polishing
The mechanical polishing of the oriented silicon steel sample is carried out and then electrolytic polishing is carried out.
a) The electrolytic solution is 10% perchloric acid alcohol solution;
b) the electrolytic polishing voltage is 15V;
c) the electrolysis time is 20S;
d) and immediately washing with clear water after polishing, then washing with alcohol, and drying. And detecting the texture of the oriented silicon steel sample by an electron back scattering diffraction device (EBSD) of a scanning electron microscope accessory. As shown in fig. 1 (a).
Example 2
The invention provides a sample preparation method of an EBSD sample with an oriented silicon steel micro texture, which comprises the following main processes: sampling → sample preparation → electrolytic polishing → scanning electron microscope EBSD analysis;
1) sampling
The silicon steel sample is oriented by adopting a linear cutting machine, and the size of the sample is 8mm multiplied by 10mm (rolling direction).
2) Sample preparation
And inlaying the oriented silicon steel sample by using a hot inlaying machine, and performing coarse grinding, fine grinding, polishing, cleaning and blow-drying according to a conventional method.
h) Carrying out primary polishing treatment on the sample by adopting 240-mesh aluminum oxide sand paper;
i) carrying out secondary polishing treatment on the sample by using 400-mesh alumina sand paper;
j) carrying out third polishing treatment on the sample by using 600-mesh alumina sand paper;
k) carrying out fourth grinding treatment on the sample by adopting 800-mesh aluminum oxide sand paper;
l) carrying out fifth grinding treatment on the test sample by adopting 1000-mesh aluminum oxide sand paper;
m) carrying out sixth grinding treatment on the sample by adopting 2000-mesh alumina sand paper;
and n) adopting a 5.0um high-efficiency diamond polishing agent to polish the sample.
3) Electrolytic polishing
The mechanical polishing of the oriented silicon steel sample is carried out and then electrolytic polishing is carried out.
e) The electrolytic solution is 10% perchloric acid alcohol solution;
f) the electrolytic polishing voltage is 15V;
g) the electrolysis time is 40S;
h) and immediately washing with clear water after polishing, then washing with alcohol, and drying. And detecting the texture of the oriented silicon steel sample by an electron back scattering diffraction device (EBSD) of a scanning electron microscope accessory. As shown in fig. 1 (b).
Example 3
The invention provides a sample preparation method of an EBSD sample with an oriented silicon steel micro texture, which comprises the following main processes: sampling → sample preparation → electrolytic polishing → scanning electron microscope EBSD analysis;
1) sampling
The silicon steel sample is oriented by adopting a linear cutting machine, and the size of the sample is 8mm multiplied by 10mm (rolling direction).
2) Sample preparation
And inlaying the oriented silicon steel sample by using a hot inlaying machine, and performing coarse grinding, fine grinding, polishing, cleaning and blow-drying according to a conventional method.
o) carrying out first polishing treatment on the sample by adopting 240-mesh aluminum oxide sand paper;
p) carrying out secondary polishing treatment on the sample by adopting 400-mesh alumina sand paper;
q) carrying out third polishing treatment on the sample by adopting 600-mesh alumina sand paper;
r) carrying out fourth grinding treatment on the sample by adopting 800-mesh aluminum oxide sand paper;
s) carrying out fifth grinding treatment on the sample by adopting 1000-mesh aluminum oxide sand paper;
t) carrying out sixth grinding treatment on the sample by adopting 2000-mesh alumina sand paper;
u) polishing the sample by using a 5.0um high-efficiency diamond polishing agent.
3) Electrolytic polishing
The mechanical polishing of the oriented silicon steel sample is carried out and then electrolytic polishing is carried out.
i) The electrolytic solution is 10% perchloric acid alcohol solution;
j) the electrolytic polishing voltage is 18V;
k) the electrolysis time is 60S;
l) rinsing with clear water immediately after polishing, rinsing with alcohol, and blow-drying. And detecting the texture of the oriented silicon steel sample by an electron back scattering diffraction device (EBSD) of a scanning electron microscope accessory. As shown in fig. 1 (c).
The change of the micro texture of the oriented silicon steel can influence the type of the macro texture and the magnetic performance of the final oriented silicon steel, and the internal structure and the characteristics of the material can be better analyzed only by analyzing and researching the characteristics, components and evolution process of the micro texture. The Electron Back Scattering Diffraction (EBSD) technique is a commonly used research method for characterizing material texture at present, and its principle is that electron beams are excited on the surface of an inclined sample in a scanning electron microscope to form diffraction patterns, so as to determine the grain orientation, the grain boundary type, and the like. Through EBSD analysis, the internal structure of the material can be further understood, so that different properties of the material can be inferred. EBSD can not only observe the size, shape and distribution of crystal grains, but also measure the proportion and distribution of various oriented crystal grains in a sample, determine orientation differences among different phases or different crystal grains in the sample, analyze different types of grain boundaries and properties thereof, and is very important for analyzing microtexture.
The EBSD sample preparation requirement of the micro texture of the oriented silicon steel is strict, the EBSD can be used for observing the directly polished surface, but the quality of the diffraction pattern can be improved by electrolytic polishing under most conditions. The control of the voltage and the electrolysis time during the electrolytic polishing is very critical to obtain the ideal polishing effect.
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 (4)
1. A sample preparation method for an EBSD sample with an oriented silicon steel microtexture is characterized by comprising the following steps:
1) sampling
Adopting a linear cutting machine to machine an oriented silicon steel sample;
2) sample preparation
Inlaying an oriented silicon steel sample by using a hot inlaying machine, and performing coarse grinding, fine grinding, polishing, cleaning and blow-drying according to a conventional method;
carrying out primary polishing treatment on the sample by adopting 240-mesh aluminum oxide sand paper;
carrying out secondary polishing treatment on the sample by using 400-mesh alumina sand paper;
carrying out third polishing treatment on the sample by using 600-mesh alumina sand paper;
carrying out fourth grinding treatment on the sample by adopting 800-mesh aluminum oxide sand paper;
carrying out fifth polishing treatment on the sample by adopting 1000-mesh alumina sand paper;
carrying out sixth grinding treatment on the sample by adopting 2000-mesh alumina sand paper;
polishing the sample by using a 5.0um high-efficiency diamond polishing agent;
3) electrolytic polishing
And performing electrolytic polishing after the oriented silicon steel sample is mechanically polished.
2. The method for preparing the EBSD sample with the oriented silicon steel micro-texture as claimed in claim 1, wherein the sample size is 8mm x 10 mm.
3. The method for preparing the EBSD sample with the oriented silicon steel microtexture as claimed in claim 1, wherein the electrolytic solution used in the electrolytic polishing process is a 10% perchloric acid alcohol solution, the electrolytic polishing voltage is 15-18V, and the electrolytic time is 20-60 s.
4. The method for preparing the EBSD sample with the oriented silicon steel microtexture as claimed in claim 1 or 3, wherein the sample is immediately washed by clean water, then washed by alcohol and dried by blowing after polishing.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN114235864A (en) * | 2021-11-11 | 2022-03-25 | 泛锐云智科技(郑州)有限公司 | Preparation method of bismuth alloy sample for EBSD test |
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CN106813966A (en) * | 2015-12-01 | 2017-06-09 | 上海梅山钢铁股份有限公司 | A kind of EBSD analysis preparation method of low-carbon (LC) steel sample |
CN110618150A (en) * | 2019-10-11 | 2019-12-27 | 马鞍山钢铁股份有限公司 | Preparation method of silicon steel EBSD sample |
CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
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- 2021-02-04 CN CN202110166669.8A patent/CN112858357A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106813966A (en) * | 2015-12-01 | 2017-06-09 | 上海梅山钢铁股份有限公司 | A kind of EBSD analysis preparation method of low-carbon (LC) steel sample |
CN110618150A (en) * | 2019-10-11 | 2019-12-27 | 马鞍山钢铁股份有限公司 | Preparation method of silicon steel EBSD sample |
CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN114235864A (en) * | 2021-11-11 | 2022-03-25 | 泛锐云智科技(郑州)有限公司 | Preparation method of bismuth alloy sample for EBSD test |
CN114235864B (en) * | 2021-11-11 | 2024-05-10 | 泛锐云智科技(郑州)有限公司 | Preparation method of bismuth alloy sample for EBSD test |
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