WO2010015156A1 - 一种含铜取向硅钢的生产方法 - Google Patents

一种含铜取向硅钢的生产方法 Download PDF

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WO2010015156A1
WO2010015156A1 PCT/CN2009/071442 CN2009071442W WO2010015156A1 WO 2010015156 A1 WO2010015156 A1 WO 2010015156A1 CN 2009071442 W CN2009071442 W CN 2009071442W WO 2010015156 A1 WO2010015156 A1 WO 2010015156A1
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annealing
steel
fine powder
cold rolling
thickness
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PCT/CN2009/071442
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English (en)
French (fr)
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吉亚明
孙换德
杨国华
杨勇杰
许云鹏
黄昌国
李国保
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宝山钢铁股份有限公司
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Priority to JP2011501094A priority Critical patent/JP5463347B2/ja
Priority to US13/058,073 priority patent/US8231739B2/en
Priority to KR1020117005426A priority patent/KR101294624B1/ko
Priority to EP09804456.3A priority patent/EP2322674B1/en
Publication of WO2010015156A1 publication Critical patent/WO2010015156A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D10/00—Modifying the physical properties by methods other than heat treatment or deformation
    • C21D10/005—Modifying the physical properties by methods other than heat treatment or deformation by laser shock processing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/008—Heat treatment of ferrous alloys containing Si
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1233—Cold rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1255—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 with diffusion of elements, e.g. decarburising, nitriding
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1266—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 between cold rolling steps
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying 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
    • C21D8/1283—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper

Definitions

  • the present invention relates to a method for producing oriented silicon steel, and more particularly to a method for producing a copper-containing oriented silicon steel having high electromagnetic properties. Background technique
  • the lower slab heating temperature is the development direction.
  • the medium temperature oriented silicon steel production process using aluminum nitride and copper as inhibitors can achieve a lower slab heating temperature (1250 ⁇ 1300 °C).
  • the technique uses two cold rolling methods with intermediate complete decarburization annealing, namely After a cold rolling, the intermediate complete decarburization annealing (to remove the carbon to less than 30 ppm) is performed, and after the second cold rolling to the thickness of the steel sheet, the low temperature recovery annealing treatment is performed, and the MgO annealing separator is applied for high temperature annealing and post treatment.
  • Oriented silicon steel bottom layer has always been a difficult point in the production of oriented silicon steel.
  • a good bottom layer is the guarantee of tension effect and insulation effect of the tension coating, but the unevenness of the joint between the bottom layer and the substrate hinders the magnetic domain activity and increases the iron loss; The presence of the resulting silicon steel is poor.
  • no underlayer oriented silicon steel has recently been developed.
  • X is as follows: slab composition in terms of mass percentage: Si: 0. 8 ⁇ 4. 8%, C: 0. 003 ⁇ 0. 1%, acid soluble A1: 0. 012 0. 05%, N: 0. 01% or 0. 01% or less, the rest is Fe and unavoidable impurities; after hot rolling and directly or after hot-rolled sheet annealing, pass through the secondary annealing once or during the intermediate annealing Or cold rolling to a final thickness, and then decarburization annealing is performed in an atmosphere gas in which the oxidation degree of the Fe-based oxide is not formed, and an oxide layer containing silicon dioxide as a main component is formed on the surface of the steel sheet.
  • the surface of the steel sheet after annealing is mirror-finished, and the film is coated with an annealing agent which is coated with alumina as a main component.
  • the water vapor partial pressure in the water and steel sheet annealing stabilizes the secondary recrystallization.
  • the production method disclosed in Korean Patent KR 526122 is a low-temperature oriented silicon steel process characterized by decarburization and nitriding simultaneously.
  • the addition of Si0 2 and C1 isolating agent to the magnesium oxide is used to prevent the formation of a bottom layer during high-temperature annealing, and the characteristics are:
  • the composition is C: 0. 045 ⁇ 0. 062, Si: 2. 9 ⁇ 3.
  • non-bottom oriented silicon steels which are (Al, Si)N or AlN+MnS as inhibitors, and adopt conventional cold or low temperature production processes of cold rolling to steel plate thickness and then decarburization annealing.
  • the purpose is to further Reduce iron loss and improve punch performance.
  • Chinese patent CN 1400319 discloses a continuous secondary recrystallization annealing process without inhibitor.
  • the process is: the weight percentage of the molten steel component is: C: 0.08% or less, Si: 1.0-8.0%, Mn : 0.005-3.0%, the steel plate is first subjected to hot rolling, then cold rolling, recrystallization annealing, secondary recrystallization annealing, Decarburization annealing, high temperature continuous annealing.
  • This process obtains a high magnetic flux density low iron loss oriented electrical steel sheet without using an inhibitor. Summary of the invention
  • An object of the present invention is to provide a method for producing a copper-containing oriented silicon steel which does not form a bottom layer in a high-temperature annealing process to obtain an oriented silicon steel having good electromagnetic properties and surface quality.
  • a method for producing a copper-containing oriented silicon steel the steps of which are:
  • the steel is converted by a converter or an electric furnace.
  • a slab having the following composition (in percentage by weight) is obtained: C: 0.010% to 0.050%, Si: 2.5% to 4 ⁇ 0% ⁇ : 0 ⁇ 1% ⁇ 0 ⁇ 30%, Als: 0 ⁇ 006% ⁇ 0 ⁇ 030%, Cu: 0 ⁇ 4% ⁇ 0 ⁇ 7%, ⁇ : 0 ⁇ 006% ⁇ 0 ⁇ 012%, S : 0.025%, the balance being Fe and unavoidable impurities;
  • shot blasting and pickling are performed to remove surface iron oxides to control the oxygen content to be less than 500 ppm; then pickling, performing a second cold rolling, and rolling to a desired thickness of the steel sheet;
  • the high-temperature annealing process is: the second cold-rolled steel plate is coated with a high-temperature annealing separator in a slurry form, and dried to make the water content of the release agent less than 1.5%; or directly dried by an electrostatic coating method;
  • the high temperature annealing of the steel sheet is carried out in a protective atmosphere containing hydrogen, and the degree of oxidation (P 0 / PH 2 ) of the protective gas is between 0.0001 and 0.2.
  • the high-temperature annealing separator is mainly composed of any one of zirconia ceramic fine powder, alumina fine powder, and silica fine powder, or zirconia ceramic fine powder, alumina fine powder, and silica fine powder. Two or three combinations.
  • Hot rolling process The slab is heated in the heating furnace to above 125 CTC, and kept for more than two hours, and hot rolled to ensure 1050 to 1200 °C.
  • the thickness of the hot-rolled sheet of the thickness of the inner-rolling temperature is more than 850.
  • the decarburization annealing and the second cold rolling are performed, and the thickness of the steel sheet obtained by the second cold rolling is 0.15 to 0.50 mm, followed by degreasing, finally high temperature annealing, tension coating and tensile flat annealing.
  • the invention adopts any one of zirconia ceramic fine powder, alumina fine powder and silica fine powder or zirconia ceramic fine powder, alumina fine powder and silica fine powder.
  • the main isolating agent, the release agent does not react with the surface oxide during the high temperature annealing process, and the high temperature annealing atmosphere is strictly controlled to make the surface oxide formed by decarburization annealing to form Si0 2 to be reduced in the high temperature annealing stage to form a glassless film.
  • the mirror-like finished product after applying the tension coating, obtains the oriented silicon steel with excellent surface quality and magnetic properties, which fundamentally solves the problem that the bottom quality of the traditional slab medium temperature heating process is unstable, the surface coating is easy to fall off, the tension effect is not obvious, and the insulation is And the problem of poor surface quality.
  • the production method of the copper-containing oriented silicon steel of the invention does not form a glass film during the high-temperature annealing process, and the intermediate decarburization annealing does not need to strictly control the decarburization annealing atmosphere in the range of not forming iron oxide, and can be at a higher oxidation degree (P 0 /
  • the intermediate decarburization annealing under PH 2 ) improves the decarburization efficiency, thereby ensuring that the carbon content is reduced to less than 30 ppm, thereby avoiding the deterioration of magnetic properties caused by the magnetic aging of the finished product, and reducing the intermediate decarburization annealing time to improve the production efficiency.
  • the invention performs shot blasting and pickling after intermediate decarburization annealing to remove the oxide layer mainly composed of iron oxide on the surface, which can effectively improve the surface quality of the slab after the secondary cold rolling and improve the surface quality of the final product.
  • the invention directly coats the release agent after high temperature annealing after the secondary cold rolling, and there is no problem of deterioration of magnetic properties and instability of the bottom layer due to the recovery annealing, and the recovery annealing process is omitted, and the production efficiency is improved.
  • the present invention does not form a bottom layer during high-temperature annealing, it is not necessary to strictly control the separator composition and the coating method, thereby improving product production stability and effectively improving the steel purification effect.
  • the mirror-like finished product is obtained, and the unevenness of the surface oxide layer and the glass film of the steel sheet which hinders the movement of the magnetic domain is eliminated, and the iron loss is remarkably reduced.
  • the invention effectively solves the problems of insufficient decarburization, reduced annealing, reduced magnetic properties, poor adhesion of the coating, inconspicuous tension effect and poor surface quality in the medium temperature slab heating production method under the condition of maintaining the slab medium temperature heating. It is a low-cost, high-efficiency and easy-to-implement method for producing oriented silicon steel sheets.
  • the slab chemical composition (Wt%) is: 0. 035% C, 3. 05% Si, 0. 020% S, with a 500 kg vacuum furnace.
  • the second cold rolling is performed, and the thickness is rolled to a finished thickness of 0.30 mm; the steel strip is coated with an annealing separator containing A1 2 0 3 slurry as a main component and dried. Thereafter, the steel strip is rolled in a nitrogen, hydrogen or pure hydrogen atmosphere at 1200 ° C for 20 hours of high temperature annealing; after unwinding, it is subjected to an insulating coating and stretch flat annealing.
  • the slab chemical composition (Wt%) is: 0. 032% C, 3. 15% Si, 0. 016% S, 0. 012% Als, 0. 0092% N, 0. 48 %Cu, 0. 20% Mn, the balance being Fe and unavoidable impurities. 5mm ⁇ The thickness of the thickness of 2. 5mm, the thickness of the slab is 2, 5mm, and the thickness is 2. 5mm Strip steel. The thickness of the finished product is 0. 30mm; after the shot blasting, the second cold rolling is performed after the shot blasting, and the thickness is 0.
  • the steel strip is coated with an annealing separator containing A1 2 0 3 slurry as the main component and dried; then the steel strip is rolled into a high temperature annealing at 1200 ° C for 20 hours in an atmosphere of nitrogen, hydrogen or pure hydrogen; Apply an insulating coating and stretch flattening.
  • the obtained magnetic properties and coating properties of the finished products are shown in Table 2, wherein the adhesion evaluation methods and standards are carried out in accordance with the national standard GB/T 2522-1988.
  • the slab chemical composition (Wt%) is: 0. 032% C, 3. 15% Si, 0. 016% S, 0. 012% Als, 0. 0092% N, 0. 48 %Cu, 0. 20% Mn, the balance being Fe and unavoidable impurities. 5mm ⁇ The thickness of the thickness of 2. 5mm, the thickness of the slab is 2, 5mm, and the thickness is 2. 5mm Strip steel. The above strip steel is subjected to shot blasting, pickling and cold rolling to a thickness of 0. 65mm and then subjected to intermediate annealing at 85CTC according to the conditions of Table 3; shot blasting, pickling followed by secondary cold rolling or direct secondary cold rolling, rolling to finished product Thickness of 0.
  • the slab chemical composition (Wt%) is: 0. 032% C, 3. 15% Si, 0. 016% S, 0. 012% Als, 0. 0092% N, 0. 48 %Cu, 0. 20% Mn, the balance being Fe and unavoidable impurities. 5mm ⁇ The thickness of the thickness of 2. 5mm, the thickness of the slab is 2, 5mm, and the thickness is 2. 5mm Strip steel. 5 ⁇ After the above-mentioned strip steel, after the blasting, pickling, cold rolling to a thickness of 0. 65mm, in the 85CTC according to the conditions of Table 4 for intermediate annealing; shot blasting, pickling after the second cold rolling, rolling to the finished thickness of 0.
  • the steel strip is coated with an electrostatic spray A1 2 0 3 as the main component of the annealing separator; after that, the steel strip is rolled in a nitrogen, hydrogen or pure hydrogen atmosphere at 1200 ° C for 20 hours of high temperature annealing; Coating and stretch flat annealing.
  • the obtained magnetic properties and coating properties are shown in Table 4.
  • the slab chemical composition (Wt%) is: 0. 032% C, 3. 15% Si, 0. 016% S, 0. 012% Als, 0. 0092% N, 0. 48 %Cu, 0. 20% Mn, the balance being Fe and unavoidable impurities. 5mm ⁇ The thickness of the thickness of 2. 5mm, the thickness of the slab is 2, 5mm, and the thickness is 2. 5mm Strip steel. 5 ⁇ After the above-mentioned strip steel, after the blasting, pickling, cold rolling to 0. 65mm thickness, in the 85CTC according to the conditions of Table 5 for intermediate annealing; shot blasting, pickling after the second cold rolling, rolling to the finished thickness of 0.
  • the steel strip is coated with an annealing separator coated with Zr0 2 slurry as the main component and dried or directly electrostatically sprayed with ⁇ 2 fine powder as the main component of the annealing separator; after that, the steel strip is rolled into nitrogen, hydrogen or In a pure hydrogen atmosphere, high temperature annealing was performed at 1200 ° C for 20 hours; after unwinding, it was subjected to an insulating coating and tensile flat annealing. The obtained magnetic properties and coating properties are shown in Table 5.
  • the method of the invention adopts the method of not forming the bottom layer in the high-temperature annealing process under the premise of maintaining the temperature heating advantage of the slab, and strictly controls the decarburization annealing and the high-temperature annealing process, and obtains the mirror-oriented silicon steel without the bottom layer, and the tension coating is implemented.
  • the finished product has good appearance and electromagnetic properties, improves the performance of the finished film, reduces the process, improves the production efficiency, and has stable product performance.
  • the equipment used is a conventional production equipment for oriented silicon steel, and the technology and control are simple and easy.

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Description

一种含铜取向硅钢的生产方法 技术领域
本发明涉及一种取向硅钢生产方法，尤其是高电磁性能的含铜取向硅钢生 产方法。 背景技术
目前， 取向硅钢生产工艺中， 较低的板坯加热温度为发展方向。 采用氮化铝及 铜为抑制剂的中温取向硅钢生产工艺可以实现较低的板坯加热温度（1250〜1300 °C)， 该技术采用含中间完全脱碳退火的两次冷轧法， 即第一次冷轧后进行中间完 全脱碳退火 (将碳脱到 30ppm以下）， 第二次冷轧至钢板厚度后直接或经过低温回复 退火处理后涂 MgO退火隔离剂进行高温退火及后处理。 板坯中温加热工艺为了在高 温退火阶段形成完整玻璃膜， 需要严格控制脱碳退火条件形成合适表面氧化层。 但 是， 中间脱碳退火的板坯较厚， 在保证形成合适氧化层脱碳退火条件下， 难以将碳 脱到 30ppm以下。 并且该工艺中间脱碳退火后进行二次冷轧， 表面氧化层被破坏， 影响表面质量。
取向硅钢底层一直是取向硅钢生产中的难点， 良好底层是张力涂层发挥张力效 果和绝缘效果的保证， 但是底层与基板结合处的凹凸会阻碍磁畴活动而使铁损增加 ； 同时玻璃膜底层的存在导致取向硅钢的冲片差。 为了达到进一步降低铁损和提高 冲片性的目的， 最近发展了无底层取向硅钢。
中国专利 03802019. X公开了的生产方法为： 板坯成分以质量百分比计为： Si : 0. 8〜4. 8%、 C: 0. 003〜0. 1%、 酸可溶性 A1 : 0. 012〜0. 05%、 N: 0. 01%或 0. 01%以 下、 其余为 Fe及不可避免的杂质； 先热轧再直接或者热轧板退火后， 通过一次或 者其间介入中间退火的二次或二次以上的冷轧制成最终的板厚， 接着， 在不形成 Fe 系氧化物的氧化度的气氛气体中进行脱碳退火， 在钢板表面上形成以二氧化硅作为 主成分的氧化层后， 通过涂布以氧化铝作为主成分的退火分离剂， 将钢板退火后的 表面制成镜面状， 通过控制以水浆状涂布干燥以氧化铝作为主成分的退火分离剂后 的带入水分及钢板退火中的水蒸气分压， 使二次再结晶稳定化。
韩国专利 KR 526122公开的生产方法是针对脱碳、 渗氮同时进行特点的低温取 向硅钢工艺采用氧化镁中添加 Si02、 C1隔离剂，使在高温退火过程中不形成底层， 其特征为： 钢坯成分按重量百分比计为 C : 0. 045〜0. 062、 Si : 2. 9〜3. 4、 P:0.015-0.035, Als (酸溶性 Al): 0· 022〜0· 032、 Cu: 0·012〜0·021、 Ν:0·006〜 0.009、 S:0.004〜0.010; 控制钢坯的加热温度在 1150-119CTC范围内； 冷轧至钢板 厚度后在 840-89CTC含氨的湿氮、氢保护气体中进行脱碳、渗氮使用重量比例为 100 份 Mg0+3〜12份 Si02+25份氯离子为主要成分的隔离剂， 进行高温退火。
上述两个专利为无底层取向硅钢， 均以 (Al、 Si)N或 AlN+MnS为抑制剂， 采用 冷轧至钢板厚度再进行脱碳退火的传统高温或低温生产工艺， 其目的是为了进一步 降低铁损、 提高冲片性能。
中国专利 CN 1400319 公开了一种无抑制剂的连续式二次再结晶退火工艺。 该 工艺为： 钢水成分重量百分比为： C: 0.08%以下、 Si: 1.0-8.0%、 Mn: 0.005-3.0%, 钢板先进行热轧， 之后冷轧、 再结晶退火、 二次再结晶退火、 脱碳退火、 高温连续 退火。 该工艺在不使用抑制剂的情况下， 得到高磁通密度低铁损取向性电磁钢板。 发明内容
本发明的目的在于提供一种含铜取向硅钢的生产方法， 该方法使钢板在高温退 火过程中不形成底层， 获得具有良好电磁性能和表面质量的取向硅钢。
本发明是这样实现的： 一种含铜取向硅钢的生产方法， 其步骤为：
首先用转炉或电炉炼钢， 钢水经二次精炼和连铸后， 获得成分如下的板坯 (按 重量百分比计）： C: 0.010%〜0.050%、 Si: 2·5%〜4·0%、 Μη: 0· 1%〜0· 30%、 Als: 0· 006%〜0· 030%、 Cu: 0·4%〜0·7%、 Ν: 0· 006%〜0· 012%、 S: 0.025%， 其余为 Fe 及不可避免的杂质；
之后热轧、 酸洗、 第一次冷轧、 脱脂， 之后进行中间脱碳退火， 脱碳退火工艺 为： 钢板在 PH20/PH2=0.50〜0.88的保护气氛中， 800〜900°C温度条件下进行 3〜8 分钟脱碳退火， 使钢板的碳含量降到 30ppm以下；
接着进行抛丸和酸洗去除表面铁的氧化物， 使氧含量控制在 500ppm以下； 然后酸洗、 进行第二次冷轧， 轧制到钢板所需厚度；
再进行高温退火；
最后在钢板表面施加张力涂层及拉伸平整退火。
所述高温退火工艺为： 第二次冷轧后的钢板以水浆状涂布高温退火隔离剂， 经 过烘干使隔离剂的含水率小于 1.5%； 或者通过静电涂布方法直接进行干涂；
钢板高温退火在含氢的保护性气氛中进行， 通入保护性气体的氧化度 (P 0/PH2) 在 0.0001〜0.2之间。 所述高温退火隔离剂主要成分为氧化锆陶瓷细粉、 氧化铝细粉、 二氧化硅细粉 中的任一种或氧化锆陶瓷细粉、 氧化铝细粉、 二氧化硅细粉中的任意两种或三种组 合。
本发明热轧和冷轧以及其他工艺为常规技术手段， 具体参数如下： 热轧工艺： 板坯在加热炉内加热到 125CTC以上，保温两小时以上，进行热轧，保证 1050〜1200 °C的开轧温度， 80CTC以上的终轧温度， 最好是保证 1070〜1130°C的开轧温度， 850 以上的终轧温度， 最终轧成 2. 0〜2. 8mm厚度的热轧板。
热轧之后酸洗， 再进行第一次冷轧， 轧制到 0. 50〜0. 70mm 的中间厚度， 再进 行脱脂。
之后进行脱碳退火和第二次冷轧， 第二次冷轧得到的钢板厚度为 0. 15〜0. 50 mm, 再进行脱脂， 最后进行高温退火， 施加张力涂层及拉伸平整退火。
本发明采用氧化锆陶瓷细粉、 氧化铝细粉、 二氧化硅细粉中的任一种或氧化锆 陶瓷细粉、 氧化铝细粉、 二氧化硅细粉中的任意两种或三种组合为主的隔离剂， 在 高温退火过程中隔离剂不与表面氧化物反应， 并严格控制高温退火气氛使脱碳退火 形成 Si02为主的表面氧化物在高温退火阶段被还原， 形成无玻璃膜的镜面状成品， 施加张力涂层后获得表面质量和磁性能优良的取向硅钢， 从根本上解决了传统板坯 中温加热工艺底层质量不稳定、 表面涂层易脱落、 张力效果不明显、 绝缘性和表面 质量差问题。
本发明具有以下有益效果：
本发明含铜取向硅钢的生产方法在高温退火过程中不形成玻璃膜， 中间脱碳退 火无需将脱碳退火气氛严格控制在不形成铁氧化物范围内， 可以在较高氧化度 (P 0/PH2)下进行中间脱碳退火， 提高脱碳效率， 从而保证碳含量降低到 30ppm 以 下， 避免了成品磁时效而导致磁性能的恶化， 并可以降低中间脱碳退火时间提高生 产效率。
本发明在中间脱碳退火后进行抛丸和酸洗， 除去表面以铁氧化物为主的氧化 层， 可以有效改善二次冷轧后板坯表面质量并可改善最终成品表面质量。 本发明在 二次冷轧后直接涂布隔离剂进行高温退火， 不存在回复退火造成磁性能恶化和底层 不稳定问题， 并省去了回复退火工艺环节， 提高了生产效率。
由于本发明在高温退火过程中不形成底层， 不需要严格控制隔离剂成分和涂布 方式， 能够提高产品生产稳定性并有效改善钢质净化效果。 获得镜面状成品， 消除 了妨碍磁畴移动的钢板表面氧化层和玻璃膜的凹凸， 显著降低铁损。 总之， 本发明在保持板坯中温加热优势条件下， 有效解决中温板坯加热生产方 法中存在的脱碳不充分、 回复退火降低磁性能、 涂层附着性差、 张力效果不显著和 表面质量差问题， 是一种低成本、 高效率易实施的取向硅钢板制造方法。 本发明的最佳实施方案
实施例 1 :
用 500kg真空炉炼钢， 板坯化学成分（Wt%)为： 0. 035%C， 3. 05%Si， 0. 020%S,
0. 008%Als , 0. 0010%N, 0. 60%Cu， 0. 15%Mn其余为 Fe及不可避免的杂质。 通过对此 成分板坯加热到 1280°C、 保温 3小时进行热轧， 终轧温度为 930〜950°C， 轧后层 流冷却， 550°C ± 30°C卷取， 形成厚度 2. 5mm 的带钢。 上述带钢经抛丸、 酸洗后冷 轧到 0. 65mm厚度后进行中间退火， 将碳脱到 30ppm以下。 抛丸、 酸洗后按照下列 三种工艺进行：
(1)进行第二次冷轧， 轧制到成品厚度 0. 30mm; 钢带涂以 A1203浆液为主要成分 的退火隔离剂并烘干。 此后钢带成卷在氮、 氢或纯氢的气氛中进行 1200°C、 保温 20小时的高温退火； 开卷后经过涂绝缘涂层及拉伸平整退火。
(2)进行第二次冷轧， 轧制到成品厚度 0. 30mm; 涂布 MgO为主要成分的隔离剂， 成卷后在在氮、 氢或纯氢的气氛中进行 1200°C、 保温 20小时的高温退火； 开卷后 经过涂绝缘涂层及拉伸平整退火。
(3)进行第二次冷轧， 轧制到成品厚度 0. 30mm; 接着在湿的氮、 氢气氛中进行 70CTC以下的退火处理， 涂布 MgO为主要成分的隔离剂， 成卷后在在氮、 氢或纯氢 的气氛中进行 1200°C、 保温 20小时的高温退火； 开卷后经过涂绝缘涂层及拉伸平 整退火。
得到的成品磁性能及涂层性能见表 1。
表 1
Figure imgf000005_0001
实施例 2 :
用 500kg真空炉炼钢， 板坯化学成分（Wt%)为： 0. 032%C, 3. 15%Si， 0. 016%S， 0. 012%Als , 0. 0092%N, 0. 48%Cu， 0. 20%Mn, 其余为 Fe及不可避免的杂质。 通过对 此成分板坯加热到 1280°C、 保温 3小时进行热轧， 终轧温度为 930〜950°C， 轧后 层流冷却， 550°C ± 30°C卷取， 形成厚度 2. 5mm 的带钢。 上述带钢经抛丸、 酸洗后 冷轧到 0. 65mm厚度后在 85CTC按表 2条件进行中间退火； 抛丸、酸洗后进行第二次 冷轧， 轧制到成品厚度 0. 30mm; 钢带涂以 A1203浆液为主要成分的退火隔离剂并烘 干； 此后钢带成卷在氮、 氢或纯氢的气氛中进行 1200°C、 保温 20小时的高温退火 ； 开卷后经过涂绝缘涂层及拉伸平整退火。 得到的成品磁性能及涂层性能见表 2， 其中附着性评价方法和标准按照国家标准 GB/T 2522-1988执行。
表 2
Figure imgf000006_0001
实施例 3 :
用 500kg真空炉炼钢， 板坯化学成分（Wt%)为： 0. 032%C, 3. 15%Si， 0. 016%S， 0. 012%Als , 0. 0092%N, 0. 48%Cu， 0. 20%Mn, 其余为 Fe及不可避免的杂质。 通过对 此成分板坯加热到 1280°C、 保温 3小时进行热轧， 终轧温度为 930〜950°C， 轧后 层流冷却， 550°C ± 30°C卷取， 形成厚度 2. 5mm 的带钢。 上述带钢经抛丸、 酸洗后 冷轧到 0. 65mm厚度后在 85CTC按表 3条件进行中间退火； 抛丸、酸洗后二次冷轧或 直接进行二次冷轧， 轧制到成品厚度 0. 30mm; 钢带涂以 A1203浆液为主要成分的退 火隔离剂并烘干； 此后钢带成卷在氮、 氢或纯氢的气氛中进行 1200°C、 保温 20小 时的高温退火； 开卷后经过涂绝缘涂层及拉伸平整退火。 得到的成品磁性能及涂层 性能见表 3。
表 3
Figure imgf000007_0001
实施例 4:
用 500kg真空炉炼钢， 板坯化学成分（Wt%)为： 0. 032%C, 3. 15%Si， 0. 016%S， 0. 012%Als , 0. 0092%N, 0. 48%Cu， 0. 20%Mn, 其余为 Fe及不可避免的杂质。 通过对 此成分板坯加热到 1280°C、 保温 3小时进行热轧， 终轧温度为 930〜950°C， 轧后 层流冷却， 550°C ± 30°C卷取， 形成厚度 2. 5mm 的带钢。 上述带钢经抛丸、 酸洗后 冷轧到 0. 65mm厚度后， 在 85CTC按表 4条件进行中间退火； 抛丸、 酸洗后进行第二 次冷轧， 轧制到成品厚度 0. 30mm; 钢带涂静电喷涂 A1203为主成分的退火隔离剂； 此后钢带成卷在氮、 氢或纯氢的气氛中进行 1200°C、 保温 20小时的高温退火； 开 卷后经过涂绝缘涂层及拉伸平整退火。 得到的成品磁性能及涂层性能见表 4。
表 4
中间退火条件 磁性能 成品绝缘涂层情况
说明
PH20/PH2 时间 B8， T Pl7 W/kg 附着性 涂层外观
0. 88 5min 1. 904 1. 010 B 涂层良好均匀 发明例
0. 88 4min 1. 885 1. 041 B 涂层良好均匀 发明例
0. 80 5min 1. 895 1. 024 B 涂层良好均匀 发明例
0. 65 5min 1. 890 1. 029 B 涂层良好均匀 发明例
0. 60 5min 1. 886 1. 037 B 涂层良好均匀 发明例 实施例 5:
用 500kg真空炉炼钢， 板坯化学成分（Wt%)为： 0. 032%C, 3. 15%Si， 0. 016%S， 0. 012%Als, 0. 0092%N, 0. 48%Cu， 0. 20%Mn, 其余为 Fe及不可避免的杂质。 通过对 此成分板坯加热到 1280°C、 保温 3小时进行热轧， 终轧温度为 930〜950°C， 轧后 层流冷却， 550°C ± 30°C卷取， 形成厚度 2. 5mm的带钢。 上述带钢经抛丸、 酸洗后 冷轧到 0. 65mm厚度后， 在 85CTC按表 5条件进行中间退火； 抛丸、酸洗后进行第二 次冷轧，轧制到成品厚度 0. 30mm;钢带钢带涂以分别进行涂以 Zr02浆液为主要成分 的退火隔离剂并烘干或直接静电喷涂 ΖιΌ2细粉为主成分的退火隔离剂；此后钢带成 卷在氮、 氢或纯氢的气氛中进行 1200°C、 保温 20小时的高温退火； 开卷后经过涂 绝缘涂层及拉伸平整退火。 得到的成品磁性能及涂层性能见表 5。
表 5
Figure imgf000008_0001
本发明方法在保持板坯中温加热优势的前提下， 采用高温退火过程中不 形成底层的方法， 并严格控制脱碳退火和高温退火工艺,获得了无底层镜面状 取向硅钢， 实施张力涂层的成品具有良好的外观和电磁特性， 提高了成品的 冲片性能， 减少了工序， 提高了生产效率， 产品性能稳定， 所用设备为取向 硅钢的常规生产设备， 技术和控制简单易行。

Claims

权 利 要 求
1、 一种含铜取向硅钢的生产方法， 其步骤为：
首先用转炉或电炉炼钢， 钢水经二次精炼和连铸后， 获得成分如下的板坯 (按 重量百分比计）： C: 0. 010%〜0. 050%、 Si : 2· 5%〜4· 0%、 Μη: 0· 1%〜0· 30%、 Als : 0· 006%〜0· 030%、 Cu: 0· 4%〜0· 7%、 Ν: 0· 006%〜0· 012%、 S: 0. 025%， 其余为 Fe 及不可避免的杂质；
之后热轧、 酸洗、 第一次冷轧、 脱脂， 之后进行中间脱碳退火， 脱碳退火工艺 为： 钢板加热到 80CTC以上的均热温度， 在 PH20/PH2=0. 50〜0. 88的保护气氛中进行 8分钟以内中间脱碳退火， 退火后使钢板的碳含量降到 30ppm以下；
接着进行抛丸和酸洗去除表面铁的氧化物， 使氧含量控制在 500ppm以下； 然后酸洗、 进行第二次冷轧， 轧制到钢板所需厚度；
再进行高温退火；
最后在钢板表面施加张力涂层及拉伸平整退火。
2、 如权利要求 1 所述的的含铜取向硅钢的生产方法， 其特征在于， 所述高温 退火工艺为： 第二次冷轧后的钢板以水浆状涂布高温退火隔离剂， 经过烘干使隔离 剂的含水率小于 1. 5%； 或者通过静电涂布方法直接进行干涂；
钢板高温退火在含氢的保护性气氛中进行， 通入保护性气体的氧化度 (P 0/PH2) 在 0. 0001〜0. 2之间。
3、 如权利要求 2所述的的含铜取向硅钢的生产方法， 其特征在于， 所述高温 退火隔离剂主要成分为氧化锆陶瓷细粉、 氧化铝细粉、 二氧化硅细粉中的任一种或 氧化锆陶瓷细粉、 氧化铝细粉、 二氧化硅细粉中的任意两种或三种组合。
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