CN113776915B - Method for displaying microstructure of high-temperature annealed sample of oriented silicon steel - Google Patents
Method for displaying microstructure of high-temperature annealed sample of oriented silicon steel Download PDFInfo
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- CN113776915B CN113776915B CN202110760894.4A CN202110760894A CN113776915B CN 113776915 B CN113776915 B CN 113776915B CN 202110760894 A CN202110760894 A CN 202110760894A CN 113776915 B CN113776915 B CN 113776915B
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- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 239000003518 caustics Substances 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000012498 ultrapure water Substances 0.000 claims description 20
- 238000005260 corrosion Methods 0.000 claims description 15
- 230000007797 corrosion Effects 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000007796 conventional method Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005097 cold rolling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/204—Structure thereof, e.g. crystal structure
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for displaying microstructure of a high-temperature annealed sample of oriented silicon steel, which mainly comprises the following steps: sampling, preparing samples, corroding and metallographic observation; the grain boundary of the sample displayed by the method provided by the invention is clear and complete, meets the rating requirements of manual and metallographic analysis software, and provides more reliable conditions for accurately measuring the microstructure and magnetic performance analysis of the oriented silicon steel.
Description
Technical Field
The invention relates to the technical field of metallographic detection, in particular to a method for displaying microstructure of a high-temperature annealed sample of oriented silicon steel.
Background
The indexes for measuring the performance of the silicon steel are mainly the magnetic performance, namely lower iron core loss and higher magnetic induction intensity. In the production process of the oriented silicon steel, especially under the cold rolling process and the annealing process, the microstructure change of the oriented silicon steel is quite obvious, and the magnetic property of the oriented silicon steel is closely and indistinctly related with the grain, texture and recrystallization phenomenon. The deformation and recrystallization of the metal material are important physical metallurgical processes for regulating and controlling the microstructure and performance of the material. Researches on the microstructure and the structural cause and the evolution rule of different working procedures and the relation with macroscopic magnetic property in the production process of the cold rolling and annealing processes of the oriented silicon steel, and is beneficial to the quality control of the production process.
The cold rolled oriented silicon steel has extremely complex production process and longer flow, the oriented silicon steel completes secondary recrystallization after high-temperature annealing, gaussian grains engulf other grains, abnormal growth occurs, the grain size reaches the centimeter level, the sample after the high-temperature annealing of the oriented silicon steel is displayed by corrosive, the grain boundary is easily oxidized in the air and is difficult to identify, and the microstructure is extremely difficult to observe. Good etching effects are essential for studying the influence of the microstructure of oriented silicon steel on magnetic properties.
Disclosure of Invention
The invention aims to provide a method for displaying the microstructure of the high-temperature annealed sample of the oriented silicon steel, and the grain boundary of the sample displayed by the method provided by the invention is clear and complete, so that the rating requirements of manual and metallographic analysis software are met, and more reliable conditions are provided for accurately measuring the microstructure and magnetic performance analysis of the oriented silicon steel.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention discloses a method for displaying microstructure of a high-temperature annealed sample of oriented silicon steel, which comprises the following steps:
1) Sampling
And taking a sample after the cold rolled oriented silicon steel is annealed at a high temperature, and preparing a metallographic sample of the cold rolled oriented silicon steel after the cold rolled oriented silicon steel is annealed at a high temperature. The sample size was 100X 100mm;
2) Sample preparation
Carrying out simple pretreatment on the high-temperature annealed sample of the oriented silicon steel, lightly coarse grinding and fine grinding by using sand paper, grinding off a high-temperature MgO coating on the surface, and cleaning and drying by a conventional method;
3) Corrosion of the coupon
The method comprises three steps of corrosive agent composition and proportion, corrosive agent configuration and metallographic corrosion, and comprises the following specific steps:
a) The components and the proportions of the corrosive agent are as follows:
hydrochloric acid (1.19 g/mL) and high-purity water in a volume ratio of 1:1;
b) Configuration of corrosive agent:
i. heating high purity water to boil;
filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring with a glass rod;
heating and boiling on a heating device;
c) Metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
ii heating for 3min;
thirdly, clamping the sample out by forceps to observe the surface of the sample until clear crystal boundary appears;
iv, clamping a sample, removing a surface corrosive agent by using flowing high-purity water, and cleaning and drying by using 95% alcohol;
4) Metallographic observation
The grain boundary of the sample is clear and complete, and the rating requirements of manual and metallographic analysis software are met.
Compared with the prior art, the invention has the beneficial technical effects that:
the grain boundary of the sample displayed by the method provided by the invention is clear and complete, meets the rating requirements of manual and metallographic analysis software, and provides more reliable conditions for accurately analyzing the high-temperature annealing microstructure of the oriented silicon steel.
Drawings
The invention is further described with reference to the following description of the drawings.
FIG. 1 is a metallographic structure diagram of a high-temperature annealed sample of cold-rolled oriented silicon steel according to example 1 of the present invention.
FIG. 2 is a metallographic structure diagram of a high-temperature annealed sample of cold-rolled oriented silicon steel of example 2 of the present invention.
FIG. 3 is a metallographic structure diagram of a high temperature annealed sample of cold rolled oriented silicon steel according to example 3 of the present invention.
Detailed Description
The invention is further illustrated by reference to examples:
the test materials are oriented silicon steel high-temperature annealing sample components shown in the following table:
example 1
A method for displaying microstructure of a high-temperature annealed sample of oriented silicon steel comprises the following main processes: sampling, preparing samples, corroding and metallographic observation;
1) Sampling
And taking a sample after the cold rolled oriented silicon steel is annealed at a high temperature, and preparing a metallographic sample of the cold rolled oriented silicon steel after the cold rolled oriented silicon steel is annealed at a high temperature. The sample size was 100X 100mm.
2) Sample preparation
Carrying out simple pretreatment on the high-temperature annealed sample of the oriented silicon steel, lightly coarse grinding and fine grinding by using sand paper, grinding off a high-temperature MgO coating on the surface, and cleaning and drying by a conventional method;
3) Corrosion of the coupon
The method comprises three steps of corrosive agent composition and proportion, corrosive agent configuration and metallographic corrosion, and comprises the following specific steps:
a) The components and the proportions of the corrosive agent are as follows:
hydrochloric acid 200mL (1.19 g/mL), high purity water 200mL.
b) Configuration of corrosive agent:
i. heating high purity water to boil;
filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring with a glass rod;
heating and boiling on a heating device;
c) Metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
ii heating for 3min;
thirdly, clamping the sample out by forceps to observe the surface of the sample until clear crystal boundary appears;
iv, clamping a sample, removing a surface corrosive agent by using flowing high-purity water, and cleaning and drying by using 95% alcohol;
4) Metallographic observation
The grain boundary of the sample is clear and complete, and the rating requirements of manual and metallographic analysis software are met.
Example 2
A method for displaying microstructure of a high temperature annealed specimen of oriented silicon steel, comprising:
1) Sampling
And taking a sample after the cold rolled oriented silicon steel is annealed at a high temperature, and preparing a metallographic sample of the cold rolled oriented silicon steel after the cold rolled oriented silicon steel is annealed at a high temperature. The sample size was 100X 100mm.
2) Sample preparation
Carrying out simple pretreatment on the high-temperature annealed sample of the oriented silicon steel, lightly coarse grinding and fine grinding by using sand paper, grinding off a high-temperature MgO coating on the surface, and cleaning and drying by a conventional method;
3) Corrosion of the coupon
The method comprises three steps of corrosive agent composition and proportion, corrosive agent configuration and metallographic corrosion, and comprises the following specific steps:
a) The components and the proportions of the corrosive agent are as follows:
200mL of hydrochloric acid and 200mL of high-purity water.
b) Configuration of corrosive agent:
i. heating high purity water to boil;
filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring with a glass rod;
heating and boiling on a heating device;
c) Metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
ii, heating for 5min;
thirdly, clamping the sample out by forceps to observe the surface of the sample until clear crystal boundary appears;
iv, clamping a sample, removing a surface corrosive agent by using flowing high-purity water, and cleaning and drying by using 95% alcohol;
4) Metallographic observation
The grain boundary of the sample is clear and complete, and the rating requirements of manual and metallographic analysis software are met.
Example 3
A method for displaying microstructure of a high temperature annealed specimen of oriented silicon steel, comprising:
1) Sampling
And taking a sample after the cold rolled oriented silicon steel is annealed at a high temperature, and preparing a metallographic sample of the cold rolled oriented silicon steel after the cold rolled oriented silicon steel is annealed at a high temperature. The sample size was 100X 100mm.
2) Sample preparation
Carrying out simple pretreatment on the high-temperature annealed sample of the oriented silicon steel, lightly coarse grinding and fine grinding by using sand paper, grinding off a high-temperature MgO coating on the surface, and cleaning and drying by a conventional method;
3) Corrosion of the coupon
The method comprises three steps of corrosive agent composition and proportion, corrosive agent configuration and metallographic corrosion, and comprises the following specific steps:
a) The components and the proportions of the corrosive agent are as follows:
hydrochloric acid 300mL, high purity water 200mL.
b) Configuration of corrosive agent:
i. heating high purity water to boil;
filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring with a glass rod;
heating and boiling on a heating device;
c) Metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
ii heating for 3min;
thirdly, clamping the sample out by forceps to observe the surface of the sample until clear crystal boundary appears;
iv, clamping a sample, removing a surface corrosive agent by using flowing high-purity water, and cleaning and drying by using 95% alcohol;
4) Metallographic observation
The grain boundary of the sample is clear and complete, and the rating requirements of manual and metallographic analysis software are met.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (1)
1. A method for displaying microstructure of a high temperature annealed specimen of oriented silicon steel, comprising:
1) Sampling
And taking a sample after the cold rolled oriented silicon steel is annealed at a high temperature, and preparing a metallographic sample of the cold rolled oriented silicon steel after the cold rolled oriented silicon steel is annealed at a high temperature. The sample size was 100X 100mm;
2) Sample preparation
Carrying out simple pretreatment on the high-temperature annealed sample of the oriented silicon steel, lightly coarse grinding and fine grinding by using sand paper, grinding off a high-temperature MgO coating on the surface, and cleaning and drying by a conventional method;
3) Corrosion of the coupon
The method comprises three steps of corrosive agent composition and proportion, corrosive agent configuration and metallographic corrosion, and comprises the following specific steps:
a) The components and the proportions of the corrosive agent are as follows:
hydrochloric acid and high-purity water in a volume ratio of 1:1;
b) Configuration of corrosive agent:
i. heating high purity water to boil;
filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring with a glass rod;
heating and boiling on a heating device;
c) Metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
ii heating for 3min;
thirdly, clamping the sample out by forceps to observe the surface of the sample until clear crystal boundary appears;
iv, clamping a sample, removing a surface corrosive agent by using flowing high-purity water, and cleaning and drying by using 95% alcohol;
4) Metallographic observation
The grain boundary of the sample is clear and complete, and the rating requirements of manual and metallographic analysis software are met.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110760894.4A CN113776915B (en) | 2021-07-06 | 2021-07-06 | Method for displaying microstructure of high-temperature annealed sample of oriented silicon steel |
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| CN202110760894.4A CN113776915B (en) | 2021-07-06 | 2021-07-06 | Method for displaying microstructure of high-temperature annealed sample of oriented silicon steel |
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| CN113776915A CN113776915A (en) | 2021-12-10 |
| CN113776915B true CN113776915B (en) | 2024-03-08 |
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| CN114859003B (en) * | 2022-05-09 | 2023-11-28 | 包头钢铁（集团）有限责任公司 | Preparation method of sample for measuring Gaussian oriented grain deviation angle of oriented silicon steel |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942626A (en) * | 2010-09-18 | 2011-01-12 | 湘潭大学 | Silicon steel-containing hot dipped zinc alloy |
| WO2014078977A1 (en) * | 2012-11-26 | 2014-05-30 | 宝山钢铁股份有限公司 | Oriented silicon steel and method for manufacturing same |
| CN107843592A (en) * | 2017-10-11 | 2018-03-27 | 河钢股份有限公司 | A kind of austenitic stainless steel weld joint tissue corrosive agent and its application method |
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- 2021-07-06 CN CN202110760894.4A patent/CN113776915B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942626A (en) * | 2010-09-18 | 2011-01-12 | 湘潭大学 | Silicon steel-containing hot dipped zinc alloy |
| WO2014078977A1 (en) * | 2012-11-26 | 2014-05-30 | 宝山钢铁股份有限公司 | Oriented silicon steel and method for manufacturing same |
| CN107843592A (en) * | 2017-10-11 | 2018-03-27 | 河钢股份有限公司 | A kind of austenitic stainless steel weld joint tissue corrosive agent and its application method |
Non-Patent Citations (1)
| Title |
|---|
| 无取向硅钢晶粒与晶界特征的EBSD分析;贾涓;朱微微;代礼斌;宋新莉;袁泽喜;;武汉科技大学学报;20091015(05);全文 * |
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