WO2009117959A1 - 一种高电磁性能取向硅钢的生产方法 - Google Patents

一种高电磁性能取向硅钢的生产方法 Download PDF

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WO2009117959A1
WO2009117959A1 PCT/CN2009/071003 CN2009071003W WO2009117959A1 WO 2009117959 A1 WO2009117959 A1 WO 2009117959A1 CN 2009071003 W CN2009071003 W CN 2009071003W WO 2009117959 A1 WO2009117959 A1 WO 2009117959A1
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annealing
rolling
temperature
slab
hot rolling
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French (fr)
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杨国华
孙换德
吉亚明
李国保
黑红旭
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Baoshan Iron and Steel Co Ltd
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Baoshan Iron and Steel Co Ltd
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Priority to US12/934,897 priority Critical patent/US8333846B2/en
Priority to EP09725052A priority patent/EP2272995B1/en
Priority to JP2011501093A priority patent/JP5479448B2/ja
Priority to KR1020107023644A priority patent/KR101252561B1/ko
Publication of WO2009117959A1 publication Critical patent/WO2009117959A1/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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02—Extraction of non-metals
    • C21D3/04—Decarburising
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
    • C21D8/1255—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment with diffusion of elements, e.g. decarburising, nitriding
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment
    • C21D8/1266—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283—Application of a separating or insulating coating
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • 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
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • 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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment 
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment 
    • C21D8/0284—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the working steps
    • C21D8/1233—Cold rolling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention relates to a method for producing high electromagnetic performance oriented silicon steel. Background technique
  • the hot rolling heating temperature is above 1350 °C, the energy consumption is high, and the slag appears on the surface of the slab under such high temperature conditions. Cleaning, affecting production, and high energy consumption, equipment is easy to damage, and production costs are high. Therefore, researchers at home and abroad have carried out a lot of research to reduce the heating temperature of silicon steel.
  • the trend of the main improvement methods is divided into two according to the heating temperature range.
  • One type of hot rolling heating temperature is 1150-1250 ° C, called low temperature.
  • the slab heating technology mainly adopts the method of nitriding formation inhibitor in the latter stage to obtain the inhibition ability.
  • the low temperature slab heating technology develops rapidly, for example, US Patent US 5,049,205, Chinese Patent CN 1978707 and Korean Patent KR 2002074312
  • the method requires an increase in nitriding equipment, resulting in an increase in cost, and there is a problem that the magnetic properties of the final product are not uniform due to uneven nitriding.
  • Another hot rolling heating temperature is 1250-1320 ° C.
  • the medium temperature slab heating technology uses a Cu-containing inhibitor, and uses two cold rolling methods for the slabs that are smelted and continuously cast, and an intermediate decarburization annealing (one-time decarburization annealing) between the two cold rollings.
  • the carbon content in the steel sheet is removed to less than 30 ppm; after the second cold rolling, the MgO release agent is directly applied, or the low temperature recovery annealing is followed by the MgO release agent, followed by high temperature annealing and subsequent treatment.
  • the object of the present invention is to provide a method for producing silicon steel having high electromagnetic properties, which can achieve better secondary recrystallization and bottom quality by controlling the composition and process of the slab, thereby achieving the purpose of improving the electromagnetism of the oriented silicon steel product.
  • the invention is realized as follows: a method for producing high-electromagnetic-oriented oriented silicon steel, which comprises steelmaking by a converter or an electric furnace, after the secondary refining and continuous casting of the molten steel, obtaining a slab, followed by hot rolling, first cold Rolling, decarburization annealing, second cold rolling, coating an annealing separator containing magnesium oxide as a main component, then performing high temperature annealing, finally coating an insulating coating and performing tensile flat annealing, the composition of the slab ( In weight percent):
  • the rest are Fe and unavoidable impurities.
  • Als is acid soluble aluminum.
  • the hot rolling process is as follows: The slab is heated in a heating furnace to 1250 ⁇ 1350 ° C, kept for 2-6 hours, and then hot rolled, and the hot rolling finishing process has an opening and rolling temperature of 1050 1200 ° C, and the finishing temperature is It is 800 ° C or more.
  • the hot rolling finishing process has an opening and rolling temperature of 1070 to 1130 ° C and a finishing rolling temperature of 850 ° C or higher. It is hot rolled into a hot rolled sheet having a thickness of 2.0 to 2.8 mm.
  • the intermediate decarburization annealing is performed, and the intermediate decarburization annealed steel sheet is heated to a soaking temperature of 800 ° C or higher, and subjected to intermediate decarburization annealing in a wet hydrogen atmosphere for 10 minutes, and the carbon content of the steel sheet is reduced to 30 ppm or less after annealing. .
  • a second cold rolling is performed, and the required thickness of the finished product is 0.15 0.35 mm.
  • An annealing separator containing MgO as a main component is applied to the steel sheet.
  • high temperature annealing is performed.
  • the process is as follows: the gas is kept for 15 hours under the condition that the atmosphere is hydrogen or hydrogen containing more than 75% of the nitrogen-hydrogen mixture gas, the dry atmosphere (ie, the dew point DP ⁇ 0 °C), and the temperature is 1170 ⁇ 1230 °C.
  • the atmosphere is hydrogen or hydrogen containing more than 75% of the nitrogen-hydrogen mixture gas
  • the dry atmosphere ie, the dew point DP ⁇ 0 °C
  • the temperature is 1170 ⁇ 1230 °C.
  • the invention controls the Cu 2 S and MnS from the composition by increasing the sulfur content to S: 0.015% ⁇ 0.025%, manganese to sulfur ratio 10 Mn/S 20, and copper to manganese ratio Cu/Mn 2 by designing the composition content of the slab.
  • the proportion of the compound is such that it facilitates the development of the precipitation form of Cu 2 S during the hot rolling.
  • the rolling and finishing temperatures are strictly controlled, so that most of the sulfur in the hot rolling process is only in the form of Cu 2 S inhibitor, and the composite precipitation of MnS+Cu2S is avoided as much as possible, thereby avoiding the inhibitor. Coarse And unevenness.
  • the precipitation temperature of Cu 2 S is about 900-1100 ° C, and the precipitation peak is 1000 ° C.
  • the precipitation peak of MnS is more than 1100 ° C, so the rolling temperature higher than 1050 ° C and the finishing temperature above 800 ° C are the largest.
  • the degree of Cu 2 S is ensured to have sufficient precipitation and distribution, and the composite precipitation of MnS and Cu 2 S is inhibited, thereby ensuring that Cu 2 S and A1N are completed in the later stages of the production process.
  • the inhibition promotes the secondary recrystallization (110) [001] Gaussian direction nucleus has sufficient growth driving force, and the final product magnetic properties are significantly improved.
  • the sulfur in the as-cast structure tends to be segregated in the center, so the slab must be heated at a temperature above 1250 ° C to ensure sufficient holding time to fully dissolve the sulfide in the center. It is possible to precipitate sufficient Cu 2 S in a finely dispersed state in the subsequent hot rolling.
  • the method of the present invention increases the sulfur content, if the final high-temperature annealing desulfurization is incomplete, the magnetic properties of the product are deteriorated, especially the iron loss property, and the magnetic aging is caused, and the processing property of the product is also significantly lowered. Therefore, there is a stricter requirement for the purification annealing time in the high-temperature annealing process, that is, the purification annealing is performed under the condition that the atmosphere is hydrogen or hydrogen containing more than 75% of the nitrogen-hydrogen mixture gas, and the dew point of the dry atmosphere is DR ⁇ 0 °C. Keep the holding time at 1170 ⁇ 1230 °C for more than 15 hours.
  • the temperature is too low or the holding time is too short, harmful elements such as N and S cannot be completely eliminated, and the magnetic properties are lowered.
  • the temperature is too high, the secondary recrystallized grains are coarse, the iron loss is increased, and the quality of the glass film is lowered.
  • the invention has the following beneficial effects:
  • the invention effectively improves the form of sulfide precipitation during hot rolling by designing the composition content of the slab, controlling the slab heating and controlling the hot rolling conditions, and maximally avoids the composite inhibition of MnS+Cu 2 S.
  • the precipitation form of the agent ensures a uniform and fine precipitation of a sufficient amount of the inhibitor, and the magnetic property can be remarkably improved while maintaining the low production cost, and the iron loss is effectively reduced to obtain a high magnetic induction oriented silicon steel.
  • the difference of sulfur content, manganese content and copper content in the oriented silicon steel slab it is divided into various components. Except for the three components of S, Mn and Cu, the weight percentage of other components remained unchanged, C: 0.040%, Si: 3.17%, Als: 0.017%, N: 0.01%, S, Mn, See the three components of Cu Table 1, the rest are Fe and unavoidable impurities.
  • the slab is then treated according to the following process: after being heated in a heating furnace at a reheating temperature of 1280 ° C for 3 hours, hot rolling to a hot rolled sheet having a thickness of 2.5 mm, and the hot rolling process ensures the completion of the finish rolling.
  • the rolling temperature is 1050 1200 °C, and the finishing temperature is above 800 °C.
  • the first cold rolling is performed, after rolling to a thickness of 0.65 mm, the intermediate decarburization annealing is performed at 850 ° C in a wet hydrogen protective atmosphere.
  • composition and weight percentage of the oriented silicon steel slab are C: 0.032%, Si: 3.2%, Als: 0.012%, N: 0.01%, S: 0.016%, Mn: 0.18%, Cu: 0.42%, and the rest are Fe and Inevitable impurities.
  • the slabs are heat-heated in a heating furnace according to different reheating systems in Table 2, and then hot-rolled to a hot-rolled sheet having a thickness of 2.5 mm.
  • the rolling and finishing temperatures of the hot-rolled finishing are referred to Table 2;
  • the intermediate decarburization annealing is performed at 850 ° C in a wet hydrogen atmosphere to reduce the carbon content in the steel sheet to less than 30 ppm;
  • the second cold after the intermediate decarburization annealing Rolling rolling to a finished product thickness of 0.27mm ;
  • coating MgO as the main component of the release agent after rolling in an atmosphere of 100% H 2 , dew point of -10 ° C, temperature of 1200 ° C for 20 hours High temperature annealing; after the unwinding, after coating with insulating coating and tensile flat annealing, the obtained magnetic properties of the finished product are shown in Table 2. Effect of composition, slab heating system and hot rolling degree on magnetic properties
  • composition and weight percentage of the oriented silicon steel slab are C: 0.032%, Si: 3.2%, Als: 0.012%, N: 0.01%, S: 0.016%, Mn: 0.18%, Cu: 0.42%, and the rest are Fe and Inevitable impurities.
  • the steel was heated in a heating furnace at 1280 ° C for 3 hours and then hot rolled to a hot rolled sheet having a thickness of 2.5 mm, wherein the hot rolling and finishing rolling temperatures were 1100 ° C and 930 ° C respectively ; after pickling After the first cold rolling, after rolling to a thickness of 0.60 mm, the intermediate decarburization annealing is performed at 850 ° C in a wet hydrogen atmosphere to reduce the carbon content in the steel sheet to less than 30 ppm; the second decarburization annealing is performed for the second time.

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Description

一种高电磁性能取向硅钢的生产方法 技术领域
本发明涉及一种高电磁性能取向硅钢的生产方法。 背景技术
现在较为成熟的普通取向硅钢 （CGO) 生产技术， 采用 MnS作为主要抑制 剂， 热轧加热温度在 1350度以上， 能耗较高， 并且这样的高温条件下钢坯表面 出现化渣， 加热设备需定期清理， 影响产量， 并且能耗高， 设备易损坏， 生产 成本高。 因此国内外的科研人员开展了大量的研究来降低硅钢的加热温度， 其 主要改进方法的趋势按照加热温度范围来区分有两种， 一种热轧加热温度在 1150-1250°C， 称为低温板坯加热技术， 主要采用后阶段渗氮形成抑制剂的方法 来获得抑制能力现阶段低温板坯加热技术发展较快，例如美国专利 US 5049205、 中国专利 CN 1978707和韩国专利 KR 2002074312但这几种方法都要增加渗氮设 备， 造成成本增加， 并且存在渗氮不均匀引起最终产品磁性能不均匀的问题。
另一种热轧加热温度在 1250-1320°C， 作为与上述低温技术的区分， 亦可称 为中温板坯加热技术。 中温板坯加热技术采用含 Cu的抑制剂， 对经过冶炼和连 铸的板坯使用两次冷轧法， 在两次冷轧之间采用中间脱碳退火 （一次性脱碳退 火） 的方法， 将钢板中的碳含量脱到 30ppm以下； 第二次冷轧后直接涂 MgO隔 离剂， 或低温回复退火后再涂 MgO隔离剂， 接着进行高温退火及后续处理。 欧 洲专利 EP 0709470和中国专利 CN 1786248A公开了的技术方案属于中温板坯加 热技术， 两者的共同问题是硫含量过低， 造成抑制剂数量不足和分布不均匀， 从而影响局部或整体的抑制能力， 使二次再结晶驱动力不足， 磁性能劣化和不 均匀化。 发明内容
本发明的目的在于提供一种高电磁性能取向硅钢的生产方法， 通过控制板 坯成分和工艺获得较好的二次再结晶和底层质量， 达到提高取向硅钢产品的电 磁性能的目的。
本发明是这样实现的： 一种高电磁性能取向硅钢的生产方法， 包括用转炉 或电炉炼钢， 钢水经二次精炼和连铸后， 获得板坯， 之后进行热轧、 第一次冷 轧、 脱碳退火、 第二次冷轧， 涂布以氧化镁为主要成分的退火隔离剂， 然后进 行高温退火， 最后涂绝缘涂层和进行拉伸平整退火， 所述板坯的组分 （按重量 百分比计） 为：
C: 0.020%~0.050%
Si: 2. 6%~3.6%
S: 0.015%~0.025%
Als: 0.008%~0.028%
N: 0.005%~0.020%
Mn: 0.15%~0.5%, 且 10 Mn/S 20
Cu: 0.3%~1.2%, 且 Cu/Mn 2
其余为 Fe及不可避免的杂质。 Als 为酸溶性铝。
所述热轧工艺为： 板坯在加热炉内加热到 1250~1350°C， 保温 2~6小时， 再进行热轧， 热轧精轧过程的开轧温度为 1050 1200 °C， 终轧温度为 800°C以 上。
所述热轧精轧过程的开轧温度为 1070~1130°C， 终轧温度为 850°C以上。 经热轧轧成 2.0~2.8mm厚度的热轧板。
之后进行酸洗和第一次冷轧， 轧制到 0.50~0.70mm的中间厚度。
接着进行中间脱碳退火，将中间脱碳退火钢板加热到 800°C以上的均热温 度， 在湿氢保护气氛中进行 10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。
中间脱碳退火后， 进行第二次冷轧， 轧制到成品所需厚度 0.15 0.35 mm。 在钢板上涂布以 MgO为主要成分的退火隔离剂。
最后进行高温退火， 工艺为： 在气氛为氢气或氢气占 75%以上的氮氢混 合气、 干气氛 （即露点 D.P.<0°C )、 温度为 1170~1230°C的条件下进行保温 15 小时以上的高温退火。
本发明通过对板坯成分含量的设计， 硫含量提高到 S: 0.015%~0.025%、 锰硫比 10 Mn/S 20、 以及铜锰比 Cu/Mn 2， 从成分上控制 Cu2S和 MnS的化合物比例， 使得热轧过程中有利于向 Cu2S的析出形式发展。 并且， 在热轧过程中严格控制开轧和终轧温度， 使热轧过程中大多数硫仅以 Cu2S抑 制剂的形式， 尽可能避免 MnS+Cu2S的复合析出， 从而避免了抑制剂的粗大 和不均匀化。 Cu2S析出温度约为 900~1100°C， 析出峰值为 1000°C ; 而 MnS 的析出峰值大于 1100°C， 因此大于 1050°C的开轧温度和 800°C以上的终轧温 度，最大程度的保证了 Cu2S有足够的析出量和分布，同时抑制了 MnS和 Cu2S 的复合析出，从而确保生产工艺的后阶段 Cu2S和 A1N—起完成对其他位向晶 粒生长的抑制作用，促使二次再结晶 (110)[001] 高斯方向的晶核具有足够的生 长驱动力， 最终产品磁性能显著提高。
当硫含量高时， 铸态组织中硫容易在中心形成偏聚， 因此板坯加热时必 须在 1250°C以上的温度下保证足够的保温时间， 才能使中心的硫化物充分固 溶， 才有可能在之后的热轧中使足够的 Cu2S以细小弥散的状态析出。
高温退火时， 大量细小的 Cu2S和少量 MnS处于弥散状态， 使表面脱 S 减慢， 增强了抑制力并提高了二次再结晶温度， 使二次晶粒位向更准确， 磁 性能提高。
由于本发明方法提高了硫含量， 如果最终高温退火脱硫不完全， 会引起 产品磁性能劣化， 尤其是铁损性能， 并引起磁时效， 同时产品的加工性能也 会明显降低。 因此对高温退火工艺中的净化退火时间有更严格的要求， 即需 要在气氛为氢气或氢气占 75%以上的氮氢混合气、 干气氛下露点 D.R<0°C的 条件下进行净化退火， 在 1170~1230°C下保温时间 15小时以上。 温度过低或 保温时间过短， N、 S等有害元素无法完全排除， 磁性能降低； 温度过高， 二 次再结晶晶粒粗大， 铁损增加， 并且玻璃膜质量下降。
本发明具有以下有益效果： 本发明通过板坯成分含量的设计、 板坯加热 和热轧条件的控制， 有效改善热轧过程中硫化物析出形式， 最大程度避免了 MnS+Cu2S的复合抑制剂的析出形式，从而保证足够量的抑制剂均匀和细小的 析出， 在保持低生产成本的情况下能够显著提高磁性， 有效降低铁损， 获得 高磁感取向硅钢。
本发明的最佳实施方案
实施例 1 :
按取向硅钢板坯中硫含量、 锰含量和铜含量的不同分为多种组分。 各组 分中除 S、 Mn、 Cu三种成分外， 其他成分的重量百分比保持不变， 分别为 C: 0.040%, Si: 3.17%, Als: 0.017%, N: 0.01%, S、 Mn、 Cu三种成分含量见 表 1， 其余为 Fe及不可避免的杂质。之后将上述板坯按下面的工艺进行处理： 在 1280°C的再加热温度下在加热炉内保温 3小时后， 热轧至厚度为 2.5mm的 热轧板， 热轧过程保证精轧的开轧温度在 1050 1200 °C， 终轧温度在 800°C以 上； 酸洗后进行第一次冷轧， 轧制到 0.65mm厚度后， 在 850°C、 湿氢保护气 氛中进行中间脱碳退火， 使钢板中碳含量降到 30ppm以下； 中间脱碳退火后 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， 成卷后在气氛为 100% ¾、 露点为 -10°C， 温度为 1200 °C的条件下进行 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 见表 1 (高磁感取向硅钢常规产品的磁性能参考标准为： 磁感 B8 1.88 T， 铁 损 P17/50 1.30 W/kg， 以下同）。
Figure imgf000005_0001
磁性
硫含量 猛含量 铜含量
磁感 铁损 说明
(%) (%) (%)
B8(T) P17/50(W/kg)
0.015% 0.15% 0.3% 1.88 1.14 发明例
0.015% 0.15% 0.6% 1.88 1.16 发明例
0.015% 0.22% 0.45% 1.90 1.03 发明例
0.015% 0.22% 0.6% 1.91 1.07 发明例
0.015% 0.3% 0.6% 1.89 1.13 发明例
0.015% 0.3% 0.8% 1.88 1.18 发明例
0.020% 0.2% 0.4% 1.90 0.99 发明例
0.020% 0.2% 0.6% 1.91 1.01 发明例
0.020% 0.3% 0.6% 1.90 1.05 发明例
0.020% 0.3% 0.8% 1.90 1.12 发明例
0.020% 0.4% 0.8% 1.89 1.10 发明例
0.020% 0.4% 1.0% 1.88 1.21 发明例
0.025% 0.25% 0.5% 1.90 1.08 发明例
0.025% 0.25% 0.6% 1.90 1.15 发明例
0.025% 0.32% 0.65% 1.90 1.17 发明例
0.025% 0.32% 0.8% 1.88 1.19 发明例
0.025% 0.5% 1.0% 1.88 1.21 发明例
0.025% 0.5% 1.2% 1.88 1.23 发明例 0.010% 0.15% 0.6% 1.84 1.32 比较例
0.020% 0.15% 0.6% 1.86 1.28 比较例
0.020% 0.2% 0.3% 1.84 1.35 比较例
0.020% 0.3% 0.4% 1.82 1.39 比较例
0.020% 0.4% 0.6% 1.82 1.42 比较例
0.020% 0.5% 1.1% 1.79 1.59 比较例
0.030% 0.4% 1.0% 1.67 1.65 比较例 实施例 2:
取向硅钢板坯的组分及重量百分比为 C: 0.032%， Si: 3.2%, Als: 0.012%, N: 0.01%, S: 0.016%, Mn: 0.18%, Cu: 0.42%, 其余为 Fe及不可避免的杂质。 将板坯按表 2中不同的再加热制度在加热炉内保温后热轧至厚度为 2.5mm的 热轧板， 其热轧精轧的开轧和终轧温度参考表 2; 酸洗后进行第一次冷轧， 轧 制到 0.60mm厚度后， 在 850°C、 湿氢保护气氛中进行中间脱碳退火， 使钢板 中碳含量降到 30ppm以下； 中间脱碳退火后进行第二次冷轧， 轧制到成品厚 度 0.27mm; 涂布 MgO为主要成分的隔离剂， 成卷后在气氛为 100% H2、 露 点为 -10°C， 温度为 1200 °C的条件下进行 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， 得到的成品磁性能见表 2。 成分、 板坯加热制度及热轧制度对磁性能的影响
板坯加热 精轧终 磁性
精轧开轧温
制度 轧温度 磁感 铁损 说明
度
B8(T) P17/50(W/kg)
1250°C X 800 °C 发明例
1050°C 1.88 1.21
2h
1250°C X 800 °C 发明例
1200 °C 1.88 1.19
2h
1250°C X 850 °C 发明例
1100°C 1.89 1.15
2h
1250°C X 876 °C 发明例
1100°C 1.89 1.12
2h
1280°C X 890 °C 发明例
1100°C 1.90 1.11
2h 1250°C X 869 °C
1070°C 1.90 1.14 发明例 2h
1250°C X 912°C
1130。C 发明例
1.91 1.03
2h
1250°C X 907 °C 发明例
1100°C 1.91 1.02
3h
1280°C X 930°C 发明例
1100°C 1.90 1.06
3h
1250°C X 865 °C 比较例
1100°C 1.66 1.67
1.5h
1280°C X 874 °C 比较例
1100°C 1.68 1.63
1.5h
1280°C X 867 °C 比较例
1000°C 1.79 1.45
3h
1280°C X 948 °C 比较例
1250°C 1.85 1.34
3h
1280°C X 764V 比较例
1100°C 1.82 1.39
3h 实施例 3 :
取向硅钢板坯的组分及重量百分比为 C: 0.032%， Si: 3.2%, Als: 0.012%, N: 0.01%, S: 0.016%, Mn: 0.18%, Cu: 0.42%, 其余为 Fe及不可避免的杂 质。 将其在 1280 °C加热炉内保温 3小时后热轧至厚度为 2.5mm的热轧板， 其 中热轧精轧的开轧和终轧温度分别为 1100 °C和 930 °C ; 酸洗后进行第一次冷 轧， 轧制到 0.60mm厚度后， 在 850 °C、 湿氢保护气氛中进行中间脱碳退火， 使钢板中碳含量降到 30ppm以下； 中间脱碳退火后进行第二次冷轧， 轧制到 成品厚度 0.27mm; 涂布 MgO为主要成分的隔离剂后， 通过施加不同的高温 退火工艺如表 3， 验证其对成品磁性的影响， 后经过涂绝缘涂层及拉伸平整退 火， 得到高温退火工艺对应的成品磁性能见表 3。
表 3 高温退火工艺变化对磁性能的影响
高温退火 1¾温退 退火保 退火 磁性 说明
Figure imgf000008_0001
C00l.0/600ZN3/X3d 6S6.TI/600Z OAV

Claims

权 利 要 求
1、 一种高电磁性能取向硅钢的生产方法， 包括用转炉或电炉炼钢， 钢水 经二次精炼和连铸后， 获得板坯， 之后进行热轧、 第一次冷轧、 脱碳退火、 第二次冷轧， 涂布以氧化镁为主要成分的退火隔离剂， 然后进行高温退火， 最后涂绝缘涂层和进行拉伸平整退火， 其特征在于， 所述板坯的组分 （按重 量百分比计） 为：
C: 0.020%~0.050%
Si: 2.6%~3.6%
S: 0.015%~0.025%
Als: 0.008%~0.028%
N: 0.005%~0.020%
Mn: 0.15%~0.5%, 且 10 Mn/S 20
Cu: 0.3%~1.2%, 且 Cu/Mn 2
其余为 Fe及不可避免的杂质。
2、 如权利要求 1所述的高电磁性能取向硅钢的生产方法， 其特征在于， 所述热轧工艺为： 板坯在加热炉内加热到 1250~1350°C， 保温 2~6小时， 再进 行热轧， 热轧精轧过程的开轧温度为 1050 1200 °C， 终轧温度为 800°C以上。
3、 如权利要求 2所述的高电磁性能取向硅钢的生产方法， 其特征在于， 所述热轧精轧过程的开轧温度为 1070~1130°C， 终轧温度为 850°C以上。
4、 如权利要求 1所述的高电磁性能取向硅钢的生产方法， 其特征在于， 所述高温退火工艺为： 在气氛为氢气或氢气占 75%以上的氮氢混合气、 干气 氛、 温度为 1170~1230°C的条件下进行保温 15小时以上的高温退火。
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CN101545072A (zh) 2009-09-30
US8333846B2 (en) 2012-12-18
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