WO2014078977A1 - 取向硅钢及其制造方法 - Google Patents

取向硅钢及其制造方法 Download PDF

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Publication number
WO2014078977A1
WO2014078977A1 PCT/CN2012/001684 CN2012001684W WO2014078977A1 WO 2014078977 A1 WO2014078977 A1 WO 2014078977A1 CN 2012001684 W CN2012001684 W CN 2012001684W WO 2014078977 A1 WO2014078977 A1 WO 2014078977A1
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Prior art keywords
silicon steel
oriented silicon
ratio
annealing
magnetic
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PCT/CN2012/001684
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English (en)
French (fr)
Inventor
杨国华
刘献东
李国保
杨勇杰
胡卓超
黑红旭
张军
宿德军
孙焕德
吴美洪
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宝山钢铁股份有限公司
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Application filed by 宝山钢铁股份有限公司 filed Critical 宝山钢铁股份有限公司
Priority to MX2015005961A priority Critical patent/MX2015005961A/es
Priority to JP2015543225A priority patent/JP6379100B2/ja
Priority to EP20178527.6A priority patent/EP3725908A1/en
Priority to KR1020157013350A priority patent/KR20150067381A/ko
Priority to EP12888787.4A priority patent/EP2924139B1/en
Priority to KR1020177001489A priority patent/KR20170010445A/ko
Priority to US14/646,985 priority patent/US10566119B2/en
Priority to RU2015119302A priority patent/RU2636214C2/ru
Publication of WO2014078977A1 publication Critical patent/WO2014078977A1/zh

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    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
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    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C8/00—Solid 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
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    • C23C—COATING 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
    • C23C8/00—Solid 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
    • C23C8/06—Solid 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
    • C23C8/08—Solid 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
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    • C23C—COATING 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
    • C23C8/00—Solid 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
    • C23C8/80—After-treatment
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    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
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    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
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    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
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    • C21D2201/05—Grain orientation

Definitions

  • the present invention relates to an oriented silicon pin and a method of manufacturing the same, and more particularly to an oriented silicon steel excellent in magnetic properties and a method of manufacturing the same.
  • Oriented silicon steel is widely used in power transmission and transformation products such as large transformers, and it is one of the indispensable raw materials in the development of the power industry.
  • the main technical indicators of oriented silicon steel magnetic properties include magnetic induction and iron loss. Iron loss is directly related to the core loss of transformers and other power transmission and transformation products. Some people say that the history of silicon steel product development is actually the history of continuous decline of iron loss;
  • the sense of magnetic induction also known as the magnetic flux density, reflects the strength of the magnetization of the ferromagnetic material in the magnetic field, and the change in the magnetic induction at the unit magnetic field strength is expressed by the magnetic permeability.
  • the magnetic permeability is more suitable for characterizing the magnetic properties of products under certain magnetic field strength.
  • the survey in the public literature related to oriented silicon steel, there are few studies directly related to magnetic properties such as magnetic permeability, and there are few studies on the influence of oriented silicon steel material structure on key properties such as magnetic permeability.
  • Japanese Patent JP 60-59045A and Chinese Patent CN 91103357 respectively disclose a method of cold rolling aging rolling, which can increase the number of small crystal grains having a grain equivalent circular diameter D 2 mm or less in an oriented silicon steel product, thereby reducing the orientation of the silicon steel. Iron loss of the finished product.
  • the above patent documents specifically refer to the premise that the secondary recrystallization of the oriented silicon steel product is perfect, and it is advantageous to appropriately increase the number of small crystal grains to reduce iron loss, and the small crystal grains here should be specifically understood as the direction of the muse texture. That is, the (110) [001] direction deviates from the small-sized crystal grains having a small angle, and otherwise it is difficult to achieve the effect of improving the magnetic properties.
  • the slab towel of the patent is added with a large amount of Cr, which is not only unfavorable to environmental protection, but also disadvantageous to the stable oriented silicon steel product which obtains the magnetic properties.
  • the patent recommends heating the slab at a high temperature of about 1400 ° C. This requires a dedicated heating furnace, which consumes less energy, and slag appears on the surface of the slab. The heating equipment needs to be cleaned regularly, affecting the output. , as well as reduced yields and equipment maintenance costs, are not suitable for promotion.
  • An object of the present invention is to provide an oriented silicon steel excellent in magnetic properties and a method for producing the same.
  • the inventors have found that the proportion of small crystal grains having a grain size of less than 5 mm (hereinafter referred to as D ⁇ 5 mm) in the oriented silicon steel product is not more than 3%, preferably not more than 2%, and the oriented silicon steel is 1.7 T under magnetic induction.
  • the magnetic permeability and the 1.5T lower magnetic permeability ratio ⁇ 17/ ⁇ 15 are 0.50 or more, and preferably ().55 or more, an oriented silicon steel product excellent in magnetic properties can be obtained.
  • the inventors have found that by using a slab of suitably oriented oriented silicon steel and an optimized cold rolling step, the ratio of the area of small ⁇ particles of D ⁇ 5 mm in the oriented silicon steel product is controlled to not more than 3% and the ratio of magnetic permeability is The ⁇ 17/ ⁇ 15 is controlled to be 0.50 or more, and the oriented silicon steel product excellent in magnetic properties can be stably obtained.
  • the invention relates to an oriented silicon steel with excellent magnetic properties, wherein the ratio of small crystal grain area of D ⁇ 5mm in the oriented silicon steel is not more than 3%, preferably not more than 2%; and the magnetic permeability of the oriented silicon steel product is 1.7T magnetic induction
  • the magnetic permeability ratio ⁇ at the time of 1.5 T is 7/ ⁇ 15 and is 0.50 or more, preferably 0.55 or more.
  • the large number of small grains deviating from the Gaussian texture in the oriented silicon steel product will seriously degrade the magnetic properties of the oriented steel, and the grain size (equivalent circle diameter) of the oriented silicon steel finished product has a large grain orientation of D>5mm and the muse
  • the average deviation angle of the texture is generally within 7°, so the ratio of the small crystal grain area of D ⁇ 5mm is controlled within a certain range, that is, the area ratio of the large-sized crystal grains of the finished silicon steel, which can better ensure the orientation of the silicon steel has 3 ⁇ 4. Good magnetic properties and magnetic performance stability.
  • the inventors have found that in the oriented silicon steel finished product, the small crystal grain area of D ⁇ 5 mm accounts for less than 3% of the total area, which can greatly improve the magnetic property excellent rate of the oriented silicon steel finished product and the whole coil pass rate. Further, the inventors have found that the ratio of the magnetic permeability ⁇ at a magnetic induction of 1.7T of the oriented silicon steel product to the magnetic permeability ⁇ 15 at 1.5T of ⁇ 17/ ⁇ 15 is ⁇ ).50 or more, which is sufficiently ensured to be stably obtained. Oriented silicon steel product with excellent magnetic properties with high magnetic induction and low iron loss.
  • the invention also relates to a method for producing oriented silicon steel, the sequence comprising the steps of:
  • the slab of oriented silicon steel is heated to 1100 ⁇ 1200'C and hot rolled to obtain a hot rolled sheet;
  • the slab of the oriented silicon steel comprises, by weight percentage, the following components: 2.5 to 4.0% of Si, 0.010, 0.040% of acid-soluble aluminum, Als, 0.004 to 0.012% of N, and 0.015% or less of S;
  • the small grain area ratio of the grain size of less than 5 mm in the oriented silicon steel product is not more than 3%.
  • the magnetic permeability of the oriented silicon steel product under 1.7T magnetic induction and the magnetic permeability ratio of 1.5T are ⁇ 17/ U 15 is 0.50 or more ⁇ >
  • the invention can ensure that the steel plate contains sufficient nitride inhibitor in the production process by controlling the content of Si and the content of the constituent elements of the inhibitor, such as Als, N and S, in the oriented silicon steel slab composition to obtain a perfect secondary re- Crystallization, and the degree of orientation of the secondary recrystallized grains in the Gaussian texture direction, that is, the (110) [001] direction. Further, in the case of using the slab of the oriented silicon steel of the present invention, A1N is a main bismuth preparation, and generation of an inhibitor having a high solid solution temperature such as sulfide is suppressed.
  • the solid solution temperature of A1N is about 1280'C, which varies slightly with the concentration fluctuation of A1 or N in the slab, but is significantly lower than the solid solution temperature using MnS or MnSe as the main inhibitor system (see national patent US 5711825).
  • the present invention employs a method in which the inhibitor is partially dissolved, and the heating temperature of the slab is effectively reduced to 1200'C or less.
  • the partial solid solution of the inhibitor is relative to the complete solid solution of the inhibitor.
  • the method of completely solid-solving the inhibitor means that the fine precipitates in the steel called the inhibitor reach a state of complete solid solution when the slab before hot rolling is heated, and then precipitate and adjust in the annealing process after the heat of $L and thereafter. Precipitation status.
  • the method of the invention does not require a dedicated silicon steel heating furnace, can use a conventional carbon steel heating furnace, and realize cross hot rolling production with other steel grades such as carbon steel, and the production equipment, instruments, instruments and the like control equipment are compared with the general oriented silicon steel. There is no change in production, so production control and operation are simple, no need to increase training for production operators, and production costs are reduced.
  • Si 2.5 to 4.0%.
  • the eddy current loss of the oriented silicon steel decreases as the Si content increases. If the Si content is less than 2.5%, the effect of reducing the eddy current loss cannot be achieved. If the Si content is higher than 4.0%, the cold rolling mass production cannot be performed due to the increase in brittleness.
  • Acid soluble aluminum Als 0.010 ⁇ 0,040%.
  • the main inhibitor component of the bismuth-sensitive silicon steel if the content of the acid-soluble aluminum Als is less than 0.010%, sufficient A1N cannot be obtained, the suppression strength is insufficient, and secondary recrystallization does not occur; if the content of Als is less than 0.040% Then, the inhibitor is coarsened in size and the inhibitory effect is lowered.
  • N 0.004 0.012%. Similar to the action of acid-soluble aluminum, N also acts as a soil inhibitor component of bismuth-sensitive silicon steel. If the N content is less than 0.004%, sufficient A1N cannot be obtained, and the inhibition strength is insufficient; if the N content is higher than 0.012%, The underlying defects increase.
  • S 0.015% or less. If the S content is in the range of 0.015%, segregation and precipitation tend to occur, resulting in an increase in secondary recrystallization defects.
  • the present invention adopts a cold rolling method of a large reduction ratio (a cold rolling reduction ratio of 85% or more), which contributes to an increase in the dislocation density of the cold rolled sheet, and forms more muse in the initial re-formation.
  • the crystal nucleus, and providing more favorable texture, is beneficial to the full secondary recrystallization and the secondary recrystallization grain orientation degree, thereby finally significantly improving the magnetic properties of the oriented steel product.
  • the cold rolling reduction ratio herein refers to the ratio of the amount of reduction in cold rolling to the thickness before unpressing.
  • the method for producing oriented silicon steel in the present invention can directly perform cold rolling after hot rolling without annealing the hot rolled sheet, and at this point, the production cost of the oriented silicon steel can be further reduced, and the potential is large. benefit.
  • the annealing temperature of the hot-rolled sheet annealing treatment is preferably 900 to l i50'C, annealing cooling
  • the speed is preferably 20 ° C / s ⁇ 100 ° C / s, if the cooling rate exceeds 100 'C / S , the uniformity of the microstructure in the steel after rapid cooling, the improvement of the magnetic properties of the final product is reduced, and if ⁇ It is produced at a cooling rate of more than 100'C/s, and the shape of the steel plate is poor, making it difficult to carry out subsequent production.
  • the annealing treatment in the method for producing oriented silicon steel of the present invention can be carried out in a manner conventionally used in the conventional art, for example, decarburization annealing, coating annealing separator, annealing annealing, and coating of insulating coating on the cold rolled sheet.
  • a hot drawing flat annealing wherein the annealing spacer is used to prevent the key plates from sticking to each other at a high temperature, and a material mainly based on materials such as MgO may be used:
  • the insulating coating is used to improve the insulation of the surface of silicon steel. At present, it is widely used as a raw material mainly composed of chromic anhydride, colloidal Si ⁇ 3 ⁇ 4 and Mg, and A1 phosphate.
  • the method of producing the oriented silicon steel of the present invention further comprises subjecting the cold rolled sheet to a nitriding treatment prior to annealing.
  • the invention obtains a supplemental nitride inhibitor by nitriding treatment to enhance the concentration of the inhibitor, and ensures that the A1N having sufficient strength in the later stage of the production process can inhibit the growth of other sites, thereby facilitating the improvement of secondary recrystallization.
  • the degree of orientation of the grains in the Gaussian texture direction significantly improves the magnetic properties of the oriented silicon steel products.
  • the invention controls the small crystal grain area ratio of D ⁇ 5mm in the oriented silicon steel finished product to not more than 3% by using the slab of the appropriately oriented oriented silicon steel and the optimized cold rolling step, and the magnetic permeability ratio ⁇ 17/y
  • the control of 15 is 0.50 or more, and the oriented silicon steel product excellent in magnetic properties can be stably obtained.
  • the invention controls the ratio of small crystal grain area of D ⁇ 5mm in the finished silicon steel product to not more than 3%, and the magnetic permeability under the magnetic induction of the oriented silicon steel product of 1.7T and the magnetic permeability ratio of 1.5T are ⁇ 17/
  • the ⁇ 15 is controlled to be 0.50 or more, and an oriented silicon steel product excellent in magnetic properties is obtained.
  • the present invention preferably controls the grain size and proportion of the oriented silicon steel finished product while effectively reducing the slab heating temperature and the production cost by using the slab of the appropriate oriented silicon steel and the optimized cold rolling step. -
  • the magnetic permeability in the range of constant magnetic induction ensures a good resynthesis of secondary recrystallization, and finally obtains an oriented silicon steel product with excellent magnetic properties.
  • the composition and weight percentage of the oriented silicon steel slab are C: 0.050%, Si: 3.0%, Als: 0.030%, N: 0.007%, S: 0.008%, Mn: 0.14%, and the balance is Fe and inevitable impurities.
  • the slab is heated in a heating furnace of 1000-1250 'C, hot rolled, rolled to a thickness of 2.5 mm hot rolled sheet, cold rolled the hot rolled sheet, and the hot rolled sheet is rolled at different cold rolling reduction rates to After the thickness of the finished product of 0.30 mm, decarburization annealing is performed, and an annealing separator containing cerium oxide as a main component is applied, and annealing is performed after rolling, and nitriding treatment is performed after final cold rolling and annealing under secondary annealing.
  • the coated silicon steel is obtained by coating the insulating coating and stretching and annealing.
  • the relationship between the small grain area ratio of D ⁇ 5mm and the magnetic permeability ratio ⁇ 17/ ⁇ 15 in the oriented silicon steel finished product and the magnetic properties of the oriented silicon steel finished product were studied. The results are shown in Table 1.
  • Table 1 Effect of small grain area ratio of D ⁇ 5mm and magnetic permeability ratio ⁇ 17/ ⁇ 15 on magnetic properties of finished silicon steel products
  • Example 9 [5 and Comparative Example 6-14
  • composition and weight percentage of the oriented silicon steel slab were C: 0.075%, Si: 3.3°/. , Als: 0.031%, N: 0.009%, S: 0.012%, Mn: 0.08%, the balance being Fe and unavoidable impurities.
  • the slab is heated in a heating furnace at five different heating temperatures of 1050 ⁇ 1250'C, then hot rolled, rolled to a thickness of 2.3 mm hot rolled sheet, and cold rolled by hot rolled sheet, pressed with different cold rolling.
  • the alloy After rolling to a thickness of 0.20 ⁇ 0.40mm different specifications, the alloy is decarburized and annealed, coated with magnesium oxide as the main component of the annealing separator, and then annealed after rolling; after the final cold rolling, the commercial temperature annealing The nitriding treatment is carried out before the secondary recrystallization; after the unwinding, the coated silicon steel is obtained by coating the insulating coating and stretching and annealing. Slab heating temperature and cold rolling The relationship between the reduction ratio and the small grain area ratio of D ⁇ 5 mm and the permeability ratio ⁇ 17/ ⁇ 15 in the finished silicon steel finished product were studied. The results of the study are shown in Table 2.
  • the slab is heated and then hot rolled in a temperature range of 110 (1200 ° C), and a cold rolling reduction ratio of 85% or more is employed. It can be ensured that the ratio of small crystal area of D ⁇ 5mm in the oriented silicon key product does not exceed 3%, and the magnetic permeability under 1.7T magnetic induction and the magnetic permeability ratio ⁇ 17/ ⁇ 15 at 1.5T are above 0.50, thereby ensuring Obtained oriented silicon steel finished product with excellent magnetic properties.
  • composition and weight percentage of the oriented silicon steel slab are C: 0.065%, Si: 3.2%, Als: 0.025%, N: 0.010%, S: 0.015%, Mn: 0.18%, and the balance is Fe and unavoidable impurities.
  • the slab is heated in an il50'C heating furnace and then hot rolled.
  • Examples 17-31 using hot-rolled sheet annealing compared with Example 16 which was not annealed by hot-rolled sheets reduced the proportion of small grain areas of D ⁇ 5 mm in the oriented silicon steel finished product or improved its The magnetic permeability ratio is ⁇ 17/ ⁇ 15, thereby improving the magnetic properties of the finished silicon steel product.
  • the temperature of 900 1150 'C, 20 ° C / s or more The cooling rate is annealed on the hot-rolled sheet to ensure that the magnetic permeability ratio of ⁇ 17/ ⁇ 15 is 0.55 or more, so that the magnetic properties of the oriented silicon steel finished product can be further stably improved.
  • the experimental results of the present invention prove that the ratio of the small grain area of E 5 mm in the oriented silicon steel finished product does not exceed 3%, and the magnetic permeability under the magnetic induction of the oriented silicon steel product of 1.7 T and the magnetic permeability ratio at 1.5 T ⁇ 17 /
  • U 15 is 0.50 or more
  • an oriented silicon steel product excellent in magnetic properties can be obtained.
  • the ratio of the small crystal grain area of D ⁇ 5 mm in the oriented silicon steel product can be controlled to not more than 3%, and the magnetic permeability ratio ⁇ is The 17/ ⁇ 15 control is 0.50 or more, so that an oriented silicon steel product excellent in magnetic properties can be stably obtained.
  • the invention controls the ratio of the small crystal grain area of D ⁇ 5mm in the finished silicon steel product to not more than 3%, and the magnetic permeability under the magnetic induction of the oriented silicon steel product of 1.7T and the magnetic permeability ratio of 1.5T ⁇ 17/
  • the ⁇ 15 is controlled to be 0.50 or more, and an oriented silicon steel product excellent in magnetic properties is obtained.
  • the present invention preferably controls the grain size and proportion of the oriented silicon steel product and the magnetic quantity by effectively reducing the slab heating temperature and the production cost by using the slab of the appropriate oriented silicon steel and the optimized cold rolling step.
  • the magnetic permeability within the sensing range ensures that the secondary recrystallization has a good Gaussian texture orientation, and finally the oriented silicon steel product with excellent magnetic properties is stably obtained.

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Abstract

一种磁性能优异的取向硅钢及其制造方法。本发明通过将取向硅钢成品中D<5mm的小晶粒面积比例控制为不超过3%，并且将取向硅钢成品1.7T磁感下的磁导率和1.5T下的磁导率比值µ17/µ15控制为0.50以上，获得了磁性能出色的取向硅钢。另外，本发明通过采用成分合适的取向硅钢的板坯以及优化的冷轧步骤，在有效降低板坯加热温度和生产成本的同时，较好控制了取向硅钢成品的晶粒尺寸和比例，以及一定磁感范围内的磁导率，保证了二次再结晶具有良好的高斯织构取向，最终稳定获得了磁性能优异的取向硅钢产品。

Description

取向硅钢及其制造方法
技术领域
本发明涉及一种取向硅销及其制造方法， 尤其涉及一种磁性能优异的取向硅钢及其制造 方法。
背景技术
取向硅钢被广泛应用于大型变压器等输变电产品中， 其是电力行业发展中不可或缺的原 材料之一。 g前， 人们致力于获得磁性能优异的取向硅钢。 取向硅钢磁性能的主要技术指标 包括磁感和铁损， 铁损直接关系到变压器等输变电产品使用时的铁芯损耗， 有人称硅钢产品 发展的历史其实就是铁损不断下降的历史； 磁感即磁感应强度， 又称为磁通密度， 反映铁磁 性材料在磁场中磁化的强弱， 而单位磁场强度下磁感的变化值用磁导率表示。 在用户使用条 件下 硅钢产品性能与外加磁场强度条件息息相关， 因此磁导率尤其是变压器等产品工作点 附近的磁导率更适于表征产品在一定磁场强度下的磁特性。 而根据调研， 在取向硅钢相关的 公幵文献中， 与磁导率等磁性能直接相关的研究还很少， 而在取向硅钢材料结构对磁导率等 关键性能影响方面的研究则更少。
日本专利 JP 60-59045A和中国专利 CN 91103357分别公开了通过冷轧时效轧制的方法， 可提高取向硅钢成品中晶粒等效圆直径 D 2mm以下的小晶粒数量， 从而可降低取向娃钢成 品的铁损。 但上述专利文献均特指在取向硅钢成品二次再结晶完善的前提下， 适当地提髙小 晶粒数量对降低铁损有利， 而且这里的小晶粒应特定理解为与髙斯织构方向即 (110)[001]方向 偏离角度较小的小尺寸晶粒， 否则难以达到提髙磁性能的效果。 因此， 仅仅提髙取向硅钢成 品中小晶粒的数量不应成为判断取向硅钢磁性能提高的标准， 这是因为小尺寸晶粒的晶粒取 向出现大角度偏离髙斯织构方向的可能性很大， 其远髙于大尺寸晶粒， 而大量出现的大角度 偏离高斯织构的小晶粒会严重劣化取向硅钢成品的磁性能。 相反， 晶粒等效圆直径 D≥5mm 的大晶粒取向与高斯织构的平均偏离角一般在 7。以内， 因此， 在通常情况卜'， 提髙取向硅钢 成品中大晶粒的数量或面积比例， 或者说将小晶粒数量或面积比例控制在一定范围内' 可以 较好地保证取向硅钢具有良好的磁性能以及磁性能稳定性。 美国专利 US 7887645B1中提到通过控制取向硅钢热乳板中奥氏体相 比例， 增加常化 冷速， 可以提高磁导率。 但该专利中的 "磁导率"特指磁场强度在 796A/m下的磁感， 其并不 是通常物理意义上所定义的磁导率。 并且该专利的板坯巾大量添加 Cr， 不仅不利于环保， 而 且不利于稳定获得髙磁性能的取向硅钢产品。 另外， 该专利中推荐在约 1400'C的高温下对板 坯进行加热， 这需要配置专用的加热炉， 能耗较髙， 并且钢坯表面出现化渣， 需要对加热设 备进行定期清理， 影响产量， 以及成材率降低、 设备维护成本髙， 不适合推广。
美国专利 US 5718775A 中提到要控制取向硅钥成品在 1.0T磁感下的磁导率不低于 0.03H/m。但是根据实际技术磁化磁滞回线分析， 在较低磁场下， 磁感较低时， 磁畴畴壁发生 移动； 隨着磁场强度增加， 磁感提髙， 约在 1.5~1.9T下时， 依靠畴壁移动已经长大的磁畴和 尚未被吞并掉的磁畴发生不可逆的转动， 使磁化矢量逐渐与磁场方向平行。 这个过程一直发 生直到所有磁畴的磁化矢量转到与磁场方向平行， 此时达到该材料的饱和磁感值 Bs。变压器 等产品应用的工作点一般设计在 1.5 1.7T的磁感范围， 因此美国专利 US 5718775 A提出对 1.0T磁感下取向硅钢的磁导率控制要求并不具有实际意义。
上述现有技术虽然在改善取向砬钢的磁导率和铁损方面取得了一些进展，但取向硅钢在 L5〜1.7T工作磁密下的磁性能仍有较大的改进空间。 人们希望开发出在 1.5~1.7T工作磁密下 具有优异磁性能的取向硅钢, 以满足变压器等电子设备的要求。 此外， 目前的取向硅钢的制 造方法还有较大的改进空间， 可获得磁性能优异的取向硅钢的制造方法的研发也具有重要的 意义以及广阔的应用前景。 发明内容
本发明的目的是提供一种磁性能优异的取向硅钢及其制造方法。 本发明人发现， 在取向 硅钢成品中晶粒尺寸小于 5mm (以下简称为 D<5mm)的小晶粒面积比例不超过 3%、优选不 超过 2%， 并且取向硅钢成品 1.7T磁感下的磁导率和 1.5T下 ^磁导率比值 μ 17/μ 15为 0.50 以上、 优选为（).55以上时， 可获得磁性能出色的取向硅钢成品。 进一步地， 本发明人发现， 通过采用成分合适的取向硅钢的板坯以及优化的冷轧步骤将取向硅钢成品中 D<5mm的小昴 粒面积比例控制为不超过 3%并且将磁导率比值 μ 17/ μ 15控制为 0.50以上,可稳定获得磁性 能优异的取向硅钢产品。
本发明涉及一种磁性能优异的取向硅钢， 该取向硅钢中 D<5mm的小晶粒面积比例不超 过 3%、 优选不超过 2%; 并且该取向硅钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ】7/ μ 1 5为 0.50以上、 优选 0.55以上。 取向硅钢成品中大量出现的偏离高斯织构的小晶粒会严重劣化取向 钢成品的磁性能， 而取向硅钢成品的晶粒尺寸（等效圆直径） D>5mm的大晶粒取向与髙斯织构的平均偏离角一 般在 7°以内， 因此控制 D<5mm小晶粒面积比例在一定范围内， 即提髙取向硅钢成品大尺寸 晶粒的面积比例， 可以较好的保证取向硅钢具有 ¾好的磁性能以及磁性能稳定性。 本发明人 发现，在取向硅钢成品中 D<5mm的小晶粒面积占总面积比例在 3%以内， 可大幅提高取向硅 钢成品的磁性能优良率以及整卷合格率。进一步地， 本发明人发现， 在取向硅钢成品 1.7T磁 感下的磁导率 μΠ和 1.5T下的磁导率 μ15的比值 μ17/μ15为 ί).50以上时，充分保证了可稳定 获得具有高磁感、 低铁损的优良磁性能的取向硅钢产品。
本发明还涉及一种取向硅钢的制造方法， 其顺序包括如下步骤：
将取向硅钢的板坯加热到 1100〜1200'C后迸行热轧以获得热轧板；
以 85%以上的冷轧压下率对热轧板进行冷轧以获得具有取向硅钢成品的厚度的冷轧板： 对冷轧板进行退火处理以获得取向硅钢成品； 其中，
所述取向硅钢的板坯以重量百分比计包含如下成分： 2.5〜4.0%的 Si, 0.010 0.040%的酸 可溶性铝 Als, 0.004~0.012%的 N， 0.015%以下的 S; 以及
所述取向硅钢成品中晶粒尺寸小于 5mm的小晶粒面积比½不超过 3%. 并且所述取向硅 钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ 17/U 15为 0.50以上■>
本发明通过在取向硅钢板坯成分中控制 Si含量和抑制剂组成元素含量， 如 Als、 N和 S 含量， 可以保证钢板在生产过程中含有足够的氮化物抑制剂， 以获得完善的二次再结晶， 并 提高二次再结晶晶粒在高斯织构方向即 (110)[001]方向的取向度。进一步地， 在使用本发明的 取向硅钢的板坯的情况中， A1N为主要抻制剂， 硫化物等具有高固溶温度的抑制剂的产生被 抑制。 A1N的固溶温度约为 1280'C , 随着板坯中 A1或 N的浓度波动略有变化， 但都显著低 于采用 MnS或 MnSe作为主要抑制剂系统的固溶温度 （参见 国专利 US 5711825); 而且本 发明采用抑制剂部分固溶的方法， 将板坯的加热温度有效降低至 1200'C以下。所谓抑制剂部 分固溶是相对于抑制剂完全固溶而言的。 抑制剂完全固溶的方法是指被称为抑制剂的钢中微 小析出物在热轧前的板坯加热时达到完全固溶的状态， 然后在热 $L及之后的退火工序中析出 并调整析出状态。 这种方法存在一个问题， 即为了使析出物完全固溶， 要求在 1350"C以上的 高温下进行加热， 比一般钢种的板坯加热温度髙出约 200'C , 为此需要专用的加热炉， 而且 存在熔融氧化铁皮即化渣较多的问题。 而来用抑制剂部分固溶的方法， 板坯加热温度低于抑 制剂完全固溶的温度， 板坯加热时钢中抑制剂只达到部分固溶， 虽然在热轧后获得的抑制剂 强度有所降低， 但通过后工序氮化处理可以补充氮化物抑制剂以保证二次再结晶的霈要。 因 此， 本发明的方法无需专用的硅钢加热炉， 可釆用常规碳钢加热炉， 与碳钢等其他钢种实现 交叉热轧生产， 且生产设备及仪器、 仪表等控制设备相对于一般取向硅钢生产无变化， 因而 生产控制和操作简便， 无需对生产操作人员增加培训， 生产成本降低。
取向硅钢板坯中 Si与各抑制剂的含量和基本作用说明如下-
Si: 2.5〜4.0%。 取向硅钢涡流损耗随着 Si含量的提高而降低， 如果 Si含量低于 2.5%则 无法达到降低涡流损耗的效果； 如果 Si含量高于 4.0%则由于脆性增加而无法进行冷轧批量 生产。
酸可溶性铝 Als: 0.010~0，040%。 作为髙磁感取向硅钢的主要抑制剂成分， 如果酸可溶 性铝 Als的含量低于 0.010%, 则无法获得足够的 A1N, 抑制强度不够， 不发生二次再结晶； 如果 Als的含量髙于 0.040%, 则抑制剂尺寸粗化， 抑制效果降低。
N: 0.004 0.012%。 与酸可溶性铝作用相近， N也作为髙磁感取向硅钢的土要抑制剂成 分，如果 N含量低于 0.004%,则无法获得足够的 A1N,抑制强度不够；如果 N含量高于 0.012%, 则底层缺陷增加。
S: 0.015%以下。如果 S含量商于 0.015%, 则易发生偏聚析出， 造成二次再结晶缺陷增 加。
另外， 本发明采用大压下率（85%以上的冷轧压下率） 的冷轧轧制方法， 有助于提高冷 轧板位错密度， 在初次再结品中形成更多的髙斯晶核， 并提供更多的有利织构， 有利于充分 发生二次再结晶和提髙二次再结晶晶粒取向度， 从而最终显著提髙取向 钢产品的磁性能。 此处的冷轧压下率是指冷轧中的压下量与未压下前的厚度的比值。
本发明中的取向硅钢的制造方法可在热轧之后直接进行冷轧 ' 而无锘对热轧板进行退火 处理， 就该点来说， 可进一步降低取向硅钢的生产成本， 具有较大的潜在效益。
就进一步提高取向硅钢成品的磁性能来说， 优选在冷轧前， 对热轧板进行热轧板退火处 理， 其中， 热轧板退火处理的退火温度优选为 900~l i50'C， 退火冷却速度优选为 20°C/s~100°C/s, 如果冷却速度超过 100'C/S, 则由于快冷后钢中组织均匀性变差， 对最终产 品磁性能的改善作用降低， 而且若釆用超过 100'C/s 的冷却速度进行生产， 钢板板形差， 很 难进行后续生产。 通过对热轧板进行热轧板退火处理， 可进一步提髙初次冉结晶时高斯晶核 的数量和有利织构的强度， 帮助完善二次再结晶， 提髙取向硅钢成品的磁性能。
本发明的取向硅钢的制造方法中的退火处理可按照传统技术中通常釆用的方式进行， 比 如对冷轧板顺序进行脱碳退火、 涂布退火隔离剂、 髙温退火、 涂布绝缘涂层以及热拉伸平整 退火，其中退火隔离剂用于防止高温下钥板之间彼此粘结，可使用以 MgO等材料为主的原料： 绝缘涂层用于提髙硅钢表面的绝缘性等， 目前广泛釆用以铬酐、 胶体 Si<¾和 Mg、 A1磷酸盐 为主的原料。
就进一步提髙取向硅钢成品的磁性能来说， 优选本发明的取向硅钢的制造方法还包括在 髙温退火之前对冷轧板进行渗氮处理。 本发明通过渗氮处理获得补充的氮化物抑制剂可增强 抑制剂浓度，确保生产工艺的后阶段有足够强度的 A1N完成对其他位向晶粒生长的抑制作用， 从而有利于提高二次再结晶晶粒在高斯织构方向的取向度，显著提髙取向硅钢成品的磁性能。
本发明通过采用成分合适的取向硅钢的板坯以及优化的冷轧步骤， 将取向硅钢成品中 D<5mm的小晶粒面积比例控制为不超过 3%,并且将磁导率比值 μ 17/y 15控制为 0.50以上， 可稳定获得磁性能优异的取向硅钢产品。
本发明通过将取向硅钢成品中 D<5mm的小晶粒面积比例控制为不超过 3%, 并且将取 向硅钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ 17/μ 15控制为 0.50以上， 获得 了磁性能出色的取向硅钢成品。 另外， 本发明通过釆用成分合适的取向硅钢的板坯以及优化 的冷轧歩骤， 在有效降低板坯加热温度和生产成本的同时， 较好控制了取向硅钢成品的晶粒 尺寸和比例以及- 定磁感范围内的磁导率， 保证了二次再结晶具有良好的髙斯织构取向， 最 终稳定获得了磁性能优异的取向硅钢产品。 具体实施方式
下面结合实施例对本发明进行更详细地说明，但本发明的保护范围并不限于这些实施例。 实施例 1-8和比较例 1-5
取向硅钢板坯的组分及重量百分比为 C: 0.050%, Si: 3.0%, Als: 0.030%, N: 0.007%, S: 0.008%, Mn: 0.14%, 其余为 Fe及不可 免的杂质。 将板坯在 1000-1250'C的加热炉内加热 后热轧， 轧至 2.5mm热轧板厚， 对热轧板进行冷轧， 以不同的冷轧压下率将热轧板轧制到 0.30mm成品厚度后，进行脱碳退火，涂布氧化镌为主要成分的退火隔离剂， 成卷后进行髙温 退火； 在最终冷轧后、 髙温退火二次再结晶之前进行滲氮处理： 开卷后经过涂绝缘涂层及拉 伸平整退火， 得到取向硅钢成品。 对取向硅钢成品中 D<5mm的小晶粒面积比例以及磁导率 比值 μ17/μ15与取向硅钢成品的磁性能之间的关系进行了研究， 研究结果参见表 1。 表 1 収向硅钢成品中 D<5mm的小晶粒面积比例及磁导率比值 μ17/μ15对其磁性能的影响
Figure imgf000007_0001
由表 1可知，与 D<5min的小晶粒面积比例超过 3%或者磁导率比值 μ17/μ15小于 0.50的 比较例 1-5相比，取向硅钢成品中 D<5mm的小晶粒面积比例不超过 3%并且 1.7T磁感下的磁 导率和 1.5T下的磁导率比值 μ17/μ15≥0.50的实施例 1-8具有更髙的磁感以及更低的铁损。进 一步地， 由表 1可知， 与实施例 6相比， D<5mm的小晶粒面积比例在 2%以下的实施例 4中 的取向硅钢成品的磁性能得到进一步地改善； 与实施例 4相比， 磁导率比值 μ17/μ15为 0.55 的实施例 3中的取向硅钢成品的磁性能得到进一步地改善。 实施例 9-〖5和比较例 6-14
取向硅钢板坯的组分及重量百分比为 C: 0.075%, Si: 3.3°/。， Als: 0.031%, N: 0.009%, S: 0.012%, Mn: 0.08%, 其余为 Fe及不可避免的杂质。 将板坯在加热炉内以 1050〜1250'C五种 不同的加热温度迸行加热后热轧， 轧至 2.3mm热轧板厚， 对热轧板进行冷轧， 以不同的冷轧 压下率分别轧制到 0.20~0.40mm不同规格成品厚度后， 进行脱碳退火， 涂布氧化镁为主要成 分的退火隔离剂， 成卷后进行髙温退火； 在最终冷轧后、 商温退火二次再结晶之前进行渗氮 处理； 开卷后经过涂绝缘涂层及拉伸平整退火， 得到取向硅钢成品。 对板坯加热温度和冷轧 压下率与取向硅钢成品中 D<5mm的小晶粒面积比例以及磁导率比值 μ17/μ15之间的关系进 行了研究， 研究结果参见表 2。
板坯加热温度和冷乱压下率对取向陆钢成品中 D<5mm的小晶粒面积比例
以及磁导率比值 μ17/μ15的影响
Figure imgf000008_0001
由表 2可知， 在采用本发明中的取向硅钢板坯的情况下， 通过在 110( 1200'C温度范围 内对板坯进行加热后热轧， 并且采用 85%以上的冷轧压下率， 可以保证取向硅钥成品中 D<5mm的小晶粒面积比例不超过 3%, 并且 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ17/μ15在 0.50以上， 从而可确保获得磁性能优异的取向硅钢成品。 实施例 16-31
取向硅钢板坯的组分及重量百分比为 C: 0.065%, Si: 3.2%, Als: 0.025%, N: 0.010%, S: 0.015%, Mn: 0.18%, 其余为 Fe及不可避免的杂质。 将板坯在 il50'C加热炉内加热后热轧， 轧至 3.0mm热礼板厚， 对热轧板进行 （A)直接冷乳， 或者 （B)在 850~1200°C的温度、 以 及 15-25'C/S 的冷却速度下进行热轧板退火， 之后以 85%的冷轧压下率进行冷轧， 轧制到 0.30mm成品厚度后，进行脱碳退火，涂布氧化镁为主要成分的退火隔离剂， 成卷后逬行髙温 退火； 在最终冷轧后、 高温退火二次再结晶之前进行渗氮处理； 开卷后经过涂绝缘涂层及拉 伸平整退火， 得到取向硅钢成品。 对热轧板退火条件与取向硅钢成品中 D<5mm的小晶粒面 积比例以及磁导率比值 μ17/μ15之间的关系进行了研究， 研究结果参见表 3。
表 3 热轧板退火条件对取向硅钢成品中 D<5mm的小晶粒面积比例
以及磁导率比值 μ!7/μ15的影响
Figure imgf000009_0001
由表 3可知， 与未采用热轧板退火的实施例 16相比， 采用了热轧板退火的实施例 17-31 降低了取向硅钢成品中 D<5mm的小晶粒面积比例或者提高了其磁导率比值 μ17/μ15，从而提 高了取向硅钢成品的磁性能。 进一步地， 由表 3可知， 以 900 1150 'C的温度、 20°C/s以上的 冷却速度对热轧板迸行退火， 可保证 μ17/μ15磁导率比值在 0.55以上， 从而可进一步稳定提 高取向硅钢成品的磁性能。
本发明的实验结果证明，在取向硅钢成品中 E 5mm的小晶粒面积比例不超过 3%，并且 取向硅钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ 17/ U 15为 0.50以上时， 可获 得磁性能出色的取向硅钢成品。 通过采用本发明中的成分合适的取向硅钢的板坯以及优化的 冷轧步骤， 可将取向硅钢成品中 D<5mm的小晶粒面积比例控制为不超过 3%，并且将磁导率 比值 μ 17/μ 15控制为 0.50以上， 从而可稳定获得磁性能优异的取向硅钢产品。
本发明通过将取向硅钢成品中 D<5mm的小晶粒面积比例控制为不超过 3%,并且将取向 硅钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ 17/ μ 15控制为 0.50以上， 获得了 磁性能出色的取向硅钢成品。 另外， 本发明通过釆用成分合适的取向硅钢的板坯以及优化的 冷轧步骤 在有效降低板坯加热温度和生产成本的同时， 较好控制了取向硅钢成品的晶粒尺 寸和比例以及一定磁感范围内的磁导率， 保证了二次再结晶具有良好的高斯织构取向， 最终 稳定获得了磁性能优异的取向硅钢产品。

Claims

权 利 要 求 书
1. 一种取向 Γ圭钢， 其特征在于， 所述取向硅钢中晶粒尺寸小于 5mm的小晶粒面积比例 不超过 3%, 并且所述取向硅钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 y 17/μ 15 为 0.50以上。
2.如权利要求 1所述的取向娃钢， 其特征在于， 所述取向硅钢中晶粒尺寸小于 5mm的 小晶粒面积比例不超过 2%。
3.如权利要求 1-2中任一项所述的取向硅钢，其特征在于，所述取向硅钢 1.7T磁感下的 磁导率和 1.5T下的磁导率比值 μ 17/μ 15为 0.55以上。
4. 一种取向硅钢的制造方法， 其顺序包括如下歩骤：
将取向硅钢的板坯加热到〖100~1200'C后进行热轧以获得热轧板；
以 85%以上的冷轧压下率对热轧板进行冷轧以获得具有取向硅钢成品的厚度的冷札板； 对冷轧板进行退火处理以获得取向硅钢成品： 其中， ,
所述取向硅钢的板坯以重量百分比计包含如下成分： 2.5~4.0%的 Si, 0.01O~0.O40%的酸 可溶性铝 Als， 0.004 0.012°/。的 N, 0.015%以下的 S, 以及
所述取向硅钢成品中晶粒尺寸小于 5mm的小晶粒面积比例不超过 3%, 并且所述取向硅 钢成品 1.7T磁感下的磁导率和 1.5T下的磁导率比值 μ 17/ U 15为 0.50以上。
5.如权利要求 4所述的取向硅钢的制造方法， 其特征在于， 所述制造方法还包括： 在冷 轧前， 对所述热轧板进行热轧板退火处理。
6.如权利要求 5所述的取向硅钢的制造方法， 其特征在于， 所述热轧板退火处理的退火 温度为 900〜1150 , 退火冷却速度为 20〜100。C/s。
7.如权利要求 4所述的取向硅钢的制造方法， 其特征在亍， 所述退 处理顺序包括： 脱 碳退火、 涂布退火隔离剂、 高温退火、 涂布绝缘涂层以及热拉伸平整退火。
8.如权利要求 7所述的取向硅钢的制造方法， 其特征在于， 所述制造方法还包括在所述 髙温退火之前对所述冷轧板进行渗氮处理。
9.如权利要求 4-8中任一项所述的取向硅钢的制造方法， 其特征在于， 所述取向硅钢成 品中晶粒尺寸小于 5mm的小晶粒面积比例不超过 2%。
10. 如权利要求 4-8中任一项所述的取向硅钢的制造方法， 其特征在于， 所述取向硅钥 成品 1.7T磁感下的磁导率和 L5T下的磁导率比值 U 17/ U 15为 0.55以上。
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RU2015119302A (ru) 2017-01-10
US20150302962A1 (en) 2015-10-22
KR20170010445A (ko) 2017-01-31
RU2636214C2 (ru) 2017-11-21
CN103834856A (zh) 2014-06-04
EP2924139B1 (en) 2021-02-10
JP2016505706A (ja) 2016-02-25
US10566119B2 (en) 2020-02-18
JP6379100B2 (ja) 2018-08-22
EP3725908A1 (en) 2020-10-21
MX2015005961A (es) 2015-09-10
EP2924139A1 (en) 2015-09-30
KR20150067381A (ko) 2015-06-17
CN103834856B (zh) 2016-06-29

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