WO2024002260A1 - Oriented silicon steel and manufacturing method therefor - Google Patents

Oriented silicon steel and manufacturing method therefor Download PDF

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WO2024002260A1
WO2024002260A1 PCT/CN2023/103985 CN2023103985W WO2024002260A1 WO 2024002260 A1 WO2024002260 A1 WO 2024002260A1 CN 2023103985 W CN2023103985 W CN 2023103985W WO 2024002260 A1 WO2024002260 A1 WO 2024002260A1
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silicon steel
oriented silicon
annealing
temperature
steel
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PCT/CN2023/103985
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French (fr)
Chinese (zh)
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凌晨
李国保
杨勇杰
吉亚明
黑红旭
胡卓超
姜全力
马长松
吴美洪
赵自鹏
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宝山钢铁股份有限公司
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Publication of WO2024002260A1 publication Critical patent/WO2024002260A1/en

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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/68Temporary coatings or embedding materials applied before or during heat treatment
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D3/00Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02Extraction of non-metals
    • C21D3/04Decarburising
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
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    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/005Heat treatment of ferrous alloys containing Mn
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D6/00Heat treatment of ferrous alloys
    • C21D6/008Heat treatment of ferrous alloys containing Si
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    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216Modifying 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
    • C21D8/1222Hot rolling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216Modifying 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
    • C21D8/1233Cold rolling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying 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
    • C21D8/1255Modifying 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 with diffusion of elements, e.g. decarburising, nitriding
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying 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
    • C21D8/1272Final recrystallisation annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283Application of a separating or insulating coating
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/001Ferrous alloys, e.g. steel alloys containing N
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/008Ferrous alloys, e.g. steel alloys containing tin
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/12Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/16Ferrous alloys, e.g. steel alloys containing copper
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24Nitriding
    • C23C8/26Nitriding of ferrous surfaces

Definitions

  • the present invention relates to a oriented silicon steel and a manufacturing method thereof, in particular to a oriented silicon steel with low magnetostriction and a manufacturing method thereof.
  • Grain-oriented silicon steel is a soft magnetic material characterized by sharp ⁇ 110 ⁇ 001> orientation (i.e. Gaussian grains). Oriented silicon steel is often used to make transformer cores and is an important functional material for making transformer cores.
  • oriented silicon steel can be divided into ordinary oriented silicon steel (referred to as CGO) and high magnetic induction oriented silicon steel (referred to as Hi-B); compared with CGO silicon steel, Hi -B silicon steel has lower iron loss, higher magnetic induction intensity and smaller magnetostriction.
  • CGO ordinary oriented silicon steel
  • Hi-B high magnetic induction oriented silicon steel
  • the noise performance of transformers has become an indicator that manufacturers focus on. Since the magnetostriction of oriented silicon steel has a decisive influence on the noise performance of transformers, low magnetostriction oriented silicon steel has become a research hotspot.
  • the existing technology mainly reduces the magnetostriction of oriented silicon steel through the following three technical routes: 1) improving the Gauss grain orientation of the finished oriented silicon steel; 2) reducing the finished thickness of the oriented silicon steel; and 3) Apply high tension coating. All three technical routes can reduce the magnetostriction of oriented silicon steel.
  • CN111748731A (published on October 9, 2020, "Low magnetostrictive oriented silicon steel and manufacturing method thereof") produces localized structures due to local sequential structural arrangement by performing thermal stretching and magnetic annealing on the silicon steel substrate under specific conditions.
  • the preferential orientation of the grains caused by magnetic inhomogeneity increases the unidirectional magnetic anisotropy along the rolling direction (i.e., the volume of the 180° magnetic domain wall increases and the volume of the 90° magnetic domain wall decreases), This reduces the 90° magnetic domain volume of the finished oriented silicon steel, thereby reducing the magnetostriction of the oriented silicon steel, thereby reducing the overall noise level of the transformer.
  • the magnetic annealing temperature is 750-200°C
  • the magnetic field direction is the rolling direction or transverse direction
  • the magnetic field size is a DC magnetic field of 2500A/m + a pulse field of short-term pulse magnetic field of 50000A/m (50ms, 1 -10Hz).
  • the L v A (17/50) of the finished oriented silicon steel thus obtained is ⁇ 55dB(A).
  • CN105220071A discloses a oriented silicon steel.
  • the L v A(17) of the finished oriented silicon steel made in this way is less than 55dB(A). The vibration generated by the transformer core made of this oriented silicon steel is small, and the overall noise level of the transformer is reduced.
  • CN107881411A discloses a low-iron loss and low-noise oriented silicon steel. This application reduces iron loss and magnetostriction/reduces noise by strictly controlling the vertical reflectance R of the magnesium silicate bottom layer of the oriented silicon steel substrate to visible light to 40-60%, while ensuring uniform gloss of the magnesium silicate bottom layer.
  • the magnetostrictive vibration noise value of the final product is less than 60dB(A), which is especially suitable for transformers.
  • magnetostriction can be reduced to a certain extent by controlling the 90° magnetic domain distribution and the coating tension level.
  • both of the above methods require the use of additional equipment or conditions to reduce magnetostriction, and the reduction in magnetostriction is not significant.
  • adding a magnetic field to affect the 90° magnetic domain in CN111748731A can increase the volume of the 180° magnetic domain wall, if the Gaussian texture of the oriented silicon steel substrate itself is not sharp enough, it will be difficult to reduce the amplitude of magnetostriction by adding external conditions later. Relatively limited.
  • the method of refining magnetic domains by increasing coating tension also has the same problem, and this method also has extremely high requirements on coating performance.
  • magnetostriction can be reduced to a certain extent by reducing the thickness of the silicon steel sheet.
  • rolling silicon steel to a thinner thickness will be more difficult and will also result in increased costs.
  • the inventor hopes to develop a new type of oriented silicon steel with low magnetostriction and its manufacturing method.
  • the production process will be green and On the basis of reducing consumption, it essentially increases the magnetic induction intensity of oriented silicon steel and reduces the magnetostriction of oriented silicon steel (by reducing the deviation angle of Gaussian grains), thus achieving high magnetic induction intensity and low magnetostriction of oriented silicon steel.
  • Level matching the inventor hopes to develop a new type of oriented silicon steel with low magnetostriction and its manufacturing method.
  • the main purpose of the present invention is to provide a oriented silicon steel and a manufacturing method thereof, which have excellent magnetic property matching (especially in terms of high magnetic induction intensity and low magnetostriction) while reducing energy consumption during the production process. Media consumption is significantly reduced.
  • the present application provides a oriented silicon steel, which, in addition to containing more than 90% Fe and unavoidable impurities, also contains the following chemical elements in mass percentage:
  • C 0.020-0.080%, Si: 2.00-4.50%, Mn: 0.01-0.10%, S ⁇ 0.005%, acid-soluble Al: 0.010-0.040%, N: 0.002-0.015%, Nb: 0.006-0.120%, and At least one selected from the group consisting of P: 0.01-0.10%, Sn: 0.01-0.30%, and Cu: 0.01-0.50%.
  • the oriented silicon steel contains the following chemical elements in mass percentage:
  • the thickness of the oriented silicon steel is 0.15-0.30mm.
  • the magnetic induction intensity B8 of the oriented silicon steel is >1.95T, and the magnetostrictive vibration speed sound pressure level L v A ⁇ 50dB (A).
  • the present application provides a method for manufacturing the above-mentioned oriented silicon steel, the method includes the following steps:
  • Hot rolling including rough rolling, coiling and holding and finishing rolling
  • the thickness of the slab is 180-250mm.
  • the heating temperature of the slab is 900-1150°C.
  • the acquired inhibitor process of nitriding treatment is used in this application, so the content of inhibitor elements in the slab is relatively low.
  • the heating temperature in step 2) is conducive to reducing energy consumption while obtaining a sufficient amount of inhibitor.
  • the heating temperature of the slab in step 2) is preferably controlled to 900-1150°C.
  • the thickness of the intermediate billet after rough rolling is 35-50 mm.
  • the end temperature of rough rolling is higher than 950°C
  • the coiling temperature is 800-1050°C
  • the coiling time is 30-200s
  • the start temperature of finishing rolling is lower than 1050°C.
  • This application sets the end temperature of rough rolling to higher than 950°C, which can ensure that the curling temperature is 800-1050°C, the coiling time is 30-200s, and the starting temperature of subsequent finishing rolling is lower than 1050°C.
  • the layers of the hot-rolled plate itself heat each other during the heat preservation process after coiling, so no additional heating is needed; and the coiling between rough rolling and finishing rolling can In order to make the structure of the hot-rolled plate more fully recrystallized, at the same time, some inhibitors can be dispersed and precipitated.
  • the coiling temperature is lower than 800°C or the coiling time is less than 30s, the expected structural recrystallization effect of the hot rolled plate cannot be achieved; when the coiling temperature is higher than 1050°C or the coiling time exceeds 200s, the crystallization of the intermediate billet will not be achieved. The granular structure and precipitated inhibitors will coarsen, adversely affecting the development of subsequent tissue and Gaussian texture. Therefore, it is preferable to set the temperature and/or time during hot rolling within the above range.
  • normalized annealing treatment is performed between 3) hot rolling step and 4) cold rolling step.
  • the normalized annealing temperature does not exceed 1000°C, preferably 800-1000°C, and more preferably 800-980°C. Normalized annealing The time is 20-200s.
  • the inventor unexpectedly found that if the hot-rolled plate is conventionally normalized annealed at an annealing temperature of about 1100-1200°C according to the current existing technology, not only will it result in a normalized plate grain structure If it is too large, it will also cause the inhibitor to coarsen, eventually leading to the deterioration of the magnetic properties.
  • decarburization annealing can be achieved without subsequent normalization annealing treatment, or when normalization annealing treatment is performed at a normalization annealing temperature not exceeding 1000°C.
  • the number of Gaussian grains with an offset angle of ⁇ 3° in the final steel plate accounts for >10%, thereby obtaining a finished oriented silicon steel with the required Gaussian grain orientation and magnetic induction intensity.
  • the proportion of Gaussian grains with an offset angle of ⁇ 3° in the steel plate after decarburization annealing will be significantly reduced (i.e. significantly less than 10%).
  • the cold rolling reduction ratio is >80%.
  • the decarburization annealing temperature is 800-900°C.
  • the decarburization effect will be insignificant; when the decarburization annealing temperature is higher than 900°C, the primary recrystallization grains will be too coarse, affecting the secondary recrystallization.
  • the proportion of Gaussian grains with an offset angle of ⁇ 3° in the steel plate after decarburization annealing is >10%.
  • the proportion of Gaussian grains with an offset angle ⁇ 3° in the steel plate after decarburization annealing refers to the ratio (in %) of the number of Gaussian grains with an offset angle ⁇ 3° to the total number of Gaussian grains.
  • device angle refers to the Gaussian grain orientation deviation angle.
  • the deviation angle and proportion of Gaussian grains were observed and counted by a scanning electron microscope with an electron backscatter diffraction (EBSD) system.
  • EBSD electron backscatter diffraction
  • the nitriding amount is 50-280 ppm.
  • nitriding treatment must be performed before high-temperature annealing to form an inhibitor that is sufficient to inhibit the growth of primary recrystallized grains.
  • the nitriding amount is lower than 50ppm, the amount of inhibitors formed is insufficient; when the nitriding amount is higher than 280ppm, it will have a negative impact on the formation of the magnesium silicate bottom layer during high-temperature annealing.
  • the nitriding amount in step 6) of the present invention is strictly controlled to 50-280 ppm.
  • the annealing isolating agent can be an annealing isolating agent commonly used in the art, preferably MgO.
  • the annealing temperature is 1100-1250°C, and the annealing time is greater than 25 hours.
  • the insulating coating can be formed using a coating liquid commonly used in the art, for example, by coating a coating liquid containing phosphate, colloidal silica and chromic anhydride; the insulating coating can be formed using this method for scoring.
  • a coating liquid commonly used in the art, for example, by coating a coating liquid containing phosphate, colloidal silica and chromic anhydride; the insulating coating can be formed using this method for scoring.
  • Commonly used scoring methods in the field such as laser scoring, electrochemical scoring, toothed roller scoring, high-pressure water beam scoring, etc.
  • the oriented silicon steel and its manufacturing method of the present invention achieve the following beneficial effects:
  • the present invention obtains oriented silicon steel that matches high magnetic induction intensity and low magnetostriction at a high level.
  • the oriented silicon steel of the present invention has excellent magnetic properties (magnetic induction intensity B8>1.95T, magnetostrictive vibration speed sound pressure level L v A ⁇ 50dB(A)), and has good economic benefits and application prospects.
  • Adding an appropriate amount of element C can ensure that an appropriate proportion of ⁇ phase is obtained during hot rolling or normalization, which is conducive to the precipitation of fine dispersion inhibitors.
  • the element C content in the steel is lower than 0.020%, the proportion of ⁇ phase is low, which is not conducive to the precipitation of inhibitors; when the element C content in the steel is higher than 0.080%, the decarburization cost will increase.
  • the content of element C in the oriented silicon steel of the present invention is controlled to 0.020-0.080%, preferably 0.022-0.073%.
  • Element Si is the main element that reduces iron loss.
  • the element Si content in the steel should not be too low or too high.
  • the element Si content in silicon steel is less than 2.00%, it is difficult for the resulting oriented silicon steel to obtain the required low iron loss; when the element Si content in the steel is higher than 4.50%, cold rolling will be difficult and the yield rate will be reduced.
  • the content of element Si in the oriented silicon steel of the present invention is controlled to 2.00-4.50%, preferably 2.19-4.29%.
  • Mn Adding an appropriate amount of element Mn can form a small amount of MnS auxiliary inhibitor during continuous casting and hot rolling, which can effectively improve the microstructure and rollability of grain-oriented silicon steel.
  • the content of element Mn in the steel must be strictly controlled. When the Mn content is lower than 0.01%, it is not conducive to obtaining the required silicon steel microstructure and rolling properties; when the Mn content is higher than 0.10%, the slab heating temperature will increase significantly, and coarse MnS inhibitors will easily form. Based on these considerations, the content of element Mn in the oriented silicon steel of the present invention is controlled to 0.01-0.10%, preferably 0.01-0.09%.
  • Element S can form auxiliary inhibitors such as MnS and Cu 2 S.
  • the content of element S in steel should not be too high. When the element S content in steel is too high, it will significantly increase the slab heating temperature, which is not conducive to production. Based on these considerations, the content of element S in the grain-oriented silicon steel of the present invention is controlled to S ⁇ 0.005%, preferably ⁇ 0.004%.
  • Acid-soluble Al is an important component in forming the main inhibitor AlN.
  • the inhibitor When the acid-soluble Al content in the steel is lower than 0.010%, the inhibitor will be insufficient; when the acid-soluble Al content in the steel is higher than 0.040%, the inhibitor AlN will be coarse. Therefore, the content of acid-soluble Al in silicon steel needs to be strictly controlled. Based on these considerations, the content of acid-soluble Al in the oriented silicon steel of the present invention is controlled to 0.010-0.040%, preferably 0.012-0.039%.
  • Adding an appropriate amount of element N can appropriately suppress grain growth.
  • the element N added to silicon steel can cooperate with acid-soluble Al to form AlN before nitriding, thereby effectively inhibiting the growth of primary recrystallized grains.
  • the element N content in steel is lower than 0.002%, the growth of primary recrystallized grains cannot be effectively suppressed; when the element N content in steel is higher than 0.015%, it will significantly increase the difficulty of steelmaking.
  • the content of element N in the oriented silicon steel of the present invention is controlled to 0.002-0.015%, preferably 0.003-0.014%.
  • Nb In order to reduce the slab heating temperature, the content of elements Mn and Cu is relatively low, but this will lead to insufficient precipitation of MnS and Cu 2 S. Therefore, in order to make up for the problem of insufficient inhibitory ability of inhibitors, an appropriate amount of element Nb is added to silicon steel. Element Nb can form an auxiliary inhibitor Nb(C,N) and play the role of an auxiliary inhibitor. In addition, since the solid solution temperature of Nb(C,N) is relatively low, it can also reduce the slab heating temperature.
  • the content of element Nb in the oriented silicon steel of the present invention is controlled to 0.006-0.120%, preferably 0.006-0.118%.
  • the elements P and Sn are both grain boundary segregation elements. Adding appropriate amounts of elements P and Sn to silicon steel can act as auxiliary inhibitors. When the content of the elements P and Sn in the steel is less than 0.01% respectively, the auxiliary inhibitory effect cannot be fully exerted; when the content of the elements P and Sn in the steel is higher than 0.10% and 0.30% respectively, it will be detrimental to decarburization and nitriding. Influence. Based on these considerations, the content of element P in the grain-oriented silicon steel of the present invention is controlled to 0.01-0.10%, preferably 0.02-0.08%, and the content of element Sn is controlled to 0.01-0.30%, preferably 0.02-0.25%.
  • Adding an appropriate amount of element Cu to silicon steel can not only form auxiliary inhibitors such as Cu 2 S, but also effectively expand the ⁇ phase region, thereby facilitating the precipitation of other inhibitors.
  • the elemental Cu content in steel should not be too low or too high.
  • the content of element Cu in the grain-oriented silicon steel of the present invention is controlled to 0.01-0.50%, preferably 0.02-0.48%, such as 0.02-0.39%.
  • the oriented silicon steel of Examples 1-12 of the present invention is prepared through the following steps:
  • Nitriding in which the nitriding amount is 50-280ppm.
  • Example 10 and Example 11 also perform normalizing annealing treatment between steps 3) and 4) (the normalizing annealing temperature does not exceed 1000°C, and the normalizing annealing time is 20-200 s. ).
  • Comparative Examples 1-20 adopt similar process steps to prepare grain-oriented silicon steel, and the other comparative examples except Comparative Example 16 also perform normalized annealing treatment between steps 3) and 4).
  • the chemical element composition and process parameters of the oriented silicon steel in Examples 1-12 all meet the scope of protection required by the present invention, while at least one of the chemical element composition and/or process parameters in Comparative Examples 1-20 does not meet the requirements of the present invention. Scope of protection claimed.
  • Table 1 lists the chemical compositions of the grain-oriented silicon steels of Examples 1-12 and Comparative Examples 1-20.
  • step 5 the decarburized annealed steel plates of Examples 1-12 and Comparative Examples 1-20 are sampled, and then the deviation angle of each sample is ⁇ The proportion of 3° Gaussian grains was observed and analyzed.
  • Table 3 lists the proportion of Gaussian grains with deviation angles ⁇ 3° in the decarburized annealed steel plates of Examples 1-12 and Comparative Examples 1-20.
  • the proportion of Gaussian grains with an offset angle ⁇ 3° in the decarburized annealed steel plates of Examples 1-12 is 11%-22%.
  • the proportion of Gaussian grains with an offset angle ⁇ 3° in the decarburized annealed steel plate is 3.6%-9.4%, which is significantly lower than that of Example 1-12.
  • the finished oriented silicon steel products prepared in Examples 1-12 and Comparative Examples 1-20 were sampled, and the magnetic properties of each sample were measured and analyzed to obtain the magnetic induction intensity B8 and magnetostrictive vibration velocity and sound pressure of each oriented silicon steel sample.
  • Level L v A The finished oriented silicon steel products prepared in Examples 1-12 and Comparative Examples 1-20 were sampled, and the magnetic properties of each sample were measured and analyzed to obtain the magnetic induction intensity B8 and magnetostrictive vibration velocity and sound pressure of each oriented silicon steel sample.
  • Magnetic property test According to the national standard GB/T 13789-2008 "Method for measuring the magnetic properties of electrical steel sheets (strips) using a single-chip tester", the magnetic induction intensity of the oriented silicon steel of Examples 1-12 and Comparative Examples 1-20 Make a determination.
  • Table 4 lists the magnetic induction intensity B8 and the magnetostrictive vibration speed sound pressure level L v A of the oriented silicon steels of Examples 1-12 and Comparative Examples 1-20.
  • the magnetic induction intensity B8 of Examples 1-12 is 1.954-1.972T, and the magnetostrictive vibration speed sound pressure level L v A is 43-48dB(A).
  • the magnetic induction intensity B8 of Comparative Example 1-20 is 1.805-1.939T (obviously lower than that of Example 1-12), and the magnetostrictive vibration speed sound pressure level L v A is 51-64dB(A) (obviously higher than that of Example 1-12). 1-12).
  • the Gaussian grain orientation deviation angle ⁇ has a key influence.
  • the oriented silicon steel produced by the method of the present invention shows a high level of matching of high magnetic induction intensity and low magnetostriction.

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Abstract

Disclosed in the present invention is an oriented silicon steel, comprising, in addition to 90% or more of Fe and inevitable impurities, the following chemical elements in percentages by mass: C: 0.020-0.080%, Si: 2.00-4.50%, Mn: 0.01-0.10%, S ≤0.005%, acid-soluble Al: 0.010-0.040%, N: 0.002-0.015%, Nb: 0.006-0.120%, and at least one selected from P: 0.01-0.10%, Sn: 0.01-0.30%, and Cu: 0.01-0.50%. Further disclosed in the present invention is a manufacturing method for the oriented silicon steel, the method comprising: smelting and casting; heating; hot rolling; cold rolling; decarburization annealing; nitriding; coating of an annealing separant; high-temperature annealing; and coating of an insulating coating and scoring. The oriented silicon steel and the manufacturing method therefor of the present invention are environmentally friendly and low in terms of energy consumption, realize high-level matching between a high magnetic induction intensity and a low magnetostriction, and have very wide application prospects.

Description

一种取向硅钢及其制造方法Oriented silicon steel and its manufacturing method 技术领域Technical field
本发明涉及一种取向硅钢及其制造方法,尤其涉及一种具有低磁致伸缩的取向硅钢及其制造方法。The present invention relates to a oriented silicon steel and a manufacturing method thereof, in particular to a oriented silicon steel with low magnetostriction and a manufacturing method thereof.
背景技术Background technique
取向硅钢是一种以锋锐的{110}<001>位向(即高斯晶粒)为特征的软磁材料。取向硅钢常用于制造变压器铁芯,是制造变压器铁芯的重要功能材料。Grain-oriented silicon steel is a soft magnetic material characterized by sharp {110}<001> orientation (i.e. Gaussian grains). Oriented silicon steel is often used to make transformer cores and is an important functional material for making transformer cores.
在现有技术中,根据磁性能和高斯晶粒取向度的不同,取向硅钢可分为普通取向硅钢(简称CGO)和高磁感取向硅钢(简称Hi-B);相较于CGO硅钢,Hi-B硅钢具有更低的铁损、更高的磁感应强度和更小的磁致伸缩。近年来,随着变压器噪音性能日益得到关注,变压器噪声性能成为生产厂家重点关注的指标。由于取向硅钢的磁致伸缩对变压器的噪声性能具有决定性的影响,因此低磁致伸缩的取向硅钢成为了研究热点。In the existing technology, according to the difference in magnetic properties and Gauss grain orientation, oriented silicon steel can be divided into ordinary oriented silicon steel (referred to as CGO) and high magnetic induction oriented silicon steel (referred to as Hi-B); compared with CGO silicon steel, Hi -B silicon steel has lower iron loss, higher magnetic induction intensity and smaller magnetostriction. In recent years, as the noise performance of transformers has received increasing attention, the noise performance of transformers has become an indicator that manufacturers focus on. Since the magnetostriction of oriented silicon steel has a decisive influence on the noise performance of transformers, low magnetostriction oriented silicon steel has become a research hotspot.
在取向硅钢的生产过程中,现有技术主要通过如下三种技术路线来降低取向硅钢的磁致伸缩:1)提高取向硅钢成品的高斯晶粒取向度;2)降低取向硅钢的成品厚度;以及3)涂覆高张力涂层。这三种技术路线均可降低取向硅钢的磁致伸缩。In the production process of oriented silicon steel, the existing technology mainly reduces the magnetostriction of oriented silicon steel through the following three technical routes: 1) improving the Gauss grain orientation of the finished oriented silicon steel; 2) reducing the finished thickness of the oriented silicon steel; and 3) Apply high tension coating. All three technical routes can reduce the magnetostriction of oriented silicon steel.
CN111748731A(公开于2020年10月9日,“低磁致伸缩取向硅钢及其制造方法”)通过对硅钢基板进行特定条件下的热拉伸和磁性退火,产生由于局部按序结构排列导致局部的磁性不均匀引发的晶粒择优取向(磁畴结构重新排列),使得沿轧制方向的单向磁性各向异性增加(即,180°磁畴壁体积增加,90°磁畴壁体积减少),由此降低取向硅钢成品的90°磁畴体积,从而减小取向硅钢的磁致伸缩,进而降低变压器的整体噪声水平。该申请在如下条件下进行磁性退火:磁性退火温度为750-200℃,磁场方向为轧制方向或横向,磁场大小为直流磁场2500A/m+短时脉冲磁场50000A/m的脉冲场(50ms、1-10Hz)。由此得到的取向硅钢成品的LvA(17/50)<55dB(A)。CN111748731A (published on October 9, 2020, "Low magnetostrictive oriented silicon steel and manufacturing method thereof") produces localized structures due to local sequential structural arrangement by performing thermal stretching and magnetic annealing on the silicon steel substrate under specific conditions. The preferential orientation of the grains caused by magnetic inhomogeneity (rearrangement of the magnetic domain structure) increases the unidirectional magnetic anisotropy along the rolling direction (i.e., the volume of the 180° magnetic domain wall increases and the volume of the 90° magnetic domain wall decreases), This reduces the 90° magnetic domain volume of the finished oriented silicon steel, thereby reducing the magnetostriction of the oriented silicon steel, thereby reducing the overall noise level of the transformer. This application performs magnetic annealing under the following conditions: the magnetic annealing temperature is 750-200°C, the magnetic field direction is the rolling direction or transverse direction, and the magnetic field size is a DC magnetic field of 2500A/m + a pulse field of short-term pulse magnetic field of 50000A/m (50ms, 1 -10Hz). The L v A (17/50) of the finished oriented silicon steel thus obtained is <55dB(A).
CN105220071A(公开于2016年1月6日,“一种低噪音特性取向硅钢及其制造方法”)公开了一种取向硅钢,在取向硅钢基板中0.1%≤Cu≤0.5%、0.01%≤S≤0.05%,并且原子比Cu/S满足:5≤Cu/S≤10。在制造该取向硅钢的过程中,严格控制硅钢表面涂层张力和成品晶粒尺寸大小。由此制成的取向硅钢成品的LvA(17)<55dB(A),由该取向硅钢制成的变压器铁芯所产生的振动小,变压器的整体噪音水平得以降低。 CN105220071A (published on January 6, 2016, "A low-noise characteristic oriented silicon steel and its manufacturing method") discloses a oriented silicon steel. In the oriented silicon steel substrate, 0.1%≤Cu≤0.5%, 0.01%≤S≤ 0.05%, and the atomic ratio Cu/S satisfies: 5≤Cu/S≤10. In the process of manufacturing this oriented silicon steel, the surface coating tension of the silicon steel and the grain size of the finished product are strictly controlled. The L v A(17) of the finished oriented silicon steel made in this way is less than 55dB(A). The vibration generated by the transformer core made of this oriented silicon steel is small, and the overall noise level of the transformer is reduced.
CN107881411A(公开于2018年4月6日,“一种低噪音变压器用低铁损取向硅钢产品及其制造方法”)公开了一种低铁损低噪声的取向硅钢。该申请通过将取向硅钢基板的硅酸镁底层对可见光的垂直反射率R严格控制为40-60%、同时保证硅酸镁底层光泽均匀,来降低铁损和减小磁致伸缩/降低噪音。最终成品的磁致伸缩振动噪音值小于60dB(A),特别适用于变压器。CN107881411A (published on April 6, 2018, "A low-iron loss oriented silicon steel product for low-noise transformers and its manufacturing method") discloses a low-iron loss and low-noise oriented silicon steel. This application reduces iron loss and magnetostriction/reduces noise by strictly controlling the vertical reflectance R of the magnesium silicate bottom layer of the oriented silicon steel substrate to visible light to 40-60%, while ensuring uniform gloss of the magnesium silicate bottom layer. The magnetostrictive vibration noise value of the final product is less than 60dB(A), which is especially suitable for transformers.
由此可见,通过控制90°磁畴分布和涂层张力水平均可在一定程度上降低磁致伸缩。但是,以上两种方法均需要采用外加装备或条件来降低磁致伸缩,并且磁致伸缩降低幅度也不显著。例如,虽然CN111748731A中通过添加磁场来影响90°磁畴可以增加180°磁畴壁体积,但是如果取向硅钢基板本身的高斯织构不够锋锐,则后期通过外加条件来降低磁致伸缩的幅度也相对有限。此外,通过增加涂层张力来细化磁畴的方法也存在同样问题,而且该方法对涂层性能也具有极高的要求。此外,一些现有技术中通过降低硅钢片厚度可在一定程度上降低磁致伸缩。但是,由于硅钢的含硅量较高,将硅钢轧制成更薄厚度的难度会更大,同时还会导致成本增加。It can be seen that magnetostriction can be reduced to a certain extent by controlling the 90° magnetic domain distribution and the coating tension level. However, both of the above methods require the use of additional equipment or conditions to reduce magnetostriction, and the reduction in magnetostriction is not significant. For example, although adding a magnetic field to affect the 90° magnetic domain in CN111748731A can increase the volume of the 180° magnetic domain wall, if the Gaussian texture of the oriented silicon steel substrate itself is not sharp enough, it will be difficult to reduce the amplitude of magnetostriction by adding external conditions later. Relatively limited. In addition, the method of refining magnetic domains by increasing coating tension also has the same problem, and this method also has extremely high requirements on coating performance. In addition, in some existing technologies, magnetostriction can be reduced to a certain extent by reducing the thickness of the silicon steel sheet. However, due to the higher silicon content of silicon steel, rolling silicon steel to a thinner thickness will be more difficult and will also result in increased costs.
因此,现有技术中通过增加涂层张力和降低硅钢厚度来降低磁致伸缩的方法均存在很大局限性。相比之下,通过提高取向硅钢本身的高斯晶粒取向度(例如通过优化化学成分和调整生产工艺来提高取向硅钢成品的高斯晶粒取向度),即降低高斯晶粒的偏离角,由此提高磁感应强度可以从根本上降低取向硅钢的磁致伸缩。此外,在“双碳”战略目标的背景下,节能环保也是目前生产过程的关注重点之一。如何在降低能耗的前提下保证取向硅钢的高质量稳定生产,将成为取向硅钢的重要研发方向之一。Therefore, existing methods of reducing magnetostriction by increasing coating tension and reducing silicon steel thickness have great limitations. In contrast, by improving the Gaussian grain orientation of the oriented silicon steel itself (for example, by optimizing the chemical composition and adjusting the production process to improve the Gaussian grain orientation of the finished oriented silicon steel), that is, by reducing the deviation angle of the Gaussian grains, thus Increasing the magnetic induction intensity can fundamentally reduce the magnetostriction of grain-oriented silicon steel. In addition, in the context of the "double carbon" strategic goal, energy conservation and environmental protection are also one of the current focuses of the production process. How to ensure high-quality and stable production of grain-oriented silicon steel while reducing energy consumption will become one of the important research and development directions for grain-oriented silicon steel.
基于以上原因,本发明人期待开发一种具有低磁致伸缩的新型取向硅钢及其制造方法,通过对取向硅钢的化学成分进行高水平设计、同时对生产工艺进行合理优化,在生产过程绿色、降耗的基础上,从本质上提高取向硅钢的磁感应强度和降低取向硅钢的磁致伸缩(通过降低高斯晶粒的偏离角),由此实现取向硅钢的高磁感应强度和低磁致伸缩的高水平匹配。Based on the above reasons, the inventor hopes to develop a new type of oriented silicon steel with low magnetostriction and its manufacturing method. Through high-level design of the chemical composition of the oriented silicon steel and reasonable optimization of the production process, the production process will be green and On the basis of reducing consumption, it essentially increases the magnetic induction intensity of oriented silicon steel and reduces the magnetostriction of oriented silicon steel (by reducing the deviation angle of Gaussian grains), thus achieving high magnetic induction intensity and low magnetostriction of oriented silicon steel. Level matching.
发明内容Contents of the invention
因此,本发明的主要目的是提供一种取向硅钢及其制造方法,所述取向硅钢具有优异的磁性能匹配(特别是就高磁感应强度和低磁致伸缩而言),同时生产过程中的能源介质消耗大幅降低。Therefore, the main purpose of the present invention is to provide a oriented silicon steel and a manufacturing method thereof, which have excellent magnetic property matching (especially in terms of high magnetic induction intensity and low magnetostriction) while reducing energy consumption during the production process. Media consumption is significantly reduced.
在一方面,本申请提供了一种取向硅钢,所述取向硅钢除包含90%以上的Fe和不可避免的杂质之外,还包含以质量百分比计的如下化学元素: In one aspect, the present application provides a oriented silicon steel, which, in addition to containing more than 90% Fe and unavoidable impurities, also contains the following chemical elements in mass percentage:
C:0.020-0.080%,Si:2.00-4.50%,Mn:0.01-0.10%,S≤0.005%,酸溶性Al:0.010-0.040%,N:0.002-0.015%,Nb:0.006-0.120%,以及选自P:0.01-0.10%、Sn:0.01-0.30%和Cu:0.01-0.50%中的至少一种。C: 0.020-0.080%, Si: 2.00-4.50%, Mn: 0.01-0.10%, S≤0.005%, acid-soluble Al: 0.010-0.040%, N: 0.002-0.015%, Nb: 0.006-0.120%, and At least one selected from the group consisting of P: 0.01-0.10%, Sn: 0.01-0.30%, and Cu: 0.01-0.50%.
优选地,所述取向硅钢包含以质量百分比计的如下化学元素:Preferably, the oriented silicon steel contains the following chemical elements in mass percentage:
C:0.020-0.080%,Si:2.00-4.50%,Mn:0.01-0.10%,S≤0.005%,酸溶性Al:0.010-0.040%,N:0.002-0.015%,Nb:0.006-0.120%,以及选自P:0.01-0.10%、Sn:0.01-0.30%和Cu:0.01-0.50%中的至少一种;余量为Fe和不可避免的杂质。C: 0.020-0.080%, Si: 2.00-4.50%, Mn: 0.01-0.10%, S≤0.005%, acid-soluble Al: 0.010-0.040%, N: 0.002-0.015%, Nb: 0.006-0.120%, and At least one selected from P: 0.01-0.10%, Sn: 0.01-0.30% and Cu: 0.01-0.50%; the balance is Fe and inevitable impurities.
优选地,所述取向硅钢的厚度为0.15-0.30mm。Preferably, the thickness of the oriented silicon steel is 0.15-0.30mm.
优选地,所述取向硅钢的磁感应强度B8>1.95T,磁致伸缩振动速度声压水平LvA<50dB(A)。Preferably, the magnetic induction intensity B8 of the oriented silicon steel is >1.95T, and the magnetostrictive vibration speed sound pressure level L v A <50dB (A).
在另一方面,本申请提供了制造上述取向硅钢的方法,所述方法包括如下步骤:On the other hand, the present application provides a method for manufacturing the above-mentioned oriented silicon steel, the method includes the following steps:
1)对钢水进行冶炼和铸造,制得板坯;1) Smelting and casting molten steel to obtain slab;
2)对板坯进行加热;2) Heating the slab;
3)热轧,包括粗轧、卷取保温和精轧;3) Hot rolling, including rough rolling, coiling and holding and finishing rolling;
4)冷轧;4) Cold rolling;
5)脱碳退火;5) Decarburization annealing;
6)渗氮;6) Nitriding;
7)涂覆退火隔离剂;7) Coating annealing isolating agent;
8)高温退火;8) High temperature annealing;
9)涂覆绝缘涂层和刻痕,制得取向硅钢。9) Apply insulating coating and scoring to prepare oriented silicon steel.
优选地,在步骤1)中,板坯的厚度为180-250mm。Preferably, in step 1), the thickness of the slab is 180-250mm.
优选地,在步骤2)中,板坯的加热温度为900-1150℃。Preferably, in step 2), the heating temperature of the slab is 900-1150°C.
本申请中采用的是进行渗氮处理的后天抑制剂工艺,因此板坯中抑制剂元素含量相对较低。在步骤2)中的加热温度有利于减少能耗、同时获得足量抑制剂。当板坯加热温度低于900℃时,抑制剂元素不能有效固溶;当板坯加热温度高于1150℃时,会增加能耗和加热炉的热负荷。因此,步骤2)中板坯的加热温度优选被控制为900-1150℃。The acquired inhibitor process of nitriding treatment is used in this application, so the content of inhibitor elements in the slab is relatively low. The heating temperature in step 2) is conducive to reducing energy consumption while obtaining a sufficient amount of inhibitor. When the slab heating temperature is lower than 900°C, the inhibitor elements cannot be effectively dissolved; when the slab heating temperature is higher than 1150°C, energy consumption and the heat load of the heating furnace will increase. Therefore, the heating temperature of the slab in step 2) is preferably controlled to 900-1150°C.
优选地,在步骤3)中,粗轧结束后中间坯的厚度为35-50mm。Preferably, in step 3), the thickness of the intermediate billet after rough rolling is 35-50 mm.
优选地,在步骤3)中,粗轧的结束温度高于950℃,卷取温度为800-1050℃、卷取时间为30-200s,以及精轧的开始温度低于1050℃。Preferably, in step 3), the end temperature of rough rolling is higher than 950°C, the coiling temperature is 800-1050°C, the coiling time is 30-200s, and the start temperature of finishing rolling is lower than 1050°C.
本申请将粗轧的结束温度设定为高于950℃,可以确保卷曲温度在800-1050℃、卷取时间为30-200s以及后续精轧的开始温度低于1050℃。在该卷曲温度下,热轧板自身各层在卷取后保温过程中互相加热,因此无需再额外进行加热;并且粗轧和精轧之间的卷取可 以使热轧板的组织再结晶更加充分,同时可以弥散析出部分抑制剂。当卷取温度低于800℃或卷取时间少于30s时,无法实现预期的热轧板的组织再结晶效果;当卷取温度高于1050℃或卷取时间超过200s时,中间坯的晶粒组织和已析出的抑制剂会粗化,对后续组织和高斯织构的发展产生不利影响。因此,优选将热轧过程中的温度和/或时间设置在上述范围内。This application sets the end temperature of rough rolling to higher than 950°C, which can ensure that the curling temperature is 800-1050°C, the coiling time is 30-200s, and the starting temperature of subsequent finishing rolling is lower than 1050°C. At this coiling temperature, the layers of the hot-rolled plate itself heat each other during the heat preservation process after coiling, so no additional heating is needed; and the coiling between rough rolling and finishing rolling can In order to make the structure of the hot-rolled plate more fully recrystallized, at the same time, some inhibitors can be dispersed and precipitated. When the coiling temperature is lower than 800℃ or the coiling time is less than 30s, the expected structural recrystallization effect of the hot rolled plate cannot be achieved; when the coiling temperature is higher than 1050℃ or the coiling time exceeds 200s, the crystallization of the intermediate billet will not be achieved. The granular structure and precipitated inhibitors will coarsen, adversely affecting the development of subsequent tissue and Gaussian texture. Therefore, it is preferable to set the temperature and/or time during hot rolling within the above range.
优选地,在3)热轧步骤与4)冷轧步骤之间进行常化退火处理,常化退火温度不超过1000℃、优选为800-1000℃、更优选为800-980℃,常化退火时间为20-200s。Preferably, normalized annealing treatment is performed between 3) hot rolling step and 4) cold rolling step. The normalized annealing temperature does not exceed 1000°C, preferably 800-1000°C, and more preferably 800-980°C. Normalized annealing The time is 20-200s.
通过进行广泛研究,本发明人出乎意料地发现,如果按照目前现有技术常规地在约1100-1200℃的退火温度下对热轧板进行常化退火,不仅会导致常化板晶粒组织过大,还会导致抑制剂粗化,最终导致磁性能劣化。By conducting extensive research, the inventor unexpectedly found that if the hot-rolled plate is conventionally normalized annealed at an annealing temperature of about 1100-1200°C according to the current existing technology, not only will it result in a normalized plate grain structure If it is too large, it will also cause the inhibitor to coarsen, eventually leading to the deterioration of the magnetic properties.
通过在800-1050℃温度下对粗轧板进行卷取保温,可在后续不进行常化退火处理、或者在不超过1000℃的常化退火温度下进行常化退火处理时,实现脱碳退火后钢板中偏离角<3°的高斯晶粒的数量占比>10%,由此获得具有所需高斯晶粒取向度和磁感应强度的成品取向硅钢。相比之下,如果不对粗轧板进行卷取保温、或者卷取保温后的常化退火温度高于1000℃,则脱碳退火后钢板中偏离角<3°的高斯晶粒的数量占比会显著降低(即显著低于10%)。By coiling and insulating the rough rolled plate at a temperature of 800-1050°C, decarburization annealing can be achieved without subsequent normalization annealing treatment, or when normalization annealing treatment is performed at a normalization annealing temperature not exceeding 1000°C. The number of Gaussian grains with an offset angle of <3° in the final steel plate accounts for >10%, thereby obtaining a finished oriented silicon steel with the required Gaussian grain orientation and magnetic induction intensity. In contrast, if the rough rolled plate is not coiled and insulated, or the normalized annealing temperature after coiling and insulating is higher than 1000°C, the proportion of Gaussian grains with an offset angle of <3° in the steel plate after decarburization annealing will be significantly reduced (i.e. significantly less than 10%).
优选地,在步骤4)中,冷轧压下率>80%。Preferably, in step 4), the cold rolling reduction ratio is >80%.
优选地,在步骤5)中,脱碳退火温度为800-900℃。当脱碳退火温度低于800℃时,会导致脱碳效果不明显;当脱碳退火温度高于900℃时,会导致初次再结晶晶粒过于粗大,影响二次再结晶。Preferably, in step 5), the decarburization annealing temperature is 800-900°C. When the decarburization annealing temperature is lower than 800°C, the decarburization effect will be insignificant; when the decarburization annealing temperature is higher than 900°C, the primary recrystallization grains will be too coarse, affecting the secondary recrystallization.
优选地,在步骤5)中,脱碳退火后钢板中偏离角<3°的高斯晶粒的比例>10%。在本文中,“脱碳退火后钢板中偏离角<3°的高斯晶粒的比例”是指偏离角<3°的高斯晶粒的数量与高斯晶粒总数量的比值(以%计)。Preferably, in step 5), the proportion of Gaussian grains with an offset angle of <3° in the steel plate after decarburization annealing is >10%. In this article, "the proportion of Gaussian grains with an offset angle <3° in the steel plate after decarburization annealing" refers to the ratio (in %) of the number of Gaussian grains with an offset angle <3° to the total number of Gaussian grains.
在本文中,“偏离角”指高斯晶粒取向偏离角。高斯晶粒的偏离角和比例通过带有电子背散射衍射(EBSD)系统的扫描电子显微镜进行观察和统计。As used herein, "deviation angle" refers to the Gaussian grain orientation deviation angle. The deviation angle and proportion of Gaussian grains were observed and counted by a scanning electron microscope with an electron backscatter diffraction (EBSD) system.
优选地,在步骤6)中,渗氮量为50-280ppm。Preferably, in step 6), the nitriding amount is 50-280 ppm.
本申请中采用的是进行渗氮处理的后天抑制剂工艺。换言之,在高温退火之前必须进行渗氮处理,以形成满足抑制初次再结晶晶粒长大的抑制剂。当渗氮量低于50ppm时,抑制剂形成数量不足;当渗氮量高于280ppm时,会对高温退火过程中硅酸镁底层的形成有不良影响。基于这些考虑,本发明步骤6)中的渗氮量被严格控制为50-280ppm。What is used in this application is the acquired inhibitor process of nitriding treatment. In other words, nitriding treatment must be performed before high-temperature annealing to form an inhibitor that is sufficient to inhibit the growth of primary recrystallized grains. When the nitriding amount is lower than 50ppm, the amount of inhibitors formed is insufficient; when the nitriding amount is higher than 280ppm, it will have a negative impact on the formation of the magnesium silicate bottom layer during high-temperature annealing. Based on these considerations, the nitriding amount in step 6) of the present invention is strictly controlled to 50-280 ppm.
在步骤7)中,退火隔离剂可使用本领域常用的退火隔离剂,优选为MgO。In step 7), the annealing isolating agent can be an annealing isolating agent commonly used in the art, preferably MgO.
优选地,在步骤8)中,退火温度为1100-1250℃,退火时间大于25小时。 Preferably, in step 8), the annealing temperature is 1100-1250°C, and the annealing time is greater than 25 hours.
在步骤9)中,可使用本领域常用的涂液来形成绝缘涂层,例如通过涂覆含有磷酸盐、胶态二氧化硅和铬酐的涂液来形成绝缘涂层;刻痕可使用本领域常用的刻痕方法,例如激光刻痕、电化学刻痕、齿辊刻痕、高压水束刻痕等。In step 9), the insulating coating can be formed using a coating liquid commonly used in the art, for example, by coating a coating liquid containing phosphate, colloidal silica and chromic anhydride; the insulating coating can be formed using this method for scoring. Commonly used scoring methods in the field, such as laser scoring, electrochemical scoring, toothed roller scoring, high-pressure water beam scoring, etc.
相比于现有技术,本发明所述的取向硅钢及其制造方法实现了如下有益效果:Compared with the existing technology, the oriented silicon steel and its manufacturing method of the present invention achieve the following beneficial effects:
本发明人通过大量实验发现,初次再结晶中高斯晶粒晶核取向度对成品高斯晶粒取向度和磁感应强度有决定性影响。因此,本发明人通过对相关工艺参数进行优化设计,使得脱碳退火后钢板中偏离角<3°的高斯晶粒的比例>10%,由此获得了具有所需高斯晶粒取向度和磁感应强度的成品取向硅钢。The inventor found through a large number of experiments that the orientation of the Gaussian grain nuclei in the primary recrystallization has a decisive influence on the orientation of the Gaussian grains and the magnetic induction intensity of the finished product. Therefore, the inventor optimized the design of the relevant process parameters so that the proportion of Gaussian grains with deviation angles <3° in the steel plate after decarburization annealing was >10%, thereby obtaining the required Gaussian grain orientation and magnetic induction. Finished grain oriented silicon steel for strength.
本发明在环保降耗的生产过程的前提下,获得了高磁感应强度和低磁致伸缩高水平匹配的取向硅钢。本发明所述的取向硅钢的磁性能优异(磁感应强度B8>1.95T,磁致伸缩振动速度声压水平LvA<50dB(A)),具有良好的经济效益和应用前景。On the premise of an environmentally friendly and consumption-reducing production process, the present invention obtains oriented silicon steel that matches high magnetic induction intensity and low magnetostriction at a high level. The oriented silicon steel of the present invention has excellent magnetic properties (magnetic induction intensity B8>1.95T, magnetostrictive vibration speed sound pressure level L v A<50dB(A)), and has good economic benefits and application prospects.
具体实施方式Detailed ways
通过进行广泛研究,本发明人意外地发现,通过如上所述地对取向硅钢的化学组成进行设计,可获得综合性能优异(特别是高磁感应强度和低磁致伸缩)的取向硅钢。具体而言,上述各化学元素的设计原理如下。在本文中,除非另外明确地说明,否则元素含量以质量百分比计。Through extensive research, the inventor unexpectedly discovered that by designing the chemical composition of oriented silicon steel as described above, oriented silicon steel with excellent comprehensive properties (especially high magnetic induction intensity and low magnetostriction) can be obtained. Specifically, the design principles of each of the above chemical elements are as follows. In this article, elemental contents are expressed in mass percent unless otherwise explicitly stated.
C:添加适量的元素C能够确保在热轧或者常化过程中获得适当比例的γ相,有利于细小弥散抑制剂的析出。当钢中元素C含量低于0.020%时,γ相的比例较低,不利于抑制剂的析出;当钢中元素C含量高于0.080%时,则会增加脱碳成本。基于这些考虑,本发明所述的取向硅钢中元素C的含量被控制为0.020-0.080%,优选0.022-0.073%。C: Adding an appropriate amount of element C can ensure that an appropriate proportion of γ phase is obtained during hot rolling or normalization, which is conducive to the precipitation of fine dispersion inhibitors. When the element C content in the steel is lower than 0.020%, the proportion of γ phase is low, which is not conducive to the precipitation of inhibitors; when the element C content in the steel is higher than 0.080%, the decarburization cost will increase. Based on these considerations, the content of element C in the oriented silicon steel of the present invention is controlled to 0.020-0.080%, preferably 0.022-0.073%.
Si:元素Si是降低铁损的主要元素。为了确保成品硅钢的质量,钢中元素Si含量不宜过低或过高。当硅钢中元素Si含量低于2.00%时,所得取向硅钢难以获得所需的低铁损;当钢中元素Si含量高于4.50%,则会导致冷轧困难、降低成材率。基于这些考虑,本发明所述的取向硅钢中元素Si的含量被控制为2.00-4.50%,优选2.19-4.29%。Si: Element Si is the main element that reduces iron loss. In order to ensure the quality of finished silicon steel, the element Si content in the steel should not be too low or too high. When the element Si content in silicon steel is less than 2.00%, it is difficult for the resulting oriented silicon steel to obtain the required low iron loss; when the element Si content in the steel is higher than 4.50%, cold rolling will be difficult and the yield rate will be reduced. Based on these considerations, the content of element Si in the oriented silicon steel of the present invention is controlled to 2.00-4.50%, preferably 2.19-4.29%.
Mn:添加适量的元素Mn可在连铸和热轧过程中形成少量MnS辅助抑制剂,可有效改善取向硅钢的微观组织和轧制性。为了确保取向硅钢的性能,必须严格控制钢中元素Mn的含量。当Mn含量低于0.01%时,不利于获得所需的硅钢微观组织和轧制性;当Mn含量高于0.10%时,板坯加热温度将会显著提高,且容易形成粗大MnS抑制剂。基于这些考虑,本发明所述的取向硅钢中元素Mn的含量被控制为0.01-0.10%,优选0.01-0.09%。 Mn: Adding an appropriate amount of element Mn can form a small amount of MnS auxiliary inhibitor during continuous casting and hot rolling, which can effectively improve the microstructure and rollability of grain-oriented silicon steel. In order to ensure the performance of grain-oriented silicon steel, the content of element Mn in the steel must be strictly controlled. When the Mn content is lower than 0.01%, it is not conducive to obtaining the required silicon steel microstructure and rolling properties; when the Mn content is higher than 0.10%, the slab heating temperature will increase significantly, and coarse MnS inhibitors will easily form. Based on these considerations, the content of element Mn in the oriented silicon steel of the present invention is controlled to 0.01-0.10%, preferably 0.01-0.09%.
S:元素S能形成MnS、Cu2S等辅助抑制剂。但需要注意,钢中元素S含量不宜过高。当钢中元素S含量过高时,会显著增加板坯加热温度,不利于生产。基于这些考虑,本发明所述的取向硅钢中元素S的含量被控制为S≤0.005%,优选≤0.004%。S: Element S can form auxiliary inhibitors such as MnS and Cu 2 S. However, it should be noted that the content of element S in steel should not be too high. When the element S content in steel is too high, it will significantly increase the slab heating temperature, which is not conducive to production. Based on these considerations, the content of element S in the grain-oriented silicon steel of the present invention is controlled to S≤0.005%, preferably ≤0.004%.
酸溶性Al:酸溶性Al是形成主要抑制剂AlN的重要成分。当钢中酸溶性Al含量低于0.010%时,会导致抑制剂不足;当钢中酸溶性Al含量高于0.040%时,会导致抑制剂AlN粗大。因此,需要严格控制硅钢中酸溶性Al的含量。基于这些考虑,本发明所述的取向硅钢中酸溶性Al的含量被控制为0.010-0.040%,优选0.012-0.039%。Acid-soluble Al: Acid-soluble Al is an important component in forming the main inhibitor AlN. When the acid-soluble Al content in the steel is lower than 0.010%, the inhibitor will be insufficient; when the acid-soluble Al content in the steel is higher than 0.040%, the inhibitor AlN will be coarse. Therefore, the content of acid-soluble Al in silicon steel needs to be strictly controlled. Based on these considerations, the content of acid-soluble Al in the oriented silicon steel of the present invention is controlled to 0.010-0.040%, preferably 0.012-0.039%.
N:添加适量的元素N可以适当地抑制晶粒长大。硅钢中添加的元素N能够配合酸溶性Al在渗氮前形成AlN,从而有效抑制初次再结晶晶粒的长大。当钢中元素N含量低于0.002%时,不能有效抑制初次再结晶晶粒的长大;当钢中元素N含量高于0.015%时,会显著增加炼钢难度。基于这些考虑,本发明所述的取向硅钢中元素N的含量被控制为0.002-0.015%,优选0.003-0.014%。N: Adding an appropriate amount of element N can appropriately suppress grain growth. The element N added to silicon steel can cooperate with acid-soluble Al to form AlN before nitriding, thereby effectively inhibiting the growth of primary recrystallized grains. When the element N content in steel is lower than 0.002%, the growth of primary recrystallized grains cannot be effectively suppressed; when the element N content in steel is higher than 0.015%, it will significantly increase the difficulty of steelmaking. Based on these considerations, the content of element N in the oriented silicon steel of the present invention is controlled to 0.002-0.015%, preferably 0.003-0.014%.
Nb:为了降低板坯加热温度,元素Mn、Cu的含量相对较低,但这会导致MnS和Cu2S的析出不足。因此,为了弥补抑制剂的抑制能力不足的问题,硅钢中加入了适量元素Nb。元素Nb能够形成辅助抑制剂Nb(C,N),起到辅助抑制剂的作用。此外,由于Nb(C,N)固溶温度相对较低,还可以起到降低板坯加热温度的作用。当钢中元素Nb含量低于0.006%时,形成的抑制剂Nb(C,N)不能充分发挥抑制作用;当钢中元素Nb含量高于0.120%时,由于抑制作用太强而阻碍二次再结晶的发生。基于这些考虑,本发明所述的取向硅钢中元素Nb的含量被控制为0.006-0.120%,优选0.006-0.118%。Nb: In order to reduce the slab heating temperature, the content of elements Mn and Cu is relatively low, but this will lead to insufficient precipitation of MnS and Cu 2 S. Therefore, in order to make up for the problem of insufficient inhibitory ability of inhibitors, an appropriate amount of element Nb is added to silicon steel. Element Nb can form an auxiliary inhibitor Nb(C,N) and play the role of an auxiliary inhibitor. In addition, since the solid solution temperature of Nb(C,N) is relatively low, it can also reduce the slab heating temperature. When the element Nb content in the steel is lower than 0.006%, the inhibitor Nb(C,N) formed cannot fully exert its inhibitory effect; when the element Nb content in the steel is higher than 0.120%, the inhibitory effect is too strong and hinders the secondary recycling. Crystallization occurs. Based on these considerations, the content of element Nb in the oriented silicon steel of the present invention is controlled to 0.006-0.120%, preferably 0.006-0.118%.
P和Sn:元素P和Sn均为晶界偏析元素,硅钢中添加适量元素P和Sn可以起到辅助抑制剂的作用。当钢中元素P和Sn含量各自低于0.01%时,不能充分发挥辅助抑制的作用;当钢中元素P和Sn含量分别高于0.10%和0.30%时,会对脱碳和渗氮产生不利影响。基于这些考虑,本发明所述的取向硅钢中元素P的含量被控制为0.01-0.10%、优选0.02-0.08%,元素Sn的含量被控制为0.01-0.30%、优选0.02-0.25%。P and Sn: The elements P and Sn are both grain boundary segregation elements. Adding appropriate amounts of elements P and Sn to silicon steel can act as auxiliary inhibitors. When the content of the elements P and Sn in the steel is less than 0.01% respectively, the auxiliary inhibitory effect cannot be fully exerted; when the content of the elements P and Sn in the steel is higher than 0.10% and 0.30% respectively, it will be detrimental to decarburization and nitriding. Influence. Based on these considerations, the content of element P in the grain-oriented silicon steel of the present invention is controlled to 0.01-0.10%, preferably 0.02-0.08%, and the content of element Sn is controlled to 0.01-0.30%, preferably 0.02-0.25%.
Cu:硅钢中添加适量的元素Cu不仅可以形成Cu2S等辅助抑制剂,还可以有效扩大γ相区,从而有利于其他抑制剂的析出。但需要注意,钢中元素Cu含量不宜过低或过高。当硅钢中元素Cu含量低于0.01%时,不能充分发挥上述作用;当硅钢中元素Cu含量高于0.50%时,会增加生产成本。基于这些考虑,本发明所述的取向硅钢中元素Cu的含量被控制为0.01-0.50%,优选0.02-0.48%,例如0.02-0.39%。Cu: Adding an appropriate amount of element Cu to silicon steel can not only form auxiliary inhibitors such as Cu 2 S, but also effectively expand the γ phase region, thereby facilitating the precipitation of other inhibitors. However, it should be noted that the elemental Cu content in steel should not be too low or too high. When the element Cu content in silicon steel is less than 0.01%, the above effects cannot be fully exerted; when the element Cu content in silicon steel is higher than 0.50%, production costs will increase. Based on these considerations, the content of element Cu in the grain-oriented silicon steel of the present invention is controlled to 0.01-0.50%, preferably 0.02-0.48%, such as 0.02-0.39%.
下面将结合具体实施例来对本发明所述的取向硅钢及其制造方法进行进一步的解释和说明。然而,以下描述是用于解释本发明的说明性描述,而不意在将本发明的技术范围仅限于该描述范围。 The oriented silicon steel and its manufacturing method according to the present invention will be further explained and described below with reference to specific examples. However, the following description is an illustrative description for explaining the present invention and is not intended to limit the technical scope of the present invention to the description range.
实施例1-12Examples 1-12
本发明的实施例1-12的取向硅钢通过如下步骤制得:The oriented silicon steel of Examples 1-12 of the present invention is prepared through the following steps:
1)根据下表1所示的配方,对钢水进行冶炼和铸造,制得厚度为180-250mm的板坯。1) According to the formula shown in Table 1 below, smelt and cast the molten steel to obtain a slab with a thickness of 180-250mm.
2)在900-1150℃温度下对板坯进行加热。2) Heat the slab at a temperature of 900-1150°C.
3)对板坯进行粗轧、卷取保温和精轧:粗轧的结束温度高于950℃,卷取温度为800-1050℃、卷取时间为30-200s,精轧的开始温度低于1050℃。3) Carry out rough rolling, coiling insulation and finish rolling on the slab: the end temperature of rough rolling is higher than 950℃, the coiling temperature is 800-1050℃, the coiling time is 30-200s, and the starting temperature of finish rolling is lower than 1050℃.
4)冷轧至0.15-0.30mm的成品板厚,其中冷轧压下率>80%。4) Cold rolling to a finished plate thickness of 0.15-0.30mm, where the cold rolling reduction ratio is >80%.
5)在800-900℃温度下进行脱碳退火。5) Carry out decarburization annealing at a temperature of 800-900°C.
6)渗氮,其中渗氮量为50-280ppm。6) Nitriding, in which the nitriding amount is 50-280ppm.
7)涂覆退火隔离剂。7) Apply annealing release agent.
8)高温退火,其中退火温度为1100-1250℃、退火时间大于25小时。8) High temperature annealing, where the annealing temperature is 1100-1250°C and the annealing time is greater than 25 hours.
9)涂覆绝缘涂层和刻痕,制得取向硅钢,厚度为0.15-0.30mm。9) Apply insulating coating and scoring to prepare oriented silicon steel with a thickness of 0.15-0.30mm.
需要注意,除实施例10和实施例11之外的其他实施例在步骤3)和4)之间还进行常化退火处理(常化退火温度不超过1000℃、常化退火时间为20-200s)。It should be noted that other embodiments except Example 10 and Example 11 also perform normalizing annealing treatment between steps 3) and 4) (the normalizing annealing temperature does not exceed 1000°C, and the normalizing annealing time is 20-200 s. ).
比较例1-20Comparative Example 1-20
比较例1-20采用类似工艺步骤来制备取向硅钢,其中除比较例16之外的其他比较例在步骤3)和4)之间还进行常化退火处理。但是,实施例1-12的取向硅钢的化学元素组成和工艺参数均满足本发明要求保护的范围,而比较例1-20中的化学元素组成和/或工艺参数中的至少一个不满足本发明要求保护的范围。Comparative Examples 1-20 adopt similar process steps to prepare grain-oriented silicon steel, and the other comparative examples except Comparative Example 16 also perform normalized annealing treatment between steps 3) and 4). However, the chemical element composition and process parameters of the oriented silicon steel in Examples 1-12 all meet the scope of protection required by the present invention, while at least one of the chemical element composition and/or process parameters in Comparative Examples 1-20 does not meet the requirements of the present invention. Scope of protection claimed.
表1中列出了实施例1-12和比较例1-20的取向硅钢的化学组成。 Table 1 lists the chemical compositions of the grain-oriented silicon steels of Examples 1-12 and Comparative Examples 1-20.
表1(wt%,余量为Fe和不可避免的杂质)
Table 1 (wt%, balance is Fe and inevitable impurities)
表2-1和表2-2中列出了实施例1-12和比较例1-20在上述工艺步骤中的具体工艺参数。 The specific process parameters in the above process steps of Examples 1-12 and Comparative Examples 1-20 are listed in Table 2-1 and Table 2-2.
表2-1
table 2-1
表2-2
Table 2-2
在步骤5)中,对实施例1-12和比较例1-20的脱碳退火后钢板进行取样,然后通过带有电子背散射衍射(EBSD)系统的扫描电子显微镜对各个样品的偏离角<3°的高斯晶粒的占比情况进行观察和分析。 In step 5), the decarburized annealed steel plates of Examples 1-12 and Comparative Examples 1-20 are sampled, and then the deviation angle of each sample is < The proportion of 3° Gaussian grains was observed and analyzed.
表3中列出了实施例1-12和比较例1-20的脱碳退火后钢板中偏离角<3°的高斯晶粒的比例。Table 3 lists the proportion of Gaussian grains with deviation angles <3° in the decarburized annealed steel plates of Examples 1-12 and Comparative Examples 1-20.
表3
table 3
如表3所示,实施例1-12的脱碳退火后钢板中偏离角<3°的高斯晶粒的比例为11%-22%。而比较例1-20的脱碳退火后钢板中偏离角<3°的高斯晶粒的比例为3.6%-9.4%,显著低于实施例1-12。As shown in Table 3, the proportion of Gaussian grains with an offset angle <3° in the decarburized annealed steel plates of Examples 1-12 is 11%-22%. In Comparative Example 1-20, the proportion of Gaussian grains with an offset angle <3° in the decarburized annealed steel plate is 3.6%-9.4%, which is significantly lower than that of Example 1-12.
对实施例1-12和比较例1-20中制得的取向硅钢成品进行取样,对各个样品的磁性能进行测定和分析,得到各个取向硅钢样品的磁感应强度B8和磁致伸缩振动速度声压水平LvA。The finished oriented silicon steel products prepared in Examples 1-12 and Comparative Examples 1-20 were sampled, and the magnetic properties of each sample were measured and analyzed to obtain the magnetic induction intensity B8 and magnetostrictive vibration velocity and sound pressure of each oriented silicon steel sample. Level L v A.
在本文中,取向硅钢的相关磁性能测试方法如下所述:In this article, the relevant magnetic property testing methods of grain-oriented silicon steel are as follows:
磁性能测试:根据国家标准GB/T 13789-2008“用单片测试仪测量电工钢片(带)磁性能的方法”,对实施例1-12和比较例1-20的取向硅钢的磁感应强度进行测定。Magnetic property test: According to the national standard GB/T 13789-2008 "Method for measuring the magnetic properties of electrical steel sheets (strips) using a single-chip tester", the magnetic induction intensity of the oriented silicon steel of Examples 1-12 and Comparative Examples 1-20 Make a determination.
磁致伸缩测试:根据IEC技术报告IEC/TP 62581,采用非接触式的激光多普勒振动仪,在B=1.7T、f=2MPa(在变压器的实际工况中,取向硅钢经受的压应力为2-3MPa)条件下,对实施例1-12和比较例1-20的取向硅钢的磁致伸缩振动速度声压水平LvA进行测定。在本文中,LvA是指取向硅钢在上述测试条件下的磁致伸缩振动速度声压水平,单位为dB(A)。Magnetostriction test: According to IEC technical report IEC/TP 62581, using a non-contact laser Doppler vibrometer, the compressive stress experienced by oriented silicon steel is at B=1.7T, f=2MPa (in the actual working conditions of the transformer) Under the condition of 2-3MPa), the magnetostrictive vibration velocity and sound pressure level L v A of the oriented silicon steels of Examples 1-12 and Comparative Examples 1-20 were measured. In this article, L v A refers to the magnetostrictive vibration velocity sound pressure level of oriented silicon steel under the above test conditions, in dB(A).
表4中列出了实施例1-12和比较例1-20的取向硅钢的磁感应强度B8和磁致伸缩振动速度声压水平LvA。 Table 4 lists the magnetic induction intensity B8 and the magnetostrictive vibration speed sound pressure level L v A of the oriented silicon steels of Examples 1-12 and Comparative Examples 1-20.
表4
Table 4
如表4所示,实施例1-12的磁感应强度B8为1.954-1.972T,磁致伸缩振动速度声压水平LvA为43-48dB(A)。而比较例1-20的磁感应强度B8为1.805-1.939T(显然低于实施例1-12),磁致伸缩振动速度声压水平LvA为51-64dB(A)(显然高于实施例1-12)。 As shown in Table 4, the magnetic induction intensity B8 of Examples 1-12 is 1.954-1.972T, and the magnetostrictive vibration speed sound pressure level L v A is 43-48dB(A). The magnetic induction intensity B8 of Comparative Example 1-20 is 1.805-1.939T (obviously lower than that of Example 1-12), and the magnetostrictive vibration speed sound pressure level L v A is 51-64dB(A) (obviously higher than that of Example 1-12). 1-12).
由表1-表4可以看出,实施例1-12的脱碳退火后钢板中偏离角<3°的高斯晶粒的比例明显高于比较例1-20,其磁性能(特别是磁感应强度B8和LvA)显著优于比较例1-20。It can be seen from Tables 1 to 4 that the proportion of Gaussian grains with deviation angles <3° in the decarburized annealed steel plates of Examples 1-12 is significantly higher than that of Comparative Examples 1-20, and its magnetic properties (especially magnetic induction intensity B8 and L v A) are significantly better than Comparative Examples 1-20.
本发明人在对脱碳退火后钢板中偏离角<3°的高斯晶粒的比例进行分析后出乎意料地发现:不同的热轧和常化退火工艺参数的组合对脱碳退火后钢板中高斯晶粒取向偏离角α具有关键影响。尤其是当在本发明要求的化学元素组成范围内,通过在800-1050℃温度下对粗轧板进行卷取保温,在后续进行低温常化退火(常化退火温度不超过1000℃)、甚至不进行常化退火处理时,能显著提高脱碳退火后钢板中偏离角<3°的高斯晶粒的比例。本发明人通过大量实验发现,初次再结晶中高斯晶粒晶核取向度对成品高斯晶粒取向度和磁感应强度有决定性影响。因此,通过本发明方法制造的取向硅钢显示出高磁感应强度和低磁致伸缩的高水平匹配。After analyzing the proportion of Gaussian grains with deviation angles <3° in the decarburized annealed steel plate, the inventor unexpectedly found that different combinations of hot rolling and normalized annealing process parameters have an impact on the decarburized annealed steel plate. The Gaussian grain orientation deviation angle α has a key influence. Especially when it is within the chemical element composition range required by the present invention, by coiling and insulating the rough rolled plate at a temperature of 800-1050°C, and subsequently performing low-temperature normalized annealing (the normalized annealing temperature does not exceed 1000°C), or even Without normalizing annealing treatment, the proportion of Gaussian grains with deviation angles <3° in the steel plate after decarburization annealing can be significantly increased. The inventor found through a large number of experiments that the orientation of the Gaussian grain nuclei in the primary recrystallization has a decisive influence on the orientation of the Gaussian grains and the magnetic induction intensity of the finished product. Therefore, the oriented silicon steel produced by the method of the present invention shows a high level of matching of high magnetic induction intensity and low magnetostriction.
需要注意,本申请中记载的所有技术特征可以以任何方式进行自由组合或结合,除非彼此之间产生矛盾。在不脱离本发明的范围的情况下可对本发明进行各种修改和变化,这对本领域技术人员而言将是显而易见的。例如,作为一个实施方式的一部分显示或描述的特征可以与另一个实施方式一起使用以产生又一个实施方式。因此,本发明旨在涵盖落入所附权利要求及其等价物范围内的这些修改和变化。 It should be noted that all technical features recorded in this application can be freely combined or combined in any way, unless they conflict with each other. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope of the invention. For example, features shown or described as part of one embodiment can be used with another embodiment to produce yet a still further embodiment. Thus, it is intended that the present invention cover the modifications and variations provided they come within the scope of the appended claims and their equivalents.

Claims (11)

  1. 一种取向硅钢,其特征在于,所述取向硅钢除包含90%以上的Fe和不可避免的杂质之外,还包含以质量百分比计的如下化学元素:A kind of oriented silicon steel, characterized in that, in addition to containing more than 90% Fe and inevitable impurities, the oriented silicon steel also contains the following chemical elements in mass percentage:
    C:0.020-0.080%,Si:2.00-4.50%,Mn:0.01-0.10%,S≤0.005%,酸溶性Al:0.010-0.040%,N:0.002-0.015%,Nb:0.006-0.120%,以及选自P:0.01-0.10%、Sn:0.01-0.30%和Cu:0.01-0.50%中的至少一种。C: 0.020-0.080%, Si: 2.00-4.50%, Mn: 0.01-0.10%, S≤0.005%, acid-soluble Al: 0.010-0.040%, N: 0.002-0.015%, Nb: 0.006-0.120%, and At least one selected from the group consisting of P: 0.01-0.10%, Sn: 0.01-0.30%, and Cu: 0.01-0.50%.
  2. 根据权利要求1所述的取向硅钢,其特征在于,所述取向硅钢包含以质量百分比计的如下化学元素:The oriented silicon steel according to claim 1, characterized in that the oriented silicon steel contains the following chemical elements in mass percentage:
    C:0.020-0.080%,Si:2.00-4.50%,Mn:0.01-0.10%,S≤0.005%,酸溶性Al:0.010-0.040%,N:0.002-0.015%,Nb:0.006-0.120%,以及选自P:0.01-0.10%、Sn:0.01-0.30%和Cu:0.01-0.50%中的至少一种;余量为Fe和不可避免的杂质。C: 0.020-0.080%, Si: 2.00-4.50%, Mn: 0.01-0.10%, S≤0.005%, acid-soluble Al: 0.010-0.040%, N: 0.002-0.015%, Nb: 0.006-0.120%, and At least one selected from P: 0.01-0.10%, Sn: 0.01-0.30% and Cu: 0.01-0.50%; the balance is Fe and inevitable impurities.
  3. 根据权利要求1或2所述的取向硅钢,其特征在于,所述取向硅钢的厚度为0.15-0.30mm;优选地,所述取向硅钢的磁感应强度B8>1.95 T,磁致伸缩振动速度声压水平LvA<50dB(A)。The oriented silicon steel according to claim 1 or 2, characterized in that the thickness of the oriented silicon steel is 0.15-0.30mm; preferably, the magnetic induction intensity B8 of the oriented silicon steel>1.95 T, the magnetostrictive vibration speed sound pressure Level L v A<50dB(A).
  4. 制造权利要求1-3中任一项所述的取向硅钢的方法,所述方法包括如下步骤:The method for manufacturing the oriented silicon steel according to any one of claims 1-3, the method includes the following steps:
    1)对钢水进行冶炼和铸造,制得板坯;1) Smelting and casting molten steel to obtain slab;
    2)对板坯进行加热;2) Heating the slab;
    3)热轧,包括粗轧、卷取保温和精轧;3) Hot rolling, including rough rolling, coiling and holding and finishing rolling;
    4)冷轧;4) Cold rolling;
    5)脱碳退火;5) Decarburization annealing;
    6)渗氮;6) Nitriding;
    7)涂覆退火隔离剂;7) Coating annealing isolating agent;
    8)高温退火;8) High temperature annealing;
    9)涂覆绝缘涂层和刻痕,制得取向硅钢。9) Apply insulating coating and scoring to prepare oriented silicon steel.
  5. 根据权利要求4所述的方法,其特征在于,在步骤3)中,粗轧的结束温度高于950℃,卷取温度为800-1050℃、卷取时间为30-200s,精轧的开始温度低于1050℃。The method according to claim 4, characterized in that in step 3), the end temperature of rough rolling is higher than 950°C, the coiling temperature is 800-1050°C, the coiling time is 30-200s, and the finish rolling starts The temperature is lower than 1050℃.
  6. 根据权利要求4所述的方法,其特征在于,在步骤3)之后、步骤4)之前进行常化退火处理,常化退火温度不超过1000℃、优选为800-1000℃、更优选为800-980℃,常化退火时间为20-200s。The method according to claim 4, characterized in that a normalized annealing treatment is performed after step 3) and before step 4), and the normalized annealing temperature does not exceed 1000°C, preferably 800-1000°C, and more preferably 800-800°C. 980℃, normalized annealing time is 20-200s.
  7. 根据权利要求4-6中任一项所述的方法,其特征在于,在步骤2)中,板坯的加热温度为900-1150℃。 The method according to any one of claims 4 to 6, characterized in that in step 2), the heating temperature of the slab is 900-1150°C.
  8. 根据权利要求4-6中任一项所述的方法,其特征在于,所述方法满足如下条件中的一个以上:The method according to any one of claims 4-6, characterized in that the method satisfies more than one of the following conditions:
    在步骤1)中,板坯的厚度为180-250mm;In step 1), the thickness of the slab is 180-250mm;
    在步骤3)中,粗轧结束后中间坯的厚度为35-50mm;In step 3), the thickness of the intermediate billet after rough rolling is 35-50mm;
    在步骤4)中,冷轧压下率>80%;以及In step 4), the cold rolling reduction ratio is >80%; and
    在步骤7)中,退火隔离剂为MgO。In step 7), the annealing isolating agent is MgO.
  9. 根据权利要求4-6中任一项所述的方法,其特征在于,在步骤5)中,脱碳退火温度为800-900℃;优选地,脱碳退火后钢板中偏离角<3°的高斯晶粒的比例>10%。The method according to any one of claims 4 to 6, characterized in that in step 5), the decarburization annealing temperature is 800-900°C; preferably, the deviation angle in the steel plate after decarburization annealing is <3°. The proportion of Gaussian grains is >10%.
  10. 根据权利要求4-6中任一项所述的方法,其特征在于,在步骤6)中,渗氮量为50-280ppm。The method according to any one of claims 4-6, characterized in that in step 6), the nitriding amount is 50-280 ppm.
  11. 根据权利要求4-6中任一项所述的方法,其特征在于,在步骤8)中,退火温度为1100-1250℃,退火时间大于25小时。 The method according to any one of claims 4 to 6, characterized in that in step 8), the annealing temperature is 1100-1250°C, and the annealing time is greater than 25 hours.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02258926A (en) * 1989-03-30 1990-10-19 Nippon Steel Corp Production of grain-oriented silicon steel sheet having high magnetic flux density
CN102443736A (en) * 2010-09-30 2012-05-09 宝山钢铁股份有限公司 Method for producing high magnetic flux-density oriented silicon steel product
CN103805918A (en) * 2012-11-15 2014-05-21 宝山钢铁股份有限公司 High-magnetic induction oriented silicon steel and production method thereof
CN104561795A (en) * 2014-12-12 2015-04-29 武汉钢铁(集团)公司 High magnetic induction grain-oriented silicon steel with B800 being more than or equal to 1.94T and production method thereof
CN112391512A (en) * 2019-08-13 2021-02-23 宝山钢铁股份有限公司 High magnetic induction oriented silicon steel and manufacturing method thereof
CN114277309A (en) * 2020-09-27 2022-04-05 宝山钢铁股份有限公司 High magnetic induction oriented silicon steel and manufacturing method thereof
CN114277308A (en) * 2020-09-27 2022-04-05 宝山钢铁股份有限公司 High magnetic induction oriented silicon steel and manufacturing method thereof
CN115992331A (en) * 2021-10-19 2023-04-21 宝山钢铁股份有限公司 High-magnetic-induction oriented silicon steel and manufacturing method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02258926A (en) * 1989-03-30 1990-10-19 Nippon Steel Corp Production of grain-oriented silicon steel sheet having high magnetic flux density
CN102443736A (en) * 2010-09-30 2012-05-09 宝山钢铁股份有限公司 Method for producing high magnetic flux-density oriented silicon steel product
CN103805918A (en) * 2012-11-15 2014-05-21 宝山钢铁股份有限公司 High-magnetic induction oriented silicon steel and production method thereof
CN104561795A (en) * 2014-12-12 2015-04-29 武汉钢铁(集团)公司 High magnetic induction grain-oriented silicon steel with B800 being more than or equal to 1.94T and production method thereof
CN112391512A (en) * 2019-08-13 2021-02-23 宝山钢铁股份有限公司 High magnetic induction oriented silicon steel and manufacturing method thereof
CN114277309A (en) * 2020-09-27 2022-04-05 宝山钢铁股份有限公司 High magnetic induction oriented silicon steel and manufacturing method thereof
CN114277308A (en) * 2020-09-27 2022-04-05 宝山钢铁股份有限公司 High magnetic induction oriented silicon steel and manufacturing method thereof
CN115992331A (en) * 2021-10-19 2023-04-21 宝山钢铁股份有限公司 High-magnetic-induction oriented silicon steel and manufacturing method thereof

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