CN113029778A - Method for rapidly judging grain diameter of primary recrystallization of oriented silicon steel - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000001953 recrystallisation Methods 0.000 title claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 20
- 239000010959 steel Substances 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
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- 238000003698 laser cutting Methods 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/005—Heat treatment of ferrous alloys containing Mn
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- C21D6/00—Heat treatment of ferrous alloys
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- 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
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- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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Abstract
The invention relates to the technical field of oriented silicon steel manufacturing, and discloses a method for quickly judging the diameter of primary recrystallized grains of oriented silicon steel, which comprises the following steps: selecting hot-rolled incoming oriented silicon steel, producing, taking a plurality of tensile samples from the same part of the produced steel plate, processing, stretching and analyzing to obtain yield strength, continuously preparing metallographic samples on two sides of the part of the tensile sample, calculating the average grain diameter D of the corresponding tensile sample, carrying out statistical analysis on performance data and the average grain diameter to establish the corresponding relation between the yield strength and the grain diameter, taking a judgment sample from the produced steel plate during actual production to obtain the yield strength of the judgment sample, and further obtaining the grain diameter of the judgment sample. The method for rapidly judging the diameter of the primary recrystallized grain of the oriented silicon steel indirectly indicates the size of the primary grain through mechanical property inspection, and has the advantages of high detection speed and more accurate evaluation.
Description
Technical Field
The invention relates to the technical field of oriented silicon steel manufacturing, in particular to a method for quickly judging the diameter of primary recrystallized grains of oriented silicon steel.
Background
The control of the primary grain diameter is one of the core technologies for controlling the magnetic performance of the oriented silicon steel, and is the key point of the control of each process. From the beginning of steel making, Al, N, Mn, S and other favorable inclusions are added into steel to form AlN, MnS and other inhibitors, and in the subsequent process, the inhibitors are distributed in a dispersed manner in an effort to achieve the purpose of inhibiting the growth of crystal grains.
The decarburization annealing process is the most critical process for forming primary grains with proper size on the oriented silicon steel. The primary crystal grains are fine and uniform, the secondary recrystallization is complete in development, the Gaussian texture orientation is accurate, and the magnetism is excellent. In the manufacturing process, the size and distribution of the inhibitor are controlled through hot rolling and normalizing, the cold rolling reduction rate is controlled through the thickness of a hot rolled plate, and the control of the primary grain diameter is the most central content in the production and manufacturing of the oriented silicon steel through the heating rate, soaking temperature and time of decarburization and annealing. In recent years, with the development of the low-temperature high-magnetic-induction oriented silicon steel technology, the electromagnetic induction rapid heating technology and the nitriding technology are mature day by day, and the control of primary crystal grains is more accurate. In the decarburization annealing step, the desired target primary crystal grain size is obtained by finely dividing the chemical composition and specifically adopting different heat treatment systems, thereby increasing the overall magnetic properties.
However, the evaluation of the primary crystal grain diameter is a difficulty in the improvement of the process manufacturing process. In general, a technician samples a steel sheet after decarburization annealing and performs metallographic examination to determine the size of primary crystal grains. However, since the sample is too microscopic, the field of view of the microscope is too small, and the grain rating is poorly representative, often not as expected from actual process adjustments. Therefore, to accurately evaluate the size of the primary crystal grains, a large number of samples are required for metallographic analysis, which takes a long time and is poor in guidance on the field process, so that the process improvement time is infinitely prolonged. Subsequently, the skilled person installed an on-line iron loss meter at the exit side of the continuous decarburization annealing line and desired to determine the grain size from the iron loss tendency. However, in practice, since the range of the size variation of the primary crystal grains is small (from 18um to 35um), the subtle variation of the grain diameter is hardly reflected on the iron loss curve.
In addition, the manufacturing period of the oriented silicon steel is long, and at least about 10 days are required from the primary recrystallization annealing to the magnetic inspection of a finished product, which brings great risk to the adjustment of the process. That is, when the magnetic property is found to deteriorate, the decarburization annealing line is produced for at least 10 days, which results in a large loss of quality for the enterprise.
Disclosure of Invention
Aiming at the defects of the technology, the invention provides a method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel, which indirectly indicates the size of the primary grains through mechanical property inspection, and has the advantages of high detection speed and more accurate evaluation.
In order to achieve the purpose, the method for quickly judging the primary recrystallized grain diameter of the oriented silicon steel comprises the following steps of:
A) selecting hot-rolled incoming oriented silicon steel;
B) adjusting and controlling the conditions of the primary recrystallization annealing process of the oriented silicon steel for production;
C) respectively taking a plurality of tensile samples from the same part of the steel plate produced in the step B), and processing, stretching and analyzing the tensile samples to obtain the yield strength of the tensile samples;
D) continuously preparing metallographic samples on two sides of each tensile sample part on the steel plate, carrying out metallographic observation photographing, grading and grain size calculation, and calculating the average grain diameter of the corresponding tensile sample;
E) carrying out statistical analysis on the yield strength of the tensile sample obtained in the step C) and the average grain diameter of the corresponding tensile sample obtained in the step D), and establishing a corresponding relation between the yield strength and the grain diameter;
F) in actual production, a judgment sample is taken from the produced steel plate, the judgment sample is subjected to processing stretching and analysis to obtain the yield strength of the judgment sample, and the grain diameter of the judgment sample is obtained by combining the corresponding relation between the yield strength and the grain diameter obtained in the step E).
Preferably, in the step E), the corresponding relationship between the yield strength and the grain diameter satisfies the formula σs＝σ0+K*D-1/2Wherein σ issIs the yield strength, σ, of the tensile specimen0The coefficient of resistance to intragranular deformation, K the coefficient of influence of grain boundaries on strength, and D the grain size.
Preferably, in the step C), the tensile samples are sampled at the beginning and the end of the coil after decarburization annealing, and the tensile samples are respectively sampled in the longitudinal direction, the transverse direction and the 45 ° direction at the side, the middle and the side of the sampled steel sheet, so that the difference of the size, the shape and the like of the crystal grains in the length direction and the width direction of the whole coil due to the influence of the processes such as cold rolling reduction, primary recrystallization annealing and the like is avoided.
Preferably, in the step C), the tensile sample is prepared into a sample specified in GB/T228.1-2010 by using a milling machine or a laser cutting processing means.
Preferably, in the step D), at least 10 standard fields are respectively selected from two sides of the metallographic specimen along the testing direction of each tensile specimen, and at least two schemes are combined for grading.
Preferably, the rating scheme includes an area method and a cut-point method.
Preferably, in the step A), the hot-rolled incoming oriented silicon steel material comprises the following components in percentage by weight: 0.03-0.07% of carbon, 0.0004-0.001% of nitrogen, 3.0-3.5% of silicon, 0.05-0.15% of manganese, 0.005-0.01% of sulfur and 0.02-0.04% of aluminum.
Compared with the prior art, the invention has the following advantages:
1. the detection speed is high, the metallographic grading needs a long time, each sample needs at least 4 hours from sample preparation to grading, one sample cannot be accurately evaluated, at least more than 20 samples are needed according to general requirements, the average value is obtained after each sample is graded, the time of at least several days is needed, the strength detection only needs 10 minutes from sample preparation to result, and the process adjustment can be guided immediately;
2. the evaluation is more accurate, each steel plate is sampled and detected at different positions, the average grain size change of the strip steel along the width and length directions of the steel plate can be reflected, and the average grain diameter of the whole steel plate can be more intuitively reflected compared with a metallographic sample due to the large area of the sample;
3. the method can be used as process control index management to control the manufacturing process, and the mechanical property detection is a conventional inspection project of a cold-rolled sheet finished product, so that the detection of the intermediate process of the oriented silicon steel is very convenient and fast, the method can be brought into daily monitoring management to ensure the stability of the magnetic property of the oriented silicon steel.
Drawings
FIG. 1 is a schematic diagram showing the relationship between yield (rolling direction) and finished product magnetism of oriented silicon steel in one embodiment of the method for rapidly judging the primary recrystallized grain diameter of oriented silicon steel of the present invention;
FIG. 2 is a schematic diagram showing the relationship between yield (transverse direction) of oriented silicon steel and magnetic properties of a finished product in one embodiment of the method for rapidly judging the primary recrystallized grain diameter of oriented silicon steel.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments.
A method for rapidly judging the diameter of primary recrystallized grains of oriented silicon steel comprises the following steps:
A) selecting hot-rolled incoming oriented silicon steel;
B) adjusting and controlling the conditions of the primary recrystallization annealing process of the oriented silicon steel for production;
C) respectively taking a plurality of tensile samples from the same part of the steel plate produced in the step B), processing, stretching and analyzing the tensile samples to obtain the yield strength of the tensile samples, wherein the tensile samples are uniformly sampled at the head and the tail of the coil after decarburization and annealing, respectively taking longitudinal, transverse and 45-degree direction tensile samples from the side, middle and edge parts of the taken steel plate, and preparing the tensile samples into samples specified in GB/T228.1-2010 by adopting a milling machine or a laser cutting processing means;
D) continuously preparing metallographic samples on two sides of each tensile sample part on a steel plate, carrying out metallographic observation photographing, rating and grain size calculation, and calculating the average grain diameter of the corresponding tensile sample, wherein at least 10 standard view fields are respectively selected on the metallographic samples along two sides of each tensile sample in the testing direction, and at least two schemes are combined for rating;
E) carrying out statistical analysis on the yield strength of the tensile sample obtained in the step C) and the average grain diameter of the corresponding tensile sample obtained in the step D), establishing a corresponding relation between the yield strength and the grain diameter, wherein the corresponding relation between the yield strength and the grain diameter meets a formula sigmas＝σ0+K*D-1/2Wherein σ issIs the yield strength, σ, of the tensile specimen0Is the resistance coefficient of intragranular deformation, K is the influence coefficient of grain boundary on strength, D is the grain diameter;
F) in actual production, a judgment sample is taken from the produced steel plate, the judgment sample is subjected to processing stretching and analysis to obtain the yield strength of the judgment sample, and the grain diameter of the judgment sample is obtained by combining the corresponding relation between the yield strength and the grain diameter obtained in the step E).
In the embodiment, the low-temperature high-grade oriented silicon steel with the specification of 0.285mm is selected for testing and data tracking, and the hot-rolled incoming oriented silicon steel has the following component content ranges: 0.03-0.07% of carbon, 0.0004-0.001% of nitrogen, 3.0-3.5% of silicon, 0.05-0.15% of manganese, 0.005-0.01% of sulfur and 0.02-0.04% of aluminum. The corresponding relation between the yield strength and the grain diameter in the longitudinal tensile test can be obtained, wherein sigma0The value range is 350-390 MPa, and the K value range is 14-22 MPa-1/2。
As the magnetic data is related to the grain diameter, as shown in figures 1 and 2, the corresponding relation between the yield strength and finished product magnetism in the longitudinal tensile test can be obtained, the yield (rolling direction) of 0.285mm specification is 420MPa-495MPa, the yield (transverse direction) is 435MPa-520MPa, the magnetic induction strength is high and stable, the iron loss is low and stable, and the optimal range of the grain diameter is 20-30 um. Therefore, the grain diameter can be quickly judged by the yield strength, and the optimal magnetism can be obtained.
The method for rapidly judging the diameter of the primary recrystallized grain of the oriented silicon steel has the advantages of high detection speed and more accurate evaluation, can be used as process control index management, can timely guide a unit to adjust the production process, and avoids the occurrence of mass quality accidents.
Claims (7)
1. A method for rapidly judging the diameter of primary recrystallized grains of oriented silicon steel is characterized by comprising the following steps: the method comprises the following steps:
A) selecting hot-rolled incoming oriented silicon steel;
B) adjusting and controlling the conditions of the primary recrystallization annealing process of the oriented silicon steel for production;
C) respectively taking a plurality of tensile samples from the same part of the steel plate produced in the step B), and processing, stretching and analyzing the tensile samples to obtain the yield strength of the tensile samples;
D) continuously preparing metallographic samples on two sides of each tensile sample part on the steel plate, carrying out metallographic observation photographing, grading and grain size calculation, and calculating the average grain diameter of the corresponding tensile sample;
E) carrying out statistical analysis on the yield strength of the tensile sample obtained in the step C) and the average grain diameter of the corresponding tensile sample obtained in the step D), and establishing a corresponding relation between the yield strength and the grain diameter;
F) in actual production, a judgment sample is taken from the produced steel plate, the judgment sample is subjected to processing stretching and analysis to obtain the yield strength of the judgment sample, and the grain diameter of the judgment sample is obtained by combining the corresponding relation between the yield strength and the grain diameter obtained in the step E).
2. The method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel as set forth in claim 1, wherein: in the step E), the corresponding relation between the yield strength and the grain diameter meets the formula sigmas＝σ0+K*D-1/2Wherein σ issIs the yield strength, σ, of the tensile specimen0The coefficient of resistance to intragranular deformation, K the coefficient of influence of grain boundaries on strength, and D the grain size.
3. The method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel as set forth in claim 1, wherein: and in the step C), the tensile samples are uniformly sampled at the head and the tail of the coil after decarburization and annealing, and the tensile samples in the longitudinal direction, the transverse direction and the 45-degree direction are respectively taken at the edge, the middle part and the edge of the taken steel plate.
4. The method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel as set forth in claim 1, wherein: in the step C), the tensile sample is prepared into a sample specified in GB/T228.1-2010 by adopting a milling machine or a laser cutting processing means.
5. The method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel as set forth in claim 1, wherein: and in the step D), at least 10 standard view fields are respectively selected from two sides of the metallographic specimen along the testing direction of each tensile specimen, and at least two schemes are combined for grading.
6. The method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel as set forth in claim 5, wherein: the rating scheme includes an area method and an intercept method.
7. The method for rapidly judging the primary recrystallized grain diameter of the oriented silicon steel as set forth in claim 1, wherein: in the step A), the hot-rolled incoming oriented silicon steel material comprises the following components in percentage by weight: 0.03-0.07% of carbon, 0.0004-0.001% of nitrogen, 3.0-3.5% of silicon, 0.05-0.15% of manganese, 0.005-0.01% of sulfur and 0.02-0.04% of aluminum.
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| CN114383983A (en) * | 2021-12-02 | 2022-04-22 | 湖北亿纬动力有限公司 | Method for measuring particle size of primary particles of positive electrode material |
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