CN116559224A - Method for testing primary recrystallization temperature of oriented silicon steel - Google Patents
Method for testing primary recrystallization temperature of oriented silicon steel Download PDFInfo
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- CN116559224A CN116559224A CN202310441348.3A CN202310441348A CN116559224A CN 116559224 A CN116559224 A CN 116559224A CN 202310441348 A CN202310441348 A CN 202310441348A CN 116559224 A CN116559224 A CN 116559224A
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- 238000001953 recrystallisation Methods 0.000 title claims abstract description 80
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000012360 testing method Methods 0.000 title claims abstract description 33
- 238000000137 annealing Methods 0.000 claims abstract description 29
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 230000008859 change Effects 0.000 claims abstract description 9
- 238000005261 decarburization Methods 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 5
- 238000010008 shearing Methods 0.000 claims abstract description 5
- 230000007704 transition Effects 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 238000005097 cold rolling Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000003518 caustics Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000010998 test method Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010959 steel Substances 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
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
- G01N25/147—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation by cristallisation
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D11/00—Process control or regulation for heat treatments
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
- C21D8/1233—Cold rolling
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1272—Final recrystallisation annealing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
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Abstract
The invention discloses a method for testing the primary recrystallization temperature of oriented silicon steel, which comprises the following steps: 1) Sampling and shearing a sample; 2) Primary recrystallization temperature test, the primary recrystallization temperature test parameters are shown in the following table 1, and the primary recrystallization annealing heat preservation time is set to 6min; 3) Performing microscopic tissue analysis; 4) Hardness analysis; 5) The primary recrystallization process is selected to finally determine the primary recrystallization transition temperature of the oriented silicon steel sample through hardness change curve and microscopic structure observation, and the primary recrystallization annealing process of the oriented silicon steel is formulated, and the oriented silicon steel is produced in a continuous decarburization annealing production line of a cold-rolled silicon steel plant. The invention aims to provide a method for testing the primary recrystallization temperature of oriented silicon steel, which provides theoretical basis and empirical data for formulating the primary recrystallization annealing process and industrial production trial production of oriented silicon steel.
Description
Technical Field
The invention relates to the field of metallurgical materials, in particular to a method for testing the primary recrystallization temperature of oriented silicon steel.
Background
The carbon content of the oriented silicon steel hot rolled steel strip is about 0.025% -0.040%, the thickness is thinned to 0.63mm by primary cold rolling, then the primary recrystallization is completed by decarburization annealing in a continuous furnace, and the carbon content after the decarburization annealing is controlled below 0.003%. The primary recrystallization annealing is an important link in the production flow of the oriented silicon steel and is a key point for the performance of the oriented silicon steel product.
The primary recrystallization annealing of the oriented silicon steel is to make a sufficient number of {110} <001> primary recrystallized grains in the matrix as nuclei for secondary recrystallization and to form a structure and primary recrystallized texture favorable for the growth of the primary recrystallized grains. Primary recrystallization is a process that provides gaussian nuclei for secondary recrystallization. The successful progress of the secondary recrystallization requires two conditions: on the one hand, a proper environment (including inhibitor distribution, heating speed, annealing atmosphere and the like) is provided during high-temperature annealing, so that Gaussian grains are selectively grown; on the other hand, the primary recrystallization structure can provide Gaussian crystal nuclei with accurate orientation and large quantity. Therefore, the quality of primary recrystallization directly determines whether perfect secondary recrystallization can be developed.
Factors influencing microstructure and texture of the oriented silicon steel after primary recrystallization annealing are relatively wide, such as components of the oriented silicon steel, rolling process, rolling reduction rate of cold rolling process and the like, have relatively large influence on the type and component content of the primary recrystallization texture formed after decarburization annealing of the oriented silicon steel. The proper primary recrystallization annealing process is selected and is important to obtain the excellent magnetic performance of the oriented silicon steel product.
Disclosure of Invention
The invention aims to provide a method for testing the primary recrystallization temperature of oriented silicon steel, which is convenient for obtaining the primary recrystallization temperature of oriented silicon steel, so that a matrix has a sufficient number of {110} <001> primary recrystallized grains as crystal nuclei for secondary recrystallization, and forms a structure and a primary recrystallization texture which are favorable for the growth of the primary recrystallized grains.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention discloses a method for testing the primary recrystallization temperature of oriented silicon steel, which comprises the following steps:
1) Sampling and sample shearing
The thickness of the hot rolled raw material of the oriented silicon steel is 2.6mm, and the oriented silicon steel is subjected to primary cold rolling after pickling until the thickness is 0.63mm; taking a sample after primary cold rolling from a cold rolling production plant of oriented silicon steel; the test oriented silicon steel sheet had dimensions of 65mm long by 25mm wide by 0.63mm thick;
2) Primary recrystallization temperature test
The test parameters of the primary recrystallization temperature test are shown in the following table 1, and the primary recrystallization annealing heat preservation time is set to 6min;
3) Microscopic tissue analysis
Preparing a metallographic specimen, corroding the surface of the specimen by adopting a nitrate alcohol corrosive agent after standard grinding and polishing, observing the microstructure of the specimen by utilizing a metallographic microscope, and observing the change of the microstructure of the oriented silicon steel specimen at different temperatures;
4) Hardness analysis
Detecting the hardness of the annealed sample according to a recrystallization temperature test method, and drawing a curve of the hardness of the oriented silicon steel along with the recrystallization experimental temperature;
5) Primary recrystallization process selection
Finally determining the primary recrystallization transition temperature of the oriented silicon steel sample through the hardness change curve and microscopic structure observation, formulating the primary recrystallization annealing process of the oriented silicon steel, and testing the production of the oriented silicon steel in a continuous decarburization annealing production line of a cold-rolled silicon steel plant.
Further, the chemical composition C of the oriented silicon steel raw material is as follows: 0.030 to 0.040 percent, si:3.00 to 3.20 percent, mn:0.20 to 0.23 percent, P: 0.009-0.014%, S:0.010 to 0.013%, al s:0.012 to 0.023 percent, and the balance of Fe and unavoidable impurities.
Further, the thickness of the sample after one cold rolling of the oriented silicon steel is 0.63mm, the width is 30mm, and the length is 300mm.
Compared with the prior art, the invention has the beneficial technical effects that:
the invention provides a method for testing the primary recrystallization temperature of oriented silicon steel, which provides theoretical basis and empirical data for formulating an annealing process of primary recrystallization of oriented silicon steel and industrial production trial production.
Drawings
The invention is further described with reference to the following description of the drawings.
FIG. 1 is a microstructure of example 1;
FIG. 2 is a microstructure of comparative example 1.
Detailed Description
The invention is further illustrated by the following examples:
chemical composition C of oriented silicon steel raw materials: 0.030 to 0.040 percent, si:3.00 to 3.20 percent, mn:0.20 to 0.23 percent, P: 0.009-0.014%, S:0.010 to 0.013%, al s:0.012 to 0.023 percent, and the balance of Fe and unavoidable impurities. The thickness of the primary cold rolling sample of the oriented silicon steel is 0.63mm, the width is 30mm, and the length is 300mm.
Example 1
The invention provides a method for testing the primary recrystallization temperature of oriented silicon steel, which comprises the following process parameters and steps:
1) Sampling and sample shearing
The thickness of the hot rolled raw material of the oriented silicon steel is 2.6mm, and the hot rolled raw material is subjected to primary cold rolling to a thickness of 0.63mm after pickling. And taking a cold-rolled sample from a cold rolling production plant of the oriented silicon steel. The test oriented silicon steel sheet had dimensions of 65mm long by 25mm wide by 0.63mm thick.
2) Primary recrystallization temperature test
If the primary recrystallization temperature is set to be low when the primary recrystallization temperature is set, the primary recrystallization annealing process of the oriented silicon steel is not completely recrystallized, and the inhibitor can be disabled due to the excessively high setting. The primary recrystallization temperature test parameters are shown in table 2. The initial recrystallization annealing incubation time was set to 6 min.
TABLE 2 recrystallization temperature Experimental heating temperature parameters
3) Microscopic tissue analysis
Preparing a metallographic specimen, corroding the surface of the specimen by adopting a nitrate alcohol corrosive agent after standard grinding and polishing, observing the microstructure of the specimen by utilizing a metallographic microscope, and observing the change of the microstructure of the oriented silicon steel specimen at different temperatures.
4) Hardness analysis
And detecting the hardness of the annealed sample according to a recrystallization temperature test method, and drawing a curve of the hardness of the oriented silicon steel along with the recrystallization experimental temperature.
5) Primary recrystallization process selection
Finally determining the primary recrystallization transition temperature of the oriented silicon steel sample through the hardness change curve and microscopic structure observation, formulating the primary recrystallization annealing process of the oriented silicon steel, and testing the production of the oriented silicon steel in a continuous decarburization annealing production line of a cold-rolled silicon steel plant.
Example 2
The invention provides a method for testing the primary recrystallization temperature of oriented silicon steel, which comprises the following process parameters and steps:
1) Sampling and sample shearing
The thickness of the hot rolled raw material of the oriented silicon steel is 2.6mm, and the hot rolled raw material is subjected to primary cold rolling to a thickness of 0.63mm after pickling. And taking a cold-rolled sample from a cold rolling production plant of the oriented silicon steel. The test oriented silicon steel sheet had dimensions of 65mm long by 25mm wide by 0.63mm thick.
2) Primary recrystallization temperature test
If the primary recrystallization temperature is set to be low when the primary recrystallization temperature is set, the primary recrystallization annealing process of the oriented silicon steel is not completely recrystallized, and the inhibitor can be disabled due to the excessively high setting. The primary recrystallization temperature test parameters are shown in table 3. The initial recrystallization annealing incubation time was set at 5 min.
TABLE 3 recrystallization temperature Experimental heating temperature parameters
3) Microscopic tissue analysis
Preparing a metallographic specimen, corroding the surface of the specimen by adopting a nitrate alcohol corrosive agent after standard grinding and polishing, observing the microstructure of the specimen by utilizing a metallographic microscope, and observing the change of the microstructure of the oriented silicon steel specimen at different temperatures.
4) Hardness analysis
And detecting the hardness of the annealed sample according to a recrystallization temperature test method, and drawing a curve of the hardness of the oriented silicon steel along with the recrystallization experimental temperature.
5) Primary recrystallization process selection
Finally determining the primary recrystallization transition temperature of the oriented silicon steel sample through the hardness change curve and microscopic structure observation, formulating the primary recrystallization annealing process of the oriented silicon steel, and testing the production of the oriented silicon steel in a continuous decarburization annealing production line of a cold-rolled silicon steel plant.
As can be seen by comparing fig. 1 and fig. 2: under the condition that the experimental heating temperature of the recrystallization temperature is the same, when the primary recrystallization annealing heat preservation time is 6mi < n >, the primary recrystallization process is more sufficient, the proportion of the completely recrystallized grains is increased, and the size is more uniform.
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 (3)
1. A method for testing the primary recrystallization temperature of oriented silicon steel is characterized by comprising the following steps: comprising the following steps:
1) Sampling and sample shearing
The thickness of the hot rolled raw material of the oriented silicon steel is 2.6mm, and the oriented silicon steel is subjected to primary cold rolling after pickling until the thickness is 0.63mm; taking a sample after primary cold rolling from a cold rolling production plant of oriented silicon steel; the test oriented silicon steel sheet had dimensions of 65mm long by 25mm wide by 0.63mm thick;
2) Primary recrystallization temperature test
The test parameters of the primary recrystallization temperature test are shown in the following table 1, and the primary recrystallization annealing heat preservation time is set to 6min;
3) Microscopic tissue analysis
Preparing a metallographic specimen, corroding the surface of the specimen by adopting a nitrate alcohol corrosive agent after standard grinding and polishing, observing the microstructure of the specimen by utilizing a metallographic microscope, and observing the change of the microstructure of the oriented silicon steel specimen at different temperatures;
4) Hardness analysis
Detecting the hardness of the annealed sample according to a recrystallization temperature test method, and drawing a curve of the hardness of the oriented silicon steel along with the recrystallization experimental temperature;
5) Primary recrystallization process selection
Finally determining the primary recrystallization transition temperature of the oriented silicon steel sample through the hardness change curve and microscopic structure observation, formulating the primary recrystallization annealing process of the oriented silicon steel, and testing the production of the oriented silicon steel in a continuous decarburization annealing production line of a cold-rolled silicon steel plant.
2. The method for testing the primary recrystallization temperature of oriented silicon steel according to claim 1, wherein: chemical composition C of oriented silicon steel raw materials: 0.030 to 0.040 percent, si:3.00 to 3.20 percent, mn:0.20 to 0.23 percent, P: 0.009-0.014%, S:0.010 to 0.013%, als:0.012 to 0.023 percent, and the balance of Fe and unavoidable impurities.
3. The method for testing the primary recrystallization temperature of oriented silicon steel according to claim 1, wherein: the thickness of the sample after the primary cold rolling of the oriented silicon steel is 0.63mm, the width is 30mm, and the length is 300mm.
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| CN202310441348.3A CN116559224A (en) | 2023-04-23 | 2023-04-23 | Method for testing primary recrystallization temperature of oriented silicon steel |
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| CN202310441348.3A CN116559224A (en) | 2023-04-23 | 2023-04-23 | Method for testing primary recrystallization temperature of oriented silicon steel |
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