CN113776915A - Method for displaying microstructure of oriented silicon steel high-temperature annealing sample - Google Patents
Method for displaying microstructure of oriented silicon steel high-temperature annealing sample Download PDFInfo
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- CN113776915A CN113776915A CN202110760894.4A CN202110760894A CN113776915A CN 113776915 A CN113776915 A CN 113776915A CN 202110760894 A CN202110760894 A CN 202110760894A CN 113776915 A CN113776915 A CN 113776915A
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- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 41
- 238000000137 annealing Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005260 corrosion Methods 0.000 claims abstract description 17
- 230000007797 corrosion Effects 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 239000003518 caustics Substances 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000012498 ultrapure water Substances 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000009835 boiling Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 238000000861 blow drying 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
- 238000001035 drying Methods 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
- 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
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 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
- 238000005272 metallurgy 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
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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
- 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
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- 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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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a method for displaying the microstructure of an oriented silicon steel high-temperature annealing sample, which mainly comprises the following steps: sampling → sample preparation → corrosion → metallographic observation; the grain boundary of the sample displayed by the method provided by the invention is clear and complete, meets the grading requirements of manual and metallographic analysis software, and provides more reliable conditions for accurately measuring the oriented silicon steel microstructure and analyzing the magnetic performance.
Description
Technical Field
The invention relates to the technical field of metallographic detection, in particular to a method for displaying a microstructure of an oriented silicon steel high-temperature annealing sample.
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, particularly in the cold rolling process and the annealing process, the microstructure of the oriented silicon steel is changed obviously, and the magnetic performance of the oriented silicon steel is closely and inseparably related to the grain, texture and recrystallization phenomena. The deformation and recrystallization of the metal material are important physical metallurgy processes for regulating and controlling the microstructure and the performance of the material. The research on the microstructure, the cause and the evolution law of the texture and the relation with the macroscopic magnetic property of different process sections in the production process of the cold rolling and annealing processes of the oriented silicon steel is helpful for the quality control of the production process.
The production process of the cold-rolled oriented silicon steel is very complicated and has a long flow, the oriented silicon steel completes secondary recrystallization after high-temperature annealing, Gaussian grains engulf other grains and grow abnormally, the grain size reaches centimeter level, a sample after the high-temperature annealing of the oriented silicon steel is displayed by a corrosive agent, the sample is very easy to oxidize in the air and is difficult to identify grain boundaries, and the observation of a microstructure is very difficult. Good etching effect is essential for studying and calculating the influence of the microstructure of the oriented silicon steel on the magnetic performance.
Disclosure of Invention
The invention aims to provide a method for displaying the microstructure of an oriented silicon steel high-temperature annealing sample, the grain boundary of the sample displayed by the method provided by the invention is clear and complete, the grading requirements of manual and metallographic analysis software are met, and more reliable conditions are provided for accurately measuring the microstructure of the oriented silicon steel and analyzing the magnetic performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention discloses a method for displaying the microstructure of an oriented silicon steel high-temperature annealing sample, which comprises the following steps:
1) sampling
And (3) taking the sample of the cold-rolled oriented silicon steel after high-temperature annealing, and preparing the metallographic sample of the cold-rolled oriented silicon steel after high-temperature annealing. The sample size is 100X 100 mm;
2) sample preparation
Carrying out simple pretreatment on the oriented silicon steel high-temperature annealing sample, slightly and coarsely grinding and finely grinding by using sand paper, grinding off the high-temperature MgO coating on the surface, cleaning and drying by using a conventional method;
3) corrosion of the test specimen
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 corrosive comprises the following components in parts by weight:
hydrochloric acid (1.19g/mL) and high-purity water in a volume ratio of 1: 1;
b) preparation of the corrosive agent:
i. heating and boiling high-purity water;
ii, filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring the mixture by using a glass rod;
boiling on a heating device;
c) and metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
heating for 3 min;
using forceps to clamp the sample and observing the surface of the sample until a clear crystal boundary appears;
taking out the sample, removing the surface corrosive agent by using flowing high-purity water, and cleaning and blow-drying by using 95% alcohol;
4) metallographic observation
The grain boundary of the sample is clear and complete, and the grading 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 grading 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 illustrated in the following description with reference to the drawings.
Fig. 1 is a metallographic structure diagram of a cold-rolled oriented silicon steel high-temperature annealed specimen according to example 1 of the present invention.
Fig. 2 is a metallographic structure diagram of a cold-rolled oriented silicon steel high-temperature annealed specimen according to example 2 of the present invention.
Fig. 3 is a metallographic structure diagram of a cold-rolled oriented silicon steel high-temperature annealed specimen according to example 3 of the present invention.
Detailed Description
The invention is further illustrated with reference to the following examples:
the components of the test material, which is an oriented silicon steel high-temperature annealing sample, are shown in the following table:
example 1
A method for displaying the microstructure of an oriented silicon steel high-temperature annealing sample comprises the following main processes: sampling → sample preparation → corrosion → metallographic observation;
1) sampling
And (3) taking the sample of the cold-rolled oriented silicon steel after high-temperature annealing, and preparing the metallographic sample of the cold-rolled oriented silicon steel after high-temperature annealing. The specimen size was 100X 100 mm.
2) Sample preparation
Carrying out simple pretreatment on the oriented silicon steel high-temperature annealing sample, slightly and coarsely grinding and finely grinding by using sand paper, grinding off the high-temperature MgO coating on the surface, cleaning and drying by using a conventional method;
3) corrosion of the test specimen
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 corrosive comprises the following components in parts by weight:
hydrochloric acid (200 mL, 1.19g/mL) and high purity water (200 mL).
b) Preparation of the corrosive agent:
i. heating and boiling high-purity water;
ii, filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring the mixture by using a glass rod;
boiling on a heating device;
c) and metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
heating for 3 min;
using forceps to clamp the sample and observing the surface of the sample until a clear crystal boundary appears;
taking out the sample, removing the surface corrosive agent by using flowing high-purity water, and cleaning and blow-drying by using 95% alcohol;
4) metallographic observation
The grain boundary of the sample is clear and complete, and the grading requirements of manual and metallographic analysis software are met.
Example 2
A method for displaying the microstructure of a high-temperature annealing sample of oriented silicon steel, comprising the following steps of:
1) sampling
And (3) taking the sample of the cold-rolled oriented silicon steel after high-temperature annealing, and preparing the metallographic sample of the cold-rolled oriented silicon steel after high-temperature annealing. The specimen size was 100X 100 mm.
2) Sample preparation
Carrying out simple pretreatment on the oriented silicon steel high-temperature annealing sample, slightly and coarsely grinding and finely grinding by using sand paper, grinding off the high-temperature MgO coating on the surface, cleaning and drying by using a conventional method;
3) corrosion of the test specimen
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 corrosive comprises the following components in parts by weight:
200mL of hydrochloric acid and 200mL of high purity water.
b) Preparation of the corrosive agent:
i. heating and boiling high-purity water;
ii, filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring the mixture by using a glass rod;
boiling on a heating device;
c) and metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
heating for 5 min;
using forceps to clamp the sample and observing the surface of the sample until a clear crystal boundary appears;
taking out the sample, removing the surface corrosive agent by using flowing high-purity water, and cleaning and blow-drying by using 95% alcohol;
4) metallographic observation
The grain boundary of the sample is clear and complete, and the grading requirements of manual and metallographic analysis software are met.
Example 3
A method for displaying the microstructure of a high-temperature annealing sample of oriented silicon steel, comprising the following steps of:
1) sampling
And (3) taking the sample of the cold-rolled oriented silicon steel after high-temperature annealing, and preparing the metallographic sample of the cold-rolled oriented silicon steel after high-temperature annealing. The specimen size was 100X 100 mm.
2) Sample preparation
Carrying out simple pretreatment on the oriented silicon steel high-temperature annealing sample, slightly and coarsely grinding and finely grinding by using sand paper, grinding off the high-temperature MgO coating on the surface, cleaning and drying by using a conventional method;
3) corrosion of the test specimen
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 corrosive comprises the following components in parts by weight:
300mL of hydrochloric acid and 200mL of high-purity water.
b) Preparation of the corrosive agent:
i. heating and boiling high-purity water;
ii, filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring the mixture by using a glass rod;
boiling on a heating device;
c) and metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
heating for 3 min;
using forceps to clamp the sample and observing the surface of the sample until a clear crystal boundary appears;
taking out the sample, removing the surface corrosive agent by using flowing high-purity water, and cleaning and blow-drying by using 95% alcohol;
4) metallographic observation
The grain boundary of the sample is clear and complete, and the grading requirements of manual and metallographic analysis software are met.
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. A method for displaying the microstructure of a high-temperature annealing sample of oriented silicon steel is characterized by comprising the following steps:
1) sampling
And (3) taking the sample of the cold-rolled oriented silicon steel after high-temperature annealing, and preparing the metallographic sample of the cold-rolled oriented silicon steel after high-temperature annealing. The sample size is 100X 100 mm;
2) sample preparation
Carrying out simple pretreatment on the oriented silicon steel high-temperature annealing sample, slightly and coarsely grinding and finely grinding by using sand paper, grinding off the high-temperature MgO coating on the surface, cleaning and drying by using a conventional method;
3) corrosion of the test specimen
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 corrosive comprises the following components in parts by weight:
hydrochloric acid and high-purity water in a volume ratio of 1: 1;
b) preparation of the corrosive agent:
i. heating and boiling high-purity water;
ii, filling high-purity water into a beaker, adding hydrochloric acid into the water, and uniformly stirring the mixture by using a glass rod;
boiling on a heating device;
c) and metallographic corrosion:
i. completely soaking the ground high-temperature annealing sample in corrosive liquid;
heating for 3 min;
using forceps to clamp the sample and observing the surface of the sample until a clear crystal boundary appears;
taking out the sample, removing the surface corrosive agent by using flowing high-purity water, and cleaning and blow-drying by using 95% alcohol;
4) metallographic observation
The grain boundary of the sample is clear and complete, and the grading requirements of manual and metallographic analysis software are met.
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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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| CN113776915B CN113776915B (en) | 2024-03-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114859003A (en) * | 2022-05-09 | 2022-08-05 | 包头钢铁（集团）有限责任公司 | Preparation method of sample for measuring deviation angle of Gauss-oriented grains 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
- 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 |
|---|
| 贾涓;朱微微;代礼斌;宋新莉;袁泽喜;: "无取向硅钢晶粒与晶界特征的EBSD分析", 武汉科技大学学报, no. 05, 15 October 2009 (2009-10-15) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114859003A (en) * | 2022-05-09 | 2022-08-05 | 包头钢铁（集团）有限责任公司 | Preparation method of sample for measuring deviation angle of Gauss-oriented grains of oriented silicon steel |
| 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 |
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