WO2015096430A1 - 一种取向高硅电工钢的制备方法 - Google Patents
一种取向高硅电工钢的制备方法 Download PDFInfo
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- WO2015096430A1 WO2015096430A1 PCT/CN2014/080681 CN2014080681W WO2015096430A1 WO 2015096430 A1 WO2015096430 A1 WO 2015096430A1 CN 2014080681 W CN2014080681 W CN 2014080681W WO 2015096430 A1 WO2015096430 A1 WO 2015096430A1
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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
- C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
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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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
- C21D8/1255—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment with diffusion of elements, e.g. decarburising, nitriding
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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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
- 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
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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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
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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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
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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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
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
Definitions
- the invention belongs to the technical field of metallurgy, and in particular relates to a preparation method of oriented high silicon electrical steel.
- Electrical steel is the main core material of power electronic equipment. As the silicon content increases, the magnetic permeability of electrical steel increases, and the electrical conductivity And the magnetostriction coefficient is decreased, so the silicon content is 4.0 to 7.0% by weight of the high silicon electrical steel compared to the ordinary electrical steel (Si ⁇ 3.5%) has low iron loss and low noise; but subject to the intrinsic hard brittleness of high silicon electrical steel, currently only JFE in Japan
- the steel company realized mass production by chemical vapor deposition (Japan Publication No. JP63227717A, JP63069915A) Patent).
- Electrical steel has magnetic anisotropy, so it has a strong ⁇ ( ⁇ 001>//RD, RD is rolling direction) texture of oriented electrical steel along the rolling Oriented electrical steel having a magnetic property significantly higher than that of non-oriented electrical steel; oriented electrical steel having a silicon content of less than 3.5% by weight is usually divided into two Class: Ordinary Oriented Electrical Steel (CGO) and High Magnetic Sense Oriented Electrical Steel (Hi-B).
- CGO Ordinary Oriented Electrical Steel
- Hi-B High Magnetic Sense Oriented Electrical Steel
- the manufacturing technology of oriented high-silicon electrical steel (the weight percentage of silicon is 4.0-7.0%) is only the Japanese steel producer. It has been reported that it is not available in China; in Japanese Patent No. 4-80321, the scheme of using AlN second phase particles as the main inhibitor is adopted.
- the acid-soluble aluminum is controlled in the range of 0.012 to 0.048% to obtain oriented high-silicon electrical steel; however, the high-silicon electrical steel is brittle, in order to To ensure continuous forming and high yield, from the beginning of smelting to the final finish annealing, each process needs to consider formability Demand, if we consider the control requirements of the inhibitor, the range of process parameters in the production process will be extremely narrow and unfavorable.
- the slab needs to be heated above 1300 ° C to solidify the nascent MnS into the matrix;
- the high silicon content in the steel leads to a decrease in the melting point, and the high-silicon electrical steel slab heated by the high temperature above 1300 ° C is prone to cracking during hot rolling.
- the yield is significantly reduced.
- the slab still needs to be 1200 °C Long-term heating around.
- the silicon steel solution must face the conflict between the fine control of the inhibitor behavior and the fine control of the forming process, and the steel plate is added.
- the inhibitors such as S and N, which are unfavorable to magnetic properties, form elements, which must be removed by a high temperature purification annealing process, and the high temperature Purification annealing is usually carried out in pure hydrogen at 1200 ° C for a long time, and the energy consumption is large and the efficiency is low.
- the present invention provides a method for preparing an oriented high-silicon electrical steel without using various second phase particles such as AlN, MnS, Cu 2 S as an inhibitor.
- second phase particles such as AlN, MnS, Cu 2 S as an inhibitor.
- the preparation method of the oriented high silicon electrical steel of the present invention is carried out as follows:
- the slab is heated to 1000 ⁇ 1200 ° C heat treatment, the time is 5 ⁇ 600min; then hot rolling, rolling temperature 900 ⁇ 1180°C, finishing rolling temperature 750 ⁇ 1000°C, hot rolling reduction rate 50 ⁇ 99%, obtaining hot rolled steel sheet;
- the hot-rolled steel sheet is processed to 0.10 to 0.50 mm to obtain a thin steel sheet; when the rolling method is performed twice, the first time is warm cold rolling and rolling The temperature is from room temperature to 700 ° C, the reduction rate is 40 to 95%, the second time is cold rolling, the rolling temperature is from room temperature to 400 ° C, and the reduction ratio 50 to 92%; when more than two rolling methods are carried out, except for the last rolling, the other rolling is warm cold rolling, rolling temperature From room temperature to 700 ° C, the reduction rate is 40 to 95%, the last time is cold rolling, the rolling temperature is room temperature to 400 ° C, and the reduction ratio is 50 to 92%;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of decarburization annealing is 750-900 ° C, and the time is 0.5 to 60 min; after decarburization annealing, the steel sheet is fed into a heating furnace in an inert atmosphere, a reducing atmosphere or an inert reduction mixed atmosphere. Under the conditions, the temperature is heated to 1000-1200 ° C at a rate of 5 to 70 ° C / h, and the secondary recrystallization annealing is completed to obtain an oriented high silicon electrician. steel.
- the above-mentioned hot-rolled steel sheet is subjected to a normalization treatment before or after the pickling to remove the surface oxide layer, and the temperature is normalized.
- the degree is 800 to 1200 ° C
- the time is 1 to 600 min, and then cooled to room temperature to 100 ° C.
- the above intermediate annealing refers to intermediate annealing between adjacent two rollings, and the annealing temperature is 700 to 1100 ° C for a period of time. 0.5 to 600 min.
- the above inert atmosphere means a nitrogen atmosphere or an argon atmosphere.
- the above reducing atmosphere means a hydrogen atmosphere.
- the above-mentioned inert reduction mixed atmosphere means a mixed atmosphere of an inert gas and hydrogen gas, and the mixing ratio is an arbitrary ratio.
- C can refine the primary recrystallized grain size of high-silicon electrical steel and promote the occurrence of secondary recrystallization. Meanwhile, C is the right Elements with harmful magnetic properties must be removed by decarburization annealing before final annealing. More than 0.3%, decarburization is very difficult. Therefore, the C content in the raw material is controlled between 0.05 and 0.3%;
- Si is an effective element to increase the resistivity and thus reduce the eddy current loss and even the total iron loss, so it is close to the ordinary electrical steel. 4.0% of the high silicon content is used as the lower limit; on the other hand, if the silicon content exceeds 7.0%, the coercive force is increased and the saturation magnetic induction is strong. Degree and maximum permeability decrease, while processability deteriorates significantly;
- Mn is an essential element to improve the hot rolling performance, but the content exceeds 1.0%, affecting the cold workability;
- N and S are elements harmful to magnetic properties in high-silicon electrical steel, so control N ⁇ 0.01%, S ⁇ 0.02%.
- composition of the steel sheet may further contain one or more of the following components: P, Sn, Sb, Cu, Mo, Ni;
- P, Sn, Sb, Cu, Mo, Ni The proper addition of the upper element can refine the primary recrystallized grain size and promote secondary recrystallization.
- the annealing of the steel sheet of the invention is mainly composed of decarburization annealing and secondary recrystallization annealing, and may or may not include a high temperature purification annealing process to obtain oriented high silicon electrical steel, which means that AlN, MnS, Cu 2 are not used in the whole preparation process.
- Various second phase particles such as S are used as inhibitors; the main advantages of the method of the present invention are: (1) avoiding low efficiency of the heating furnace caused by high temperature heating of the slab, serious oxidation of the slab, low yield, and high energy consumption. (2) avoiding the addition of inhibitors such as AlN and MnS second phase particles, increasing the strength of the oriented high-silicon electrical steel and reducing the plastic toughness, thereby causing an additional processing problem.
- the invention is a production process based on a rolling manufacturing process and equipment of a non-oriented high-silicon electrical steel sheet; Method of Invention
- Method of Invention In the production of non-oriented high-silicon electrical steel sheets by strict control of chemical composition, hot rolling, warm cold rolling and annealing systems
- the high-efficiency and low-cost of oriented high-silicon electrical steel sheets can be realized by adding decarburization annealing and secondary recrystallization high-temperature annealing equipment on the line. Manufacturing has broad application prospects.
- Figure 1 is a graph showing the relationship between the secondary recrystallization ratio and the C content of oriented high silicon electrical steel
- FIG. 2 is a diagram showing the orientation of the secondary recrystallization of the oriented high-silicon electrical steel in the second embodiment of the present invention.
- the vertical direction is the width direction of the product;
- a is an ⁇ -oriented crystal grain, and
- b is a randomly oriented crystal grain.
- the device used for analyzing the magnetic induction in the embodiment of the present invention is an Iwatsu sy-8232B-H analyzer.
- the apparatus for secondary recrystallization late orientation imaging analysis is equipped with electron backscatter diffraction JF7001 scanning electron microscope (EBSD) analysis device.
- EBSD electron backscatter diffraction JF7001 scanning electron microscope
- heating under an inert atmosphere, a reducing atmosphere, an inert reduction mixed atmosphere is a combined blank
- the material is first placed in a heating furnace with an inert gas, a reducing gas or an inert reducing mixed gas for heating and heat preservation, heating and heat preservation
- the heating furnace is sealed or the gas is kept flowing, the volume purity of nitrogen, argon and hydrogen used is ⁇ 98%.
- the room temperature in the embodiment of the present invention is different from season to season, and the actual temperature is 0 to 30 °C.
- the slab is heated to 1000 ° C for soaking, holding time 5 min; then hot rolling, rolling temperature is 900 ° C, and finally The rolling temperature is 750 ° C, the hot rolling reduction rate is 50%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then the first rolling temperature is performed by a two-rolling method including intermediate annealing.
- the temperature is room temperature, the reduction ratio is 95%, the second rolling temperature is room temperature, the reduction ratio is 50%; the hot rolled steel sheet is processed to 0.10 mm, Obtaining a steel sheet; performing an intermediate annealing between the first and second rolling, an annealing temperature of 700 ° C, and a time of 600 min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of the decarburization annealing is 750 ° C, and the time is 60 min; Then, it is sent to a heating furnace and heated to 1000 ° C at a rate of 70 ° C / h under a nitrogen atmosphere to complete secondary recrystallization. Fire, obtaining oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.75T.
- the slab is heated to 1200 ° C for soaking, the holding time is 600 min; then hot rolling, the rolling temperature is 1180 ° C, The final rolling temperature is 1000 ° C, the hot rolling reduction rate is 90%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then the third rolling method is used, and the first two rolling temperatures are used.
- the degrees are 400 ° C and 200 ° C, respectively, the reduction rate is 40% and 95%, the third rolling temperature is 150 ° C, the reduction rate 50%, the hot-rolled steel sheet is processed to 0.10 mm to obtain a thin steel sheet; intermediate annealing is performed between adjacent two rolling, annealing temperature Degree 1100 ° C, time 0.5 min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of decarburization annealing is 900 ° C, and the time is 0.5 min; Then, it is sent to a heating furnace and heated to 1200 ° C at a rate of 5 ° C / h under a hydrogen atmosphere to complete secondary recrystallization. Fire, obtaining oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.55T.
- the slab is heated to 1100 ° C for soaking, holding time of 300 min; then hot rolling, the rolling temperature is 1000 ° C, The final rolling temperature is 800 ° C, the hot rolling reduction rate is 95%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then the first rolling temperature is performed by a two-rolling method including intermediate annealing. Degree at 300 ° C, the reduction rate is 40%, the second rolling temperature is 300 ° C, the reduction rate is 92%; processing hot-rolled steel sheet To 0.20mm, obtain a thin steel plate; perform intermediate annealing between the first and second rolling, annealing temperature 900 ° C, time 4min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of the decarburization annealing is 800 ° C, and the time is 3 min; After being sent to a heating furnace, it is heated to 1100 ° C at a rate of 60 ° C / h under an argon atmosphere to complete secondary recrystallization annealing.
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.45T.
- the slab is heated to 1000 ° C for soaking, the holding time is 60 min; then hot rolling, the rolling temperature is 980 ° C, The final rolling temperature is 850 ° C, and the hot rolling reduction rate is 95%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then the first rolling is performed by a three-rolling method including intermediate annealing.
- the temperature is 500 ° C
- the reduction rate is 40% and 80%
- the third rolling temperature is 300 ° C
- the reduction rate is 60%
- the hot-rolled steel sheet is processed to 0.20 mm to obtain a thin steel sheet; intermediate annealing is performed between adjacent two rollings, and the annealing temperature is 900 ° C. Time 5min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the decarburization annealing temperature is 850 ° C, and the time is 5 min; After being sent to a heating furnace, it is heated at a rate of 50 ° C / h under a mixed atmosphere of a ratio of nitrogen and hydrogen of 2:8. 1000 ° C, complete secondary recrystallization annealing, to obtain oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.58T.
- the slab is heated to 1200 ° C for soaking, holding time 5 min; then hot rolling, rolling temperature is 1180 ° C, The final rolling temperature is 850 ° C, the hot rolling reduction rate is 99%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then the first rolling temperature is performed by a two-rolling method including intermediate annealing. Degree is 700 ° C, the reduction rate is 50%, the second rolling temperature is 400 ° C, the reduction rate is 50%, the hot-rolled steel sheet is processed. To 0.50 mm, a thin steel plate is obtained; an intermediate annealing is performed between the first and second rolling, and the annealing temperature is 1000 ° C. 2min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of decarburization annealing is 900 ° C, and the time is 0.5 min; Then, it is sent to a heating furnace and heated at a rate of 40 ° C / h under a mixed atmosphere of nitrogen and hydrogen at a ratio of 7:3. 1200 ° C, complete secondary recrystallization annealing, to obtain oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.58T.
- the slab is heated to 1100 ° C for soaking, the holding time is 200 min; then hot rolling, the rolling temperature is 1050 ° C, The final rolling temperature is 880 ° C, the hot rolling reduction rate is 90%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then rolled by the third rolling method with intermediate annealing.
- the temperature is 400 ° C, the reduction rate is 40% and 50%, respectively, the third rolling temperature is 200 ° C, the reduction rate is 92%, will
- the hot-rolled steel sheet is processed to 0.10 mm to obtain a thin steel sheet; intermediate annealing is performed between adjacent two rollings, and the annealing temperature is 700 ° C. Time 3min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of the decarburization annealing is 750 ° C, and the time is 5 min; After being sent to a heating furnace, it is heated to 1100 ° C at a rate of 30 ° C / h under a mixed atmosphere of 1:1 ratio of argon gas to hydrogen gas. Performing secondary recrystallization annealing to obtain oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.58T.
- the slab is heated to 1000 ° C for soaking, the holding time is 500 min; then hot rolling, the rolling temperature is 970 ° C, The final rolling temperature is 800 ° C, the hot rolling reduction rate is 95%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is subjected to a normalization treatment at a temperature of 800 ° C for 600 minutes, then cooled to room temperature, and then pickled.
- a normalization treatment at a temperature of 800 ° C for 600 minutes, then cooled to room temperature, and then pickled.
- the surface oxide layer In addition to the surface oxide layer;
- the first rolling temperature is 400 ° C
- the reduction rate is 70%
- the second time The rolling temperature is 400 ° C
- the reduction rate is 80%
- the hot-rolled steel sheet from which the oxide layer is removed is processed to 0.20 mm to obtain a steel sheet
- Intermediate annealing is performed between the first and second rolling, the annealing temperature is 800 ° C, and the time is 3 min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of the decarburization annealing is 800 ° C, and the time is 5 min; After being sent to a heating furnace, it is heated to 1000 ° C at a rate of 5 ° C / h under a hydrogen atmosphere to complete secondary recrystallization annealing.
- decarburization annealing 800 ° C
- the time is 5 min
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.52T.
- the slab is heated to 1200 ° C for soaking, holding time of 100 min; then hot rolling, the rolling temperature is 1150 ° C, The final rolling temperature is 900 ° C, and the hot rolling reduction rate is 90%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is subjected to a normalization treatment at a temperature of 1200 ° C for 1 min, then cooled to 100 ° C, and then pickled off.
- a normalization treatment at a temperature of 1200 ° C for 1 min, then cooled to 100 ° C, and then pickled off.
- the first two rolling temperatures are at 500 ° C, and the reduction rates are 50% and 40%, the temperature of the third rolling is 200 ° C, the reduction rate is 70%, and the hot-rolled steel sheet from which the oxide layer is removed is processed to 0.30 mm.
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of decarburization annealing is 850 ° C, and the time is 3 min; After being sent to a heating furnace, it is heated to 1200 ° C at a rate of 10 ° C / h under a hydrogen atmosphere to complete secondary recrystallization annealing.
- decarburization annealing is 850 ° C
- the time is 3 min
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.55T.
- the slab is heated to 1100 ° C for soaking, the holding time is 30 min; then hot rolling, the rolling temperature is 1050 ° C, The final rolling temperature is 840 ° C, and the hot rolling reduction rate is 95%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then the first rolling is performed by a two-rolling method including intermediate annealing.
- the temperature is 600 ° C, the reduction rate is 95%, the second rolling temperature is at room temperature, the reduction rate is 50%, and the hot rolled steel sheet is processed.
- To 0.10 mm a thin steel plate is obtained; an intermediate annealing is performed between the first and second rolling, and the annealing temperature is 1000 ° C. 1min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of the decarburization annealing is 750 ° C, and the time is 60 min; Then, it is sent to a heating furnace and heated to 1100 ° C at a rate of 5 ° C / h under a hydrogen atmosphere to complete secondary recrystallization. Fire, obtaining oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.55T.
- the slab is heated to 1200 ° C for soaking, the holding time is 600 min; then hot rolling, the rolling temperature is 1150 ° C, The final rolling temperature is 920 ° C, and the hot rolling reduction rate is 90%, and a hot rolled steel sheet is obtained;
- the hot-rolled steel sheet is pickled to remove the surface oxide layer, and then rolled by the first three times with intermediate annealing.
- the temperatures are 700 ° C, 500 ° C and 300 ° C, respectively, the reduction rates are 40%, 60% and 80%, respectively, the temperature of the fourth rolling is At room temperature, the reduction ratio is 50%, the hot-rolled steel sheet is processed to 0.10 mm to obtain a thin steel sheet; Annealing, annealing temperature 1100 ° C, time 0.5min;
- the steel sheet is subjected to decarburization annealing and secondary recrystallization annealing; the temperature of decarburization annealing is 900 ° C, and the time is 0.5 min; Then, it is sent to a heating furnace and heated to 1000 ° C at 70 ° C / h under an inert hydrogen atmosphere to complete the second re-knot. Crystal annealing to obtain oriented high silicon electrical steel;
- the magnetic induction B 8 of the oriented high silicon electrical steel is 1.55T.
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Abstract
一种取向高硅电工钢的制备方法,属于冶金技术领域,按以下步骤进行:(1)按设定成分冶炼并浇铸铸坯,其成分按重量百分比含C 0.05~0.30%,Si 4.0~7.0%,Mn 0.01~1.0%,Als 0~0.20%,Sn 0~0.50%,Sb 0~0.50%,Cu 0~0.50%,Mo 0~0.10%,Ni 0~0.50%;(2)将板坯均热处理,然后进行热轧,压下率50~99%,获得热轧钢板;(3)采用含有中间退火的两次或两次以上轧制法,将热轧钢板加工到0.10~0.50mm,获得薄钢板;(4)将薄钢板进行脱碳退火和二次再结晶退火。本发明不使用AlN、MnS、Cu2S等各种第二相颗粒作为抑制剂,即可实现完善的二次再结晶,从而获得取向高硅电工钢板,降低了板坯加热温度,简化了生产流程。
Description
本发明属于冶金技术领域,特别涉及一种取向高硅电工钢的制备方法。
电工钢是电力电子设备的主要铁芯材料,随硅含量增大,电工钢的磁导率增加、电导率
和磁致伸缩系数下降,所以硅含量重量百分比为4.0~7.0%的高硅电工钢相对普通电工钢(Si
<3.5%)具有低铁损和低噪音优势;但受制于高硅电工钢的本征硬脆性,目前只有日本的JFE
钢铁公司采用化学气相沉积法实现了批量生产(日本公开号为JP63227717A、JP63069915A
的专利)。近年来,围绕无取向高硅电工钢,中国东北大学和北京科技大学采用轧制方法,研
究了无取向高硅电工钢板带的制备技术,并且在无取向高硅电工钢超薄带和磁性能优化方面
取得进展(公开号为CN102172824B,CN101049669A和CN102126110B,CN102151695B,
CN101886215A的专利);上海大学采用扩散沉积的方法,可实现连续制备硅含量不低于6.5%
的高硅电工钢(公开号为CN103014613的专利)。
电工钢具有磁各向异性,故具有强η(<001>//RD,RD是轧向)织构的取向电工钢沿轧
向具有明显高于无取向电工钢的磁性能;硅重量百分含量小于3.5%的取向电工钢通常分为两
类:普通取向电工钢(CGO)和高磁感取向电工钢(Hi-B)。取向电工钢的制造工艺和设备复
杂,成分控制严格,杂质含量要求极低,制造工序长和影响磁性能因素多,因此其产品质量
常被认为是衡量一个国家特殊钢制造技术水平的重要标志;取向电工钢在制造过程中,一般
需要使用被称作抑制剂的第二相颗粒,其作用是在最终的高温退火过程中促进二次再结晶发
生;普通取向电工钢生产技术由Goss在1934年发明,以MnS作为抑制剂,采用二次中等压
下率冷轧。高磁感取向电工钢的主要制造方法有三种:(1)以新日铁为代表,采用AlN第二
相颗粒为主、MnS第二相颗粒为辅的抑制剂以及一次大压下率冷轧法,是目前最通用的高磁
感取向电工钢生产方法;(2)以JFE为代表,采用Sb、Mo、MnSe第二相颗粒或MnS第二
相颗粒为抑制剂以及二次冷轧法;(3)美国钢铁公司采用B、MnSe第二相颗粒或MnS第二
相颗粒为抑制剂以及一次冷轧法。
取向高硅电工钢(硅的重量百分含量为4.0~7.0%)的制造技术只有日本的钢铁生产企业
报道过,国内尚不具备;在日本专利平4-80321中,采用AlN第二相颗粒为主抑制剂的方案,
将酸溶铝控制在0.012~0.048%范围内,获得了取向高硅电工钢;但高硅电工钢脆性大,为了
保证连续成形和高成材率,从冶炼开始到最终的成品退火,每道工艺流程都需要考虑成形性
的需求,如果再考虑抑制剂的控制要求,生产过程中的工艺参数窗口范围将极其狭窄,不利
于大工业生产的连续稳定进行。例如,根据普通硅含量取向硅钢的生产工艺,采用MnS、AlN
第二相颗粒的抑制剂方案,板坯需要在1300℃以上加热使初生MnS固溶到基体中;而高硅
钢中的高硅含量导致熔点降低,经1300℃以上高温加热的高硅电工钢板坯在热轧时容易开裂,
成材率大幅下降。即使对于采用板坯低温加热技术的取向硅钢生产流程,板坯仍需进行1200℃
左右的长时间加热。此外,无论是MnS、AlN或是其它基于第二相颗粒作为抑制剂的取向高
硅钢方案,都要面对抑制剂行为的精细控制与成形过程精细控制的冲突问题,都增加了钢板
中对磁性不利的S、N等抑制剂形成元素,这些元素必须经高温净化退火工序去除,而高温
净化退火通常在1200℃下的纯氢气中长时间进行,能耗大、效率低。综上所述,针对磁性能
优异、加工性差、生产复杂的取向高硅电工钢,开发不利用第二相颗粒作为抑制剂的制造取
向高硅电工钢是目前急需解决的问题。
发明内容
针对现有取向高硅电工钢在制备技术上存在的上述问题,本发明提供一种取向高硅电工
钢的制备方法,不使用AlN、MnS、Cu2S等各种第二相颗粒作为抑制剂,通过严格控制轧制
和退火工艺参数,即可实现完善的二次再结晶,从而获得高磁感取向高硅电工钢板。
本发明的取向高硅电工钢的制备方法按以下步骤进行:
1、按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.05~0.30%,
Si4.0~7.0%,Mn0.01~1.0%,Als0~0.20%,Sn0~0.50%,Sb0~0.50%,Cu0~0.50%,Mo0~0.10%,
Ni0~0.50%,N≤0.01%,S≤0.02%,P≤0.10%,余量为Fe;
2、将铸坯加热至1000~1200℃均热处理,时间为5~600min;然后进行热轧,开轧温度
900~1180℃,终轧温度750~1000℃,热轧压下率50~99%,获得热轧钢板;
3、将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的两次或两次以上轧制法,
将热轧钢板加工到0.10~0.50mm,获得薄钢板;当进行两次轧制法时,第一次为温冷轧,轧
制温度为室温~700℃,压下率为40~95%,第二次为冷轧,轧制温度为室温~400℃,压下率
为50~92%;当进行两次以上轧制法时,除最后一次轧制外,其余次轧制为温冷轧,轧制温度
为室温~700℃,压下率为40~95%,最后一次为冷轧,轧制温度为室温~400℃,压下率为
50~92%;
4、将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为750~900℃,时间为
0.5~60min;脱碳退火后将薄钢板送入加热炉中,在惰性气氛、还原气氛或惰性还原混合气氛
条件下,以5~70℃/h的速度加热至1000~1200℃,完成二次再结晶退火,获得取向高硅电工
钢。
上述的热轧钢板在酸洗去除表面氧化层前进行或不进行常化处理,进行常化处理时的温
度为800~1200℃,时间为1~600min,然后冷却至室温~100℃。
上述的中间退火是指在相邻两次轧制之间进行中间退火,退火温度700~1100℃,时间
0.5~600min。
上述的惰性气氛是指氮气气氛或氩气气氛。
上述的还原气氛是指氢气气氛。
上述的惰性还原混合气氛是指惰性气体与氢气的混合气氛,混合比例为任意比例。
本发明的方法中成分限定的原理是:
1、C可以细化高硅电工钢初次再结晶晶粒尺寸,促进二次再结晶的发生;同时,C是对
磁性能有害的元素,在最终退火前,必须采用脱碳退火工艺去除,超过0.3%,脱碳十分困难,
因此原料中C含量控制在0.05~0.3%之间;
2、Si是提高电阻率进而降低涡流损耗乃至总铁损的有效元素,故以接近普通电工钢最
高硅含量的4.0%作为下限;另一方面,如果硅含量超过7.0%,矫顽力提高、饱和磁感应强
度和最大磁导率降低,同时加工性显著恶化;
3、Mn是提高热轧性能的必要元素,但含量超过1.0%,影响冷加工性;
4、Als是炼钢过程中不可避免的杂质,Als大于0.2%会降低高硅电工钢的冷加工性;
5、N和S是高硅电工钢中对磁性有害的元素,因此控制N≤0.01%,S≤0.02%。
此外,钢板的组成中还可含有以下成分中的一种或多种:P、Sn、Sb、Cu、Mo、Ni;以
上元素的适量添加,可以细化初次再结晶晶粒尺寸,促进二次再结晶进行。
本发明的薄钢板退火主要由脱碳退火和二次再结晶退火组成,可以包含或不包含高温净
化退火工序,获得取向高硅电工钢,是指整个制备过程中不使用AlN、MnS、Cu2S等各种第
二相颗粒作为抑制剂;本发明的方法的主要优点是:(1)避免了铸坯高温加热带来的加热炉
效率低、铸坯氧化严重、成材率低、能源消耗大的问题;(2)避免了因AlN、MnS第二相颗
粒等抑制剂的加入,增大取向高硅电工钢的强度、降低塑韧性,从而带来需额外解决的加工
成形问题。
本发明是以无取向高硅电工钢板的轧制制造流程与装备为基础开发的生产工艺;采用本
发明方法通过严格控制化学成分、热轧、温冷轧和退火制度,在无取向高硅电工钢板的生产
线上增加脱碳退火和二次再结晶高温退火设备,即可实现取向高硅电工钢板的高效率低成本
制造,具有广阔的应用前景。
图1为取向高硅电工钢二次再结晶比例与C含量的关系图;
图2为本发明实施例2中的取向高硅电工钢二次再结晶后期取向成像图;图中的水平方
向为轧制方向,垂直方向为产品的宽度方向;a为η取向晶粒,b为随机取向晶粒。
本发明实施例中分析磁感采用的设备为Iwatsu sy-8232B-H分析仪。
本发明实施例中二次再结晶后期取向成像分析采用的设备为配备有电子背散射衍射
(EBSD)分析装置的JF7001扫描电子显微镜。
本发明实施例中的在惰性气氛、还原气氛、惰性还原混合气氛条件下加热,是将组合坯
料先置于具有惰性气体、还原气体或惰性还原混合气体的加热炉中进行加热保温,加热保温
时加热炉密闭或者保持气体流通均可,采用的氮气、氩气和氢气的体积纯度≥98%。
本发明实施例中的室温根据季节不同,实际温度在0~30℃。
实施例1
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.05%,Si
4.0%,Mn1.0%,Als0.20%,N0.01%,S0.02%,P0.10%,余量为Fe;
将铸坯加热至1000℃均热处理,保温时间5min;然后进行热轧,开轧温度为900℃,终
轧温度750℃,热轧压下率为50%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的两次轧制法,第一次轧制温
度为室温,压下率为95%,第二次轧制温度为室温,压下率为50%;将热轧钢板加工到0.10mm,
获得薄钢板;在第一次和第二次轧制之间进行中间退火,退火温度700℃,时间600min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为750℃,时间为60min;
然后送入加热炉中,在氮气气氛条件下,以70℃/h的速度加热至1000℃,完成二次再结晶退
火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.75T。
实施例2
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.06%,Si
6.55%,Mn0.01%,Als0.006%,N0.008%,S0.06%,P0.008%,余量为Fe;
将铸坯加热至1200℃均热处理,保温时间600min;然后进行热轧,开轧温度为1180℃,
终轧温度1000℃,热轧压下率为90%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的三次轧制法,前两次轧制温
度分别为400℃和200℃,压下率分别为40%和95%,第三次轧制的温度在150℃,压下率为
50%,将热轧钢板加工到0.10mm,获得薄钢板;在相邻两次轧制之间进行中间退火,退火温
度1100℃,时间0.5min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为900℃,时间为0.5min;
然后送入加热炉中,在氢气气氛条件下,以5℃/h的速度加热至1200℃,完成二次再结晶退
火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.55T。
实施例3
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.30%,Si
7.0%,Mn0.05%,Als0.05%,N0.001%,S0.006%,P0.006%,余量为Fe;
将铸坯加热至1100℃均热处理,保温时间300min;然后进行热轧,开轧温度为1000℃,
终轧温度800℃,热轧压下率为95%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的两次轧制法,第一次轧制温
度在300℃,压下率为40%,第二次轧制的温度在300℃,压下率为92%;将热轧钢板加工
到0.20mm,获得薄钢板;在第一次和第二次轧制之间进行中间退火,退火温度900℃,时间
4min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为800℃,时间为3min;然
后送入加热炉中,在氩气气氛条件下,以60℃/h的速度加热至1100℃,完成二次再结晶退火,
获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.45T。
实施例4
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.30%,Si
6.45%,Mn0.05%,Als0.06%,Ni0.5%,N0.01%,S0.02%,P0.008%,余量为Fe;
将铸坯加热至1000℃均热处理,保温时间60min;然后进行热轧,开轧温度为980℃,
终轧温度850℃,热轧压下率为95%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的三次轧制法,前两次的轧制
的温度在500℃,压下率分别为40%和80%,第三次轧制的温度在300℃,压下率为60%,
将热轧钢板加工到0.20mm,获得薄钢板;在相邻两次轧制之间进行中间退火,退火温度900℃,
时间5min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为850℃,时间为5min;然
后送入加热炉中,在氮气和氢气比例为2:8的混合气氛条件下,以50℃/h的速度加热至
1000℃,完成二次再结晶退火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.58T。
实施例5
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.05%,Si
6.52%,Mn0.02%,Als0.03%,Mo0.1%,N0.002%,S0.005%,P0.008%,余量为Fe;
将铸坯加热至1200℃均热处理,保温时间5min;然后进行热轧,开轧温度为1180℃,
终轧温度850℃,热轧压下率为99%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的两次轧制法,第一次轧制温
度在700℃,压下率为50%,第二次轧制的温度在400℃,压下率为50%,将热轧钢板加工
到0.50mm,获得薄钢板;在第一次和第二次轧制之间进行中间退火,退火温度1000℃,时
间2min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为900℃,时间为0.5min;
然后送入加热炉中,在氮气和氢气比例为7:3的混合气氛条件下,以40℃/h的速度加热至
1200℃,完成二次再结晶退火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.58T。
实施例6
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.15%,Si
6.50%,Mn0.12%,Als0.002%,Sn0.01%,N0.004%,S0.006%,P0.007%,余量为Fe;
将铸坯加热至1100℃均热处理,保温时间200min;然后进行热轧,开轧温度为1050℃,
终轧温度880℃,热轧压下率为90%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的三次轧制法,前两次轧制的
温度在400℃,压下率分别为40%和50%,第三次轧制的温度在200℃,压下率为92%,将
热轧钢板加工到0.10mm,获得薄钢板;在相邻两次轧制之间进行中间退火,退火温度700℃,
时间3min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为750℃,时间为5min;然
后送入加热炉中,在氩气和氢气比例为1:1的混合气氛条件下,以30℃/h的速度加热至1100℃,
完成二次再结晶退火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.58T。
实施例7
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.23%,Si
6.47%,Mn0.02%,Als0.005%,Sn0.50%,Sb0.005%,Cu0.01%,N0.002%,S0.004%,P
0.009%,余量为Fe;
将铸坯加热至1000℃均热处理,保温时间500min;然后进行热轧,开轧温度为970℃,
终轧温度800℃,热轧压下率为95%,获得热轧钢板;
将热轧钢板进行常化处理,温度为800℃,时间为600min,然后冷却至室温,再酸洗去
除表面氧化层;
采用含有中间退火的两次轧制法,第一次的轧制温度在400℃,压下率为70%,第二次
轧制的温度在400℃,压下率为80%,将去除氧化层的热轧钢板加工到0.20mm,获得薄钢板;
在第一次和第二次轧制之间进行中间退火,退火温度800℃,时间3min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为800℃,时间为5min;然
后送入加热炉中,在氢气气氛条件下,以5℃/h的速度加热至1000℃,完成二次再结晶退火,
获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.52T。
实施例8
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.21%,Si
6.41%,Mn0.21%,Als0.003%,Sb0.50%,N0.009%,S0.002%,P0.006%,余量为Fe;板
将铸坯加热至1200℃均热处理,保温时间100min;然后进行热轧,开轧温度为1150℃,
终轧温度900℃,热轧压下率为90%,获得热轧钢板;
将热轧钢板进行常化处理,温度为1200℃,时间为1min,然后冷却至100℃,再酸洗去
除表面氧化层;
采用含有中间退火的三次轧制法,前两次的轧制的温度在500℃,压下率分别为50%和
40%,第三次轧制的温度在200℃,压下率为70%,将去除氧化层的热轧钢板加工到0.30mm,
获得薄钢板;在相邻两次轧制之间进行中间退火,退火温度900℃,时间10min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为850℃,时间为3min;然
后送入加热炉中,在氢气气氛条件下,以10℃/h的速度加热至1200℃,完成二次再结晶退火,
获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.55T。
实施例9
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.06%,Si
6.54%,Mn0.33%,Als0.01%,Sn0.14%,Sb0.01%,Cu0.50%,N0.0021%,S0.003%,P
0.008%,余量为Fe;
将铸坯加热至1100℃均热处理,保温时间30min;然后进行热轧,开轧温度为1050℃,
终轧温度840℃,热轧压下率为95%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的两次轧制法,第一次轧制的
温度在600℃,压下率为95%,第二次轧制的温度在室温,压下率为50%,将热轧钢板加工
到0.10mm,获得薄钢板;在第一次和第二次轧制之间进行中间退火,退火温度1000℃,时
间1min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为750℃,时间为60min;
然后送入加热炉中,在氢气气氛条件下,以5℃/h的速度加热至1100℃,完成二次再结晶退
火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.55T。
实施例10
按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C0.06%,Si
6.57%,Mn0.11%,Cu0.06%,N0.003%,S0.005%,P0.004%,余量为Fe;
将铸坯加热至1200℃均热处理,保温时间600min;然后进行热轧,开轧温度为1150℃,
终轧温度920℃,热轧压下率为90%,获得热轧钢板;
将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的四次轧制法,前三次轧制的
温度分别为700℃、500℃和300℃,压下率分别为40%、60%和80%,第四次轧制的温度在
室温,压下率为50%,将热轧钢板加工到0.10mm,获得薄钢板;在相邻两次轧制之间进行中
间退火,退火温度1100℃,时间0.5min;
将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为900℃,时间为0.5min;
然后送入加热炉中,在惰性氢气气氛条件下,以70℃/h的速度加热至1000℃,完成二次再结
晶退火,获得取向高硅电工钢;
取向高硅电工钢的磁感B8为1.55T。
Claims (4)
- 一种取向高硅电工钢的制备方法,其特征在于按以下步骤进行:(1)按设定成分冶炼并在1400~1600℃浇铸成铸坯,其成分按重量百分比含C 0.05~0.30%,Si4.0~7.0%,Mn0.01~1.0%,Als0~0.20%,Sn0~0.50%,Sb0~0.50%,Cu0~0.50%, Mo0~0.10%,Ni0~0.50%,N≤0.01%,S≤0.02%,P≤0.10%,余量为Fe;(2)将铸坯加热至1000~1200℃均热处理,时间为5~600min;然后进行热轧,开轧温 度900~1180℃,终轧温度750~1000℃,热轧压下率50~99%,获得热轧钢板;(3)将热轧钢板酸洗去除表面氧化层,然后采用含有中间退火的两次或两次以上轧制 法,将热轧钢板加工到0.10~0.50mm,获得薄钢板;当进行两次轧制法时,第一次为温冷轧, 轧制温度为室温~700℃,压下率为40~95%,第二次为冷轧,轧制温度为室温~400℃,压下 率为50~92%;当进行两次以上轧制法时,除最后一次轧制外,其余次轧制为温冷轧,轧制温 度为室温~700℃,压下率为40~95%,最后一次为冷轧,轧制温度为室温~400℃,压下率为 50~92%;(4)将薄钢板进行脱碳退火和二次再结晶退火;脱碳退火的温度为750~900℃,时间为 0.5~60min;脱碳退火后将薄钢板送入加热炉中,在惰性气氛、还原气氛或惰性还原混合气氛 条件下,以5~70℃/h的速度加热至1000~1200℃,完成二次再结晶退火,获得取向高硅电工 钢。
- 根据权利要求1所述的一种取向高硅电工钢的制备方法,其特征在于所述的步骤(3) 中的含有中间退火是指在相邻两次轧制之间进行中间退火,退火温度700~1100℃,时间 0.5~600min。
- 根据权利要求1所述一种的取向高硅电工钢的制备方法,其特征在于所述的惰性气 氛是指氮气气氛或氩气气氛;所述的还原气氛是指氢气气氛;所述的惰性还原混合气氛是指 惰性气体与氢气的混合气氛,混合比例为任意比例。
- 根据权利要求1所述一种的取向高硅电工钢的制备方法,其特征在于热轧钢板在酸 洗去除表面氧化层前进行或不进行常化处理,进行常化处理时的温度为800~1200℃,时间为 1~600min,然后冷却至室温~100℃。
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