JP5001611B2 - Method for producing high magnetic flux density grain-oriented silicon steel sheet - Google Patents

Method for producing high magnetic flux density grain-oriented silicon steel sheet Download PDF

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JP5001611B2
JP5001611B2 JP2006247674A JP2006247674A JP5001611B2 JP 5001611 B2 JP5001611 B2 JP 5001611B2 JP 2006247674 A JP2006247674 A JP 2006247674A JP 2006247674 A JP2006247674 A JP 2006247674A JP 5001611 B2 JP5001611 B2 JP 5001611B2
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昭 坂倉
弘 武智
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Nippon Steel Corp
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    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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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
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    • 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
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    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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    • C21D8/1211—Rapid solidification; Thin strip casting
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    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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    • 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
    • C21D8/1222—Hot rolling
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    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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    • 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
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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
    • C21D8/1255—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
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    • 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
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    • 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
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/54—Furnaces for treating strips or wire
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    • 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
    • C21D9/70—Furnaces for ingots, i.e. soaking pits
    • 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
    • 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
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/46—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting
    • 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
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation
    • H—ELECTRICITY
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0233—Manufacturing of magnetic circuits made from sheets

Description

本発明は電力用変圧器の鉄心材や回転機器の鉄心材等に使用される磁性、特に磁束密度に優れた方向性珪素鋼板を製造する方法に関するものである。   The present invention relates to a method for producing a directional silicon steel sheet excellent in magnetism, particularly in magnetic flux density, used for iron core materials for power transformers, iron core materials for rotating equipment, and the like.

方向性珪素鋼板の製造技術はN.P.Gossの２段冷延法として発表（特許文献１）され、その製造原理は微細な析出物ＭｎＳの存在下での２次再結晶現象としてJ.E.May & D.Turnbullにより１９５８年に明らかにされた（非特許文献１）。これとは別に、本発明者らはＡｌ入り１段強冷延法を発明し微細析出物ＡｌＮの有効性を発表（特許文献２）した。一方、析出物とは異なり固溶した，Ｓｂ，Ｎｂ，Ｓｅ，Ｓ，Ｍｏ，Ｃｕ，Ｓｎなどの微量元素が強い１次再結晶粒の成長抑制作用を持ち、これが２次再結晶を促進することを斉藤達雄が初めて発表（非特許文献２）した。この様に現実の製造技術で利用される２次再結晶現象は析出物もしくは固溶した微量元素の存在が不可欠であるが、析出物の全く存在しない状態での２次再結晶現象としては、一定の結晶方位で固められた安定した結晶組織からなる地（Texture Inhibition）の存在下での２次再結晶現象がC.G.Dunnによって基礎的に明らかにされた（非特許文献３）。   The technology for producing grain-oriented silicon steel sheets was announced as a two-stage cold rolling method of NPGoss (Patent Document 1), and the principle of its production is JEMay & D. as a secondary recrystallization phenomenon in the presence of fine precipitates MnS. Revealed in 1958 by Turnbull (Non-Patent Document 1). Apart from this, the present inventors invented the Al-containing one-stage strong cold rolling method and announced the effectiveness of fine precipitates AlN (Patent Document 2). On the other hand, unlike the precipitates, trace elements such as Sb, Nb, Se, S, Mo, Cu, and Sn, which are solid-dissolved, have a strong primary recrystallized grain growth inhibiting action, which promotes secondary recrystallization. Tatsuo Saito announced for the first time (Non-patent Document 2). In this way, the secondary recrystallization phenomenon used in the actual manufacturing technology requires the presence of precipitates or dissolved solid elements, but as a secondary recrystallization phenomenon in the absence of precipitates, The secondary recrystallization phenomenon in the presence of a texture (Texture Inhibition) composed of a stable crystal structure solidified in a certain crystal orientation was basically clarified by CGDunn (Non-patent Document 3).

更に高磁束密度方向性珪素鋼板の製造原理は本発明者らによるＡｌＮの２次再結晶に及ぼす効果によって明らかである（非特許文献４）。即ち、（１１０）［００１］−Ｇｏｓｓ方位単結晶の冷延・再結晶現象に及ぼすＡｌＮの効果について、出発単結晶が５nm以下の極めて微細なＡｌＮを少量含む場合には｛１１１｝＜１１０＞−Ｃ方位の１次再結晶成長組織となり、１０nm前後の微細なＡｌＮをかなり多量に含む場合には２次再結晶によって初方位（１１０）［００１］を再現し、１μｍ前後の比較的大きなＡｌＮを多量に含む場合には同様に２次再結晶によって｛１２０｝＜００１＞−Ａ方位、｛３６２｝＜０１２＞−Ｂ方位、｛１１１｝＜１１０＞−Ｃ方位の３種類の方位の２次再結晶粒が出現する。これは上述したC.G.Dunnによる不純物を全く含まない３％Ｓｉ珪素鋼単結晶の研究結果と完全に一致する。これらの研究成果から、高磁束密度方向性珪素鋼板の製造には１０nm前後のＡｌＮを熱延板の状態で確保することが決定的に重要であることがわかる。
５nm以下の極めて微細なＡｌＮでは２次再結晶は起こらないので避けるべきである。また１μｍ前後の粗大なＡｌＮは存在の意味が無い。 Furthermore, the production principle of the high magnetic flux density directional silicon steel sheet is clear by the effect of the present inventors on the secondary recrystallization of AlN (Non-patent Document 4). That is, regarding the effect of AlN on the cold rolling / recrystallization phenomenon of the (110) [001] -Goss orientation single crystal, when the starting single crystal contains a small amount of very fine AlN of 5 nm or less, {111} <110> When it becomes a primary recrystallization growth structure of -C orientation and contains a very large amount of fine AlN of about 10 nm, the first orientation (110) [001] is reproduced by secondary recrystallization, and a relatively large AlN of about 1 μm In the case where a large amount of is included, two of the three types of orientations {120} <001> -A orientation, {362} <012> -B orientation, and {111} <110> -C orientation 2 are similarly obtained by secondary recrystallization. Next recrystallized grains appear. This completely agrees with the research result of the 3% Si silicon steel single crystal containing no impurities by CGDunn described above. From these research results, it can be seen that it is critically important to secure AlN of about 10 nm in the state of hot-rolled sheet for the production of high magnetic flux density directional silicon steel sheet.
Secondary recrystallization does not occur with very fine AlN of 5 nm or less and should be avoided. In addition, coarse AlN of about 1 μm is meaningless.

従来、高磁束密度方向性珪素鋼板の製造に必要不可欠な存在である１０nm前後のＡｌＮを熱延板の状態で確保するためには、分塊圧延もしくは連続鋳造によって得られたスラブ（厚さ凡そ２００mm以上）を１３００℃以上の高温に再加熱（火焔加熱）してＡｌＮを一旦完全に固溶した後、連続熱延機の粗圧延機を用いて２０mm〜７０mm厚のバー（Ｂａｒ）とし、更に連続熱間仕上圧延機で圧延して最終板厚とし、ほぼ５００℃前後で巻取ることにより行っていたが、仕上げ圧延の際に鋼は急速冷却されていた。しかしながら、２００mm厚前後の厚手スラブでは、１３５０℃以上の高温で火焔加熱する場合にスラブ表面と下面の温度差が大きく目的とする効果を挙げるためには表面温度を極端に高くする必要に迫られ、そのためスラブ結晶粒の異常成長や、珪素鋼表面のスケールが溶解し炉内に堆積することによる作業上の問題点も発生していた。   Conventionally, in order to secure AlN of around 10 nm, which is indispensable for the production of high magnetic flux density grain-oriented silicon steel sheets, in the state of hot-rolled sheets, a slab (thickness approximately) obtained by split rolling or continuous casting. 200 mm or more) is reheated to a high temperature of 1300 ° C. or more (fired heating) to completely dissolve AlN once, and then a 20 mm to 70 mm thickness bar is formed using a continuous hot rolling machine. Furthermore, it was rolled by a continuous hot finish rolling mill to obtain a final plate thickness and wound at about 500 ° C., but the steel was rapidly cooled during finish rolling. However, for thick slabs around 200 mm thick, when the flame is heated at a high temperature of 1350 ° C. or higher, the temperature difference between the slab surface and the bottom surface is large, and in order to achieve the desired effect, the surface temperature must be extremely increased. For this reason, abnormal growth of slab crystal grains and work problems caused by the scale of the silicon steel surface being melted and deposited in the furnace have also occurred.

この問題点を解決することは非常に困難ではあるが、一つの製造方法として低温スラブ加熱法（非特許文献５）の採用や火焔加熱のあと最終段階での加熱を誘導加熱で行うことにより酸化スケールの溶解を防ぐ方法（例えば、特許文献３）などがある。更に１０nm前後の好ましいＡｌＮを熱延板と同一の厚みで確保するために、数mm厚の薄肉連続鋳造法（例えば、特許文献４，）を採用する考え方も発表されているが、従来の厚手ＣＣスラブを一旦冷却後、この冷スラブを再加熱する方法は生産性や作業性に問題があり、改善が望まれている。   Although it is very difficult to solve this problem, it is oxidized by adopting a low-temperature slab heating method (Non-patent Document 5) as one manufacturing method or induction heating at the final stage after flame heating. There exists a method (for example, patent document 3) etc. which prevent melt | dissolution of a scale. Furthermore, in order to secure preferable AlN of about 10 nm with the same thickness as the hot-rolled sheet, a concept of adopting a thin continuous casting method (for example, Patent Document 4) with a thickness of several millimeters has been announced. The method of reheating the cold slab after once cooling the CC slab has problems in productivity and workability, and improvement is desired.

さらに、厚さ２０〜８０mmの薄スラブを連続鋳造で製造し、圧延開始温度を１１００〜１２００℃とする熱間圧延を採用して方向性電磁鋼板を製造する方法が特許文献５に開示されている。しかしこの方法では、熱延中に粒寸法の大きなＡｌＮが形成され、通常の処理工程では十分な磁気特性が得られないので、脱炭焼鈍後の窒化処理を必要とする。
：米国特許１，９６５，５５９ ：特公昭３３−４７１０，Ｕ．Ｓ．Ｐ．３，１５９，５１１ （１９６２） ：特開平０５−１１７７５１号公報 ：特開平０２−２５８９２２号公報 ：特表２００−５００５６８号公報 ：Trans. AIME,，２１２（１９５８），７６９ ：斎藤達夫 日本金属学会誌, ２７（１９６３），１９１ ：Acta Metallurgica, １（１９５３），１６３ ：坂倉昭，ふぇらむ，Ｖｏｌ．９，Ｎｏ．２（２００４），５２ ：N.Takahashi,J.Harase, Mater.Sci.Forum,２０４／２０６， Ｎｏ．Ｐｔ１（１９９６），１４３ Further, Patent Document 5 discloses a method of manufacturing a grain-oriented electrical steel sheet by manufacturing a thin slab having a thickness of 20 to 80 mm by continuous casting and employing hot rolling with a rolling start temperature of 1100 to 1200 ° C. Yes. However, in this method, AlN having a large grain size is formed during hot rolling, and sufficient magnetic properties cannot be obtained in a normal processing step. Therefore, nitriding after decarburization annealing is required.
: US Patent 1,965,559 : JP-B 33-4710, U.D. S. P. 3,159,511 (1962) : JP-A-05-117751 : JP-A-02-258922 : Special table 200-500568 : Trans. AIME, 212 (1958), 769 : Tatsuo Saito Journal of the Japan Institute of Metals, 27 (1963), 191 : Acta Metallurgica, 1 (1953), 163 : Akira Sakakura, Ferum, Vol. 9, no. 2 (2004), 52 : N. Takahashi, J. Harase, Mater. Sci. Forum, 204/206, No. Pt1 (1996), 143

上記したように、従来、高磁束密度方向性珪素鋼板の製造に必要な微細ＡｌＮの分散析出効果は、厚手スラブの熱延均熱炉による高温再加熱作業によって一旦ＡｌＮを珪素鋼中に固溶したのち再び熱間圧延による急速冷却効果によって達成していたが、厚手スラブの高温加熱のスケール溶解による問題があり、また、数mm厚の薄肉連続鋳造法では結晶方位の問題や鋳造組織の脆性の問題があり、実用化を阻害する大きな問題点である。
さらに中肉の連鋳スラブを１２００℃以下の温度で熱間圧延を開始する方法では、熱延前にＡｌＮが析出し、かつ粗大化し、磁性の改善に十分効果のある状態には至っていない。 As described above, conventionally, the effect of dispersion and precipitation of fine AlN necessary for the production of a high magnetic flux density grain-oriented silicon steel sheet is that AlN is once dissolved in silicon steel by a high-temperature reheating operation using a hot slab of a thick slab. After that, it was achieved again by the rapid cooling effect by hot rolling, but there was a problem due to the high temperature heating scale melting of thick slabs, and the problem of crystal orientation and brittleness of the cast structure in the thin continuous casting method of several mm thickness This is a major problem that hinders practical application.
Furthermore, in the method of starting hot rolling of a continuous cast slab of medium thickness at a temperature of 1200 ° C. or less, AlN is precipitated and coarsened before hot rolling, and has not reached a state that is sufficiently effective for improving magnetism.

本発明は連続鋳造法により中肉厚スラブを製造し、スラブを熱延可能な最低限以上の温度に保持し、かつ溶鋼の状態で既に固溶しているＡｌＮを連続熱間圧延を行うまでは析出させることなく鋼中に保持した上で、連続熱間圧延の際の急速冷却効果によって微細に析出させることにより、厚手ＣＣスラブを一旦冷却した後、このスラブを１３５０℃以上の高温に加熱する従来の方法における問題点を解消でき、大幅な作業効率とエネルギー効率の向上でき、かつ従来より均一で優れた結晶方向性と鉄損を有する高磁束密度方向性珪素鋼板の製造方法を提供することを目的とする。   The present invention produces a medium-thick slab by a continuous casting method, maintains the slab at a temperature that is at least a minimum that can be hot-rolled, and performs continuous hot rolling of AlN that has already been dissolved in a molten steel state. Is kept in the steel without precipitation, and after the thick CC slab is cooled once by fine precipitation by the rapid cooling effect during continuous hot rolling, the slab is heated to a high temperature of 1350 ° C or higher. The present invention provides a method for producing a high-flux-density directional silicon steel sheet that can solve the problems in the conventional method, can greatly improve work efficiency and energy efficiency, and has a more uniform and superior crystal directionality and iron loss than conventional ones. For the purpose.

上記目的を達成するために本発明の構成は以下の通りである。すなわち、
（１）質量で Ｃ：０．０１０〜０．０７５％，Ｓｉ：２．９５〜４．０％，酸可溶性Ａｌ：０．０１０〜０．０４０％，Ｎ：０．００１０〜０．０１５０％，Ｓ或いはＳｅを単独または双方で０．００５〜０．１％を含み、残部Ｆｅおよび不可避的不純物からなる溶鋼を連続的に鋳造して厚さ２０〜７０mmの中肉厚バーを製造し、該バーを鋳造後或いは加熱炉より抽出後（加熱炉の在炉時間を含めて）１２００℃超（好ましくは１３５０℃未満）の温度間に、かつ５００秒以内に熱間仕上圧延機の入口に到達せしめて熱間連続圧延を開始し、該熱延で１．５mm〜５mm厚の熱延板とし、熱延終了後６００℃に達するまでの冷却時間を１５０秒以下とすることを特徴とし、以下通常の冷延、中間焼鈍、脱炭焼鈍、仕上焼鈍等を行う高磁束密度方向性珪素鋼板の製造方法。
（２）上記溶鋼中に、さらに粒界に偏析して結晶成長を抑制する，Ｓｂ：０．００５〜０．２％，Ｎｂ：０．００５〜０．２％、Ｍｏ：０．００３〜０．１、Ｃｕ：０．０２〜０．２％、Ｓｎ：０．０２〜０．３％の群から選ばれた少なくとも１種を含有することを特徴とする前記（１）に記載の高磁束密度方向性珪素鋼板の製造方法。
（３）前記中肉厚バーが１２５０℃以上の温度を保持している場合には最長でも５００秒以内に、１２００℃以上の温度を保持している場合には１５０秒以内に熱間仕上圧延機の入口に到達せしめることを特徴とする前記（１）に記載の高磁束密度方向性珪素鋼板の製造方法。
（４）連続鋳造で製造した中肉厚バーを熱間仕上圧延機の入口に到達せしめて熱間連続圧延を開始するまでの所用時間が２００秒を超える場合、或いは該バーの温度が１０００℃のように低温である場合には、これらのバーを１３００〜１３５０℃の温度に保持するための加熱炉を通すことを特徴とする前記（１）に記載の高磁束密度方向性珪素鋼板の製造方法。 In order to achieve the above object, the configuration of the present invention is as follows. That is,
(1) By mass C: 0.010 to 0.075%, Si: 2.95 to 4.0%, acid-soluble Al: 0.010 to 0.040%, N: 0.0010 to 0.0150% , S or Se alone or both in an amount of 0.005 to 0.1%, continuously casting a molten steel composed of the remaining Fe and inevitable impurities to produce a medium-thickness bar having a thickness of 20 to 70 mm, After the bar is cast or extracted from the heating furnace (including the in-furnace time of the heating furnace) at a temperature exceeding 1200 ° C. (preferably less than 1350 ° C.) and within 500 seconds, enter the hot finish rolling mill at the inlet. The hot rolling is started to reach 1.5 mm to 5 mm thickness by hot rolling, and the cooling time until reaching 600 ° C. after the hot rolling is 150 seconds or less, High magnetic flux density directionality for normal cold rolling, intermediate annealing, decarburization annealing, finish annealing, etc. A method for producing a silicon steel sheet.
(2) In the molten steel, further segregation at grain boundaries to suppress crystal growth, Sb: 0.005 to 0.2%, Nb: 0.005 to 0.2%, Mo: 0.003 to 0 0.1, Cu: 0.02 to 0.2%, Sn: at least one selected from the group of 0.02 to 0.3%, the high magnetic flux according to (1) above A method for producing a density-oriented silicon steel sheet.
(3) Hot finish rolling within 500 seconds at the longest when the medium-thickness bar maintains a temperature of 1250 ° C or higher, and within 150 seconds when the temperature of 1200 ° C or higher is maintained. The method for producing a high magnetic flux density directional silicon steel sheet according to (1), wherein the method reaches the entrance of the machine.
(4) When the required time to reach the entrance of the hot finishing mill after the medium thickness bar manufactured by continuous casting exceeds 200 seconds or when the temperature of the bar is 1000 ° C. When the temperature is low as in the above, the high magnetic flux density directional silicon steel sheet according to the above (1), which is passed through a heating furnace for maintaining these bars at a temperature of 1300 to 1350 ° C. Method.

本発明のように、連続鋳造で製造した中肉鋳片に完全に固溶した状態から熱間圧延仕上圧延機（タンデムミル）での急速冷却で得られるＡｌＮは、均一でしかも微細に分散しており、優れた結晶方位を持つ１次再結晶核を生成するに充分であると同時に、結晶成長の抑制効果も充分であり、且つ鋳造で得られた結晶組織は熱延によって破壊されているので、従来の高温加熱によるスラブの異常成長粒の悪影響もなく、最終焼鈍で均一かつ完全な２次再結晶粒を形成し、磁束密度Ｂ10≧１．９０Ｔの優れた特性を有する高磁束密度方向性珪素鋼板を得ることができる。しかも、従来のスラブ加熱炉による１３５０℃という高温再加熱作業は全く不要となり、鋼片の保有熱は完全に活用されるため著しいエネルギー効率の向上に帰することになり、従来法の難点と考えられていたスラブ高温加熱による作業上の大きな課題も解決できる。   As in the present invention, AlN obtained by rapid cooling in a hot rolling finish rolling mill (tandem mill) from a state in which it is completely dissolved in a solid cast piece produced by continuous casting is uniformly and finely dispersed. It is sufficient to generate primary recrystallized nuclei with excellent crystal orientation, and at the same time, it has a sufficient effect of suppressing crystal growth, and the crystal structure obtained by casting is destroyed by hot rolling. Therefore, there is no adverse effect of the abnormally grown grains of the slab by conventional high-temperature heating, and uniform and complete secondary recrystallized grains are formed by final annealing, and the magnetic flux density direction has excellent characteristics of magnetic flux density B10 ≧ 1.90T. -Resistant silicon steel sheet can be obtained. Moreover, the high-temperature reheating operation of 1350 ° C. in the conventional slab heating furnace is completely unnecessary, and the retained heat of the steel slab is fully utilized, which leads to a significant improvement in energy efficiency. It can also solve the major work problems caused by high-temperature heating of slabs.

以下に本発明を詳細に説明する。
まず、本発明の溶鋼中に含有する各成分の限定理由を説明する。
ＣはＳｉ量に応じて熱延中に一定のγ変態を生じせしめるために必要な元素であり、０．０１０％未満では２次再結晶を安定して生成できない。また０．０７５％を超えると脱炭焼鈍時間が長くなり、生産上好ましくないのでその含有量を０．０１０〜０．０７５％にした。
Ｓｉは２．９５％未満では高級高磁束密度方向性珪素鋼板としては優れた鉄損値が得られない。また、４％を超えて添加すると脆性のために冷間圧延時に割れ等が発生するので好ましくなく、その含有量を２．９５〜４．０％にした。
酸化溶性ＡｌおよびＮはインヒビターとして適当なＡｌＮを生成させるために必要な元素であり、且つそのために十分な量として０．０１０〜０．０４０％，０．００１０〜０．０１５０％の範囲とした。
Ｓ，ＳｅはＭｎとＭｎＳ、ＭｎＳｅを形成し、２次再結晶のための析出分散相として作用する。そのためにこれらを単独または双方で０．００５％〜０．０１５％含有させる。その他、必要に応じ、インヒビターを強くする目的でＳｂ：０．００５〜０．２％，Ｎｂ：０．００５〜０．２％、Ｍｏ：０．００３〜０．１、Ｃｕ：０．０２〜０．２％、Ｓｎ：０．０２〜０．３％の群から選ばれた少なくとも１種を含有させる事ができる。 The present invention is described in detail below.
First, the reason for limitation of each component contained in the molten steel of the present invention will be described.
C is an element necessary for causing a certain γ transformation during hot rolling depending on the amount of Si, and if it is less than 0.010%, secondary recrystallization cannot be stably generated. On the other hand, if it exceeds 0.075%, the decarburization annealing time becomes longer, which is not preferable for production, so the content is made 0.010 to 0.075%.
If Si is less than 2.95%, an excellent iron loss value cannot be obtained as a high-grade high magnetic flux density directional silicon steel sheet. Further, if added over 4%, it is not preferable because cracks and the like occur during cold rolling due to brittleness, and its content is set to 2.95 to 4.0%.
Oxidation-soluble Al and N are elements necessary for producing AlN suitable as an inhibitor, and the sufficient amount thereof is in the range of 0.010 to 0.040% and 0.0010 to 0.0150%. .
S and Se form Mn, MnS, and MnSe, and act as a precipitated dispersed phase for secondary recrystallization. Therefore, these are contained individually or in an amount of 0.005% to 0.015%. In addition, Sb: 0.005 to 0.2%, Nb: 0.005 to 0.2%, Mo: 0.003 to 0.1, Cu: 0.02 to strengthen the inhibitor as necessary. At least one selected from the group of 0.2% and Sn: 0.02 to 0.3% can be contained.

本発明の高磁束密度方向性珪素鋼鈑を製造するには熱延板の状態で１０nm前後（５〜５０nm）のＡｌＮを存在させることが必須であり、そのために、連続鋳造等の手段で２０〜７０mmの中肉厚バーを製造し、このバーの保有熱、或いは保熱炉等の温度降下を防止する加熱手段によってＡｌＮの固溶状態を保ちながら、バー温度が１２００℃以上の場合には保熱炉抽出後最大でも１５０秒以内で、１２５０℃以上の場合には最大でも５００秒以内で熱間圧延機入り口まで移行させ、熱間圧延で１．５mm〜５mm厚の熱延板とし、熱延終了後６００℃に達するまでの冷却時間を１５０秒以下とすることにより、１０nm近傍（５〜５００nm）の微細なＡｌＮを析出させる。   In order to produce the high magnetic flux density directional silicon steel sheet of the present invention, it is essential that AlN having a thickness of about 10 nm (5 to 50 nm) be present in the state of a hot-rolled sheet. If the bar temperature is 1200 ° C or higher while manufacturing a medium-thickness bar of ~ 70mm and maintaining the solid solution state of AlN by the heating means to prevent the heat retention of this bar or the temperature drop of heat insulation furnace etc. Within 150 seconds at the maximum after extraction from the heat-retaining furnace, when the temperature is 1250 ° C. or higher, the transition to the hot rolling mill entrance is performed within 500 seconds at the maximum, and hot rolled steel sheet having a thickness of 1.5 mm to 5 mm by hot rolling, By setting the cooling time until reaching 600 ° C. after the hot rolling to 150 seconds or less, fine AlN in the vicinity of 10 nm (5 to 500 nm) is deposited.

本発明でバーを２０〜７０mmの中肉厚さに限定したのは、２０mm未満では保熱に大きな設備が必要となり、また７０mmを超えると仕上圧延機のみでは熱延板を得ることができず、粗圧延機が必要になり、経済的生産が達成されないためである。   In the present invention, the bar is limited to a medium thickness of 20 to 70 mm. If it is less than 20 mm, a large facility for heat retention is required. If it exceeds 70 mm, a hot rolled sheet cannot be obtained only by a finishing mill. This is because a roughing mill is required and economic production is not achieved.

２０〜７０mm厚のバーを製造し、圧延する手段は特に限定しない。公知の連続鋳造−熱間圧延連続設備の例を図１及び図２に模式的に示した。図１は鋳型１より抽出した中肉スラブ２を連続鋳造し、切断したスラブ３を一定の温度保持のために保熱炉４に装入したあと直ちに連続仕上熱延機５で圧延して薄手熱延帯鋼を巻取６っている。また、図２は中肉スラブ２を連続鋳造した後、巻取ってコイル７とし、該コイルをコイルボックス８に装入して温度の均一化を図った後、連続仕上熱延機５で圧延し巻き取る装置である。   The means for producing and rolling a 20 to 70 mm thick bar is not particularly limited. An example of a known continuous casting-hot rolling continuous equipment is schematically shown in FIGS. FIG. 1 shows that a thin slab 2 extracted from a mold 1 is continuously cast, and the cut slab 3 is inserted into a heat-retaining furnace 4 in order to maintain a constant temperature, and then immediately rolled by a continuous finishing hot rolling machine 5 to make it thin. Hot-rolled steel strip is wound up. In FIG. 2, after the continuous slab 2 is continuously cast, it is wound to form a coil 7, and the coil is inserted into the coil box 8 to equalize the temperature, and then rolled by the continuous finishing hot rolling machine 5. A device for winding and winding.

次いで図３および図４を用いて中肉厚バーの処理条件について説明する。
質量％で０．０４５％Ｃ，３．２０％Ｓｉ，０．０２５％Ａｌ，その他不純物を含有する珪素鋼鋼塊を圧延して４０mm厚のバーを出発素材とし、これを４分割して以下の実験を試みた。これらをバー加熱炉で１３００℃で３時間保持してＡｌＮを完全に地鉄中に固溶させた後放冷し、この４種類のバーが１２５０℃，１２１０℃，１１００℃，１０００℃の温度になった時点で直ちに夫々１２５０℃，１２１０℃，１１００℃，１０００℃の温度に保った炉中に装入し、夫々１２５０℃で４８０秒間（バー加熱炉抽出後合計５００秒間）、１２１０℃で１２０秒間（同合計１５０秒間）、１１００℃で５０秒間（同合計１００秒間）、１０００℃で２０秒間（同合計５０秒間）保持後熱間圧延し、圧延終了後は大気中に放冷した。この熱履歴を総合的に図示したのが図４である。この図で曲線（Ａ）はバー加熱炉抽出後直ちに圧延を行った場合の冷却曲線、（Ｂ），（Ｃ），（Ｄ，（Ｅ）の冷却曲線は夫々上で述べた通りである。
この熱延板を冷延し、脱炭し、仕上焼鈍して最終製品とし、該製品の磁気特性（Ｂ10）を測定し、この特性と熱履歴（バー加熱炉を抽出後、保熱炉在炉時間も含めて仕上圧延機入口に到達するまでの合計時間）との関係を図３に示した。
図３から明らかな様に、図４（Ａ）の冷却曲線で示される熱延を行った場合には、保持時間が０であるため磁気特性は図３の黒丸１で示されるように最も優れたＢ10特性を示し、図４の（Ｂ）の１０００℃に２０秒保持した後熱延を行った場合の磁気特性は図３の白丸２で示されるように保持時間が短いにもかかわらずＢ10特性はかなりの劣化を示し、１００秒を超えれば２次再結晶そのものも不安定となる。
更に図４の（Ｃ）の１１００℃に５０秒保持した後熱延を行った場合の磁気特性は図３の半黒丸３で示されるように、保持時間は長いが温度が高いためにやや改善されている。更に図４の（Ｄ）の１２００℃超に１２０秒間保持した後熱延を行った場合の磁気特性は図３の黒丸４で示されるように、保持時間は長くても温度を高くすることにより最良値に近い値を示している。
最後に図４の（Ｅ）の１２５０℃に４８０秒間保持した後熱延を行った場合の磁気特性は図３の小黒丸５で示されるように、非常に長い保持時間であるにもかかわらず最良値に比較すればやや劣る程度の値を示している。
この様にバー温度の低下はＢ10特性に対して致命的であるが、１２００℃を超えて高い温度を確保すれば保持時間に猶予を与えることも可能となり、優れた特性が得られることが分かった。 Next, the processing conditions for the medium thickness bar will be described with reference to FIGS. 3 and 4.
Roll a silicon steel ingot containing 0.045% C, 3.20% Si, 0.025% Al, and other impurities in mass% to start a 40mm-thick bar, and divide this into 4 parts. I tried the experiment. These were kept in a bar heating furnace at 1300 ° C for 3 hours, and AlN was completely dissolved in the ground iron and then allowed to cool. These four bars had temperatures of 1250 ° C, 1210 ° C, 1100 ° C and 1000 ° C. Were immediately placed in furnaces maintained at temperatures of 1250 ° C., 1210 ° C., 1100 ° C., and 1000 ° C., respectively, at 1250 ° C. for 480 seconds (total of 500 seconds after bar heating furnace extraction), and at 1210 ° C. After holding for 120 seconds (same total 150 seconds), 1100 ° C. for 50 seconds (same total 100 seconds), and 1000 ° C. for 20 seconds (same total 50 seconds), hot rolling was performed, and after rolling, it was allowed to cool to the atmosphere. FIG. 4 shows the overall heat history. In this figure, the curve (A) is a cooling curve when rolling is performed immediately after extraction from the bar heating furnace, and the cooling curves of (B), (C), (D, (E) are as described above.
This hot-rolled sheet is cold-rolled, decarburized, finish-annealed to obtain the final product, and the magnetic properties (B10) of the product are measured. FIG. 3 shows the relationship with the total time required to reach the finishing mill entrance including the furnace time.
As is apparent from FIG. 3, when the hot rolling shown by the cooling curve in FIG. 4 (A) is performed, the retention time is 0, so that the magnetic characteristics are the best as shown by the black circle 1 in FIG. 4B, the magnetic properties when hot rolling is performed after holding at 1000 ° C. for 20 seconds in FIG. 4 (B) are shown in FIG. The characteristics show considerable deterioration, and if the time exceeds 100 seconds, the secondary recrystallization itself becomes unstable.
Further, the magnetic characteristics when hot rolling is performed after holding at 1100 ° C. for 50 seconds as shown in FIG. 4 (C) are slightly improved because the holding time is long but the temperature is high as shown by the half-black circle 3 in FIG. Has been. Furthermore, as shown in the black circle 4 in FIG. 3, the magnetic characteristics when the film is hot rolled after being held at 1200 ° C. for 120 seconds in FIG. 4 (D) can be obtained by increasing the temperature even if the holding time is long. A value close to the best value is shown.
Finally, as shown in FIG. 4 (E), when the magnetic rolling is performed after holding at 1250 ° C. for 480 seconds and then performing hot rolling, the small black circle 5 in FIG. 3 shows a very long holding time. Compared to the best value, the value is slightly inferior.
In this way, the decrease in the bar temperature is fatal to the B10 characteristics, but it is possible to give a grace period to the holding time if a high temperature exceeding 1200 ° C. is secured, and it is found that excellent characteristics can be obtained. It was.

図４の（Ｂ）、（Ｃ）の冷却曲線に示される熱延を行った場合には、図３から明らかなように、圧延前の保持温度が充分ではなく、これらの場合には何れもＡｌＮの析出が進行して磁性の劣化をきたすことが示された。また図４の（Ｃ）の冷却曲線の場合には、極めて短時間に熱延機入口に到達できればある程度の磁性を確保することが可能ではあるが、製造現場での条件から判断すると、少なくとも図４（Ｄ）もしくは図４（Ｅ）の冷却曲線に沿った熱履歴でないと生産作業が出来ないことが明らかである。   When the hot rolling shown in the cooling curves of FIGS. 4B and 4C is performed, as is apparent from FIG. 3, the holding temperature before rolling is not sufficient. It has been shown that precipitation of AlN proceeds and causes magnetic deterioration. In the case of the cooling curve in FIG. 4C, it is possible to ensure a certain degree of magnetism if it can reach the hot rolling machine inlet in an extremely short time. It is clear that the production work cannot be performed unless the thermal history is along the cooling curve of 4 (D) or FIG. 4 (E).

高磁束密度方向性珪素鋼板として鉄損値が重要視される３．０〜４．０％Ｓｉの場合には、Ｓｉ量が３％未満の低い場合に比べると、前記［００１５］項で述べたように、処理条件がかなり厳しく、生産作業上許容される時間は比較的短い。その理由は低Ｓｉの場合にはγ変態によってＡｌＮの固溶度が増すために析出が防止できるからである。従って、高いＳｉ量の場合には、析出防止の手段として温度を利用するしかない。その意味はＡｌＮの析出が温度が高ければ高いほど急速に遅れるので、仕上熱延機の入口に到達するのに時間が必要な場合には保持温度を高くすることを考えればよい。即ち、請求項４にあるように、連続鋳造で製造した中肉厚バーを熱間仕上圧延機の入口に到達せしめて熱間連続圧延を開始するまでの所用時間が２００秒を超える場合には、該バーを１２５０〜１３５０℃の温度に保持するための加熱炉を通す方法や、更に該バーの温度が１０００℃のように低温である場合にも該バーを１２５０〜１３５０℃の温度に保持するための加熱炉を通すような手段でＡｌＮの析出を防止することができる。   In the case of 3.0 to 4.0% Si in which the iron loss value is regarded as important as a high magnetic flux density grain-oriented silicon steel sheet, it is described in the above [0015] section as compared with the case where the Si content is less than 3%. As described above, the processing conditions are quite severe, and the time allowed for production work is relatively short. The reason is that in the case of low Si, precipitation is prevented because the solid solubility of AlN is increased by the γ transformation. Therefore, in the case of a high Si content, temperature can only be used as a means for preventing precipitation. The meaning is that the higher the temperature of AlN precipitation, the more rapidly it delays. Therefore, if it takes time to reach the inlet of the finishing hot rolling machine, the holding temperature should be increased. That is, as described in claim 4, when the required time to reach the inlet of the hot finishing mill after the medium thickness bar manufactured by continuous casting exceeds 200 seconds is required. , A method of passing through a heating furnace for maintaining the bar at a temperature of 1250 to 1350 ° C., and further maintaining the bar at a temperature of 1250 to 1350 ° C. even when the temperature of the bar is as low as 1000 ° C. Precipitation of AlN can be prevented by such means as passing through a heating furnace.

図５は０．０４６％Ｃ，３．１０％Ｓｉ，０．０２９％Ａｌの珪素鋼鋼塊を圧延して４０mm厚のバーとし１３５０℃で３０分加熱後直ちに圧延して略１０００℃で３．５厚の熱延板に仕上げ、これを熱延終了直後の冷却過程から水冷して５通りの熱延板を作成し、冷延し、脱炭し、仕上焼鈍して最終製品とした際の磁気特性と上記熱履歴との関係を図示したものである。図中太線は熱延後の冷却（水冷）開始点を示し、細線は磁気特性（Ｂ10）を示す。
この結果から、熱延終了後の材料はできる限り早い時期から急速冷却処理を行うこと、即ち、熱延終了後１５０秒を超えない範囲で、ａのような緩冷却（大気中放冷）でなく．ｂ．ｃ．ｄ．ｅのように高い温度から、できる限り速い速度で冷却を行うことが磁気特性を得るために必要となる。例えば、ｅの場合ではＢ10＝１．９５Ｔと高い値が得られる。１５０秒を超えない範囲で冷却する温度は少なくとも６００℃とする。通常熱延鋼板は６００℃以下になると巻き取られ、ゆっくり冷却されるためＡｌＮの析出はしなくなる。 FIG. 5 shows that a 0.046% C, 3.10% Si, 0.029% Al silicon steel ingot is rolled into a 40 mm thick bar, heated at 1350 ° C. for 30 minutes, and then immediately rolled to approximately 1000 ° C. at 3 ° C. When finished into a 5-thick hot-rolled sheet and water-cooled from the cooling process immediately after the end of hot-rolling to create 5 types of hot-rolled sheets, cold-rolled, decarburized, and finished annealed to obtain the final product 2 shows the relationship between the magnetic characteristics and the thermal history. The thick line in the figure indicates the starting point of cooling (water cooling) after hot rolling, and the thin line indicates the magnetic properties (B10).
From this result, the material after completion of hot rolling should be subjected to rapid cooling treatment from the earliest possible timing, that is, by slow cooling (cooling in the air) as in a range not exceeding 150 seconds after completion of hot rolling. Without. b. c. d. In order to obtain magnetic characteristics, it is necessary to perform cooling at a speed as fast as possible from a high temperature as in e. For example, in the case of e, a high value of B10 = 1.95T is obtained. The temperature for cooling in a range not exceeding 150 seconds is at least 600 ° C. Usually, a hot-rolled steel sheet is wound up when it is 600 ° C. or lower, and is cooled slowly, so that AlN does not precipitate.

図６に熱延冷却サイクルとＡｌＮ析出量との関係を示した。参考のために低Ｓｉ（１．１２％Ｓｉ，２．１７％Ｓｉ）の場合の析出曲線を併記したが、これとの比較から分るようにＳｉ量が３．１０% の場合では１２５０℃前後からＡｌＮの析出が始まり、１２００℃以下では急速に進むのに対して１．１％Ｓｉの場合は１０００℃までＡｌＮの析出はほとんど進行せず、１０００℃以下で初めて析出してくる。
これは材料のα−γ変態領域が含有Ｃ及びＳｉ量によって増減し、ＡｌＮの析出挙動がこのγ変態の量と密接に関係しているからである。 FIG. 6 shows the relationship between the hot rolling cooling cycle and the AlN precipitation amount. For reference, the precipitation curve in the case of low Si (1.12% Si, 2.17% Si) is also shown. As can be seen from the comparison with this, it is 1250 ° C. when the Si amount is 3.10%. Precipitation of AlN begins and progresses rapidly at 1200 ° C. or less, whereas in the case of 1.1% Si, AlN deposition hardly progresses to 1000 ° C., and begins to precipitate at 1000 ° C. or less.
This is because the α-γ transformation region of the material increases or decreases depending on the amount of contained C and Si, and the precipitation behavior of AlN is closely related to the amount of γ transformation.

以上を総括してＡｌＮによる結晶成長抑制効果を利用して優れた高磁束密度方向性珪素鋼板を製造する場合の熱間圧延条件は下記の通りとなる。
（１）２．９５〜４％Ｓｉを含有する珪素鋼素材でＡｌＮを完全に固溶した中肉厚バーを熱延する場合、該バーを鋳造後或いは加熱炉より抽出後、その保持温度に応じて１２５０℃以上である場合には最長でも５００秒以内に、１２００℃超である場合には好ましくは１５０秒以内に熱間仕上圧延機の入口に到達せしめて熱間圧延を開始する。
（２）上記熱延終了後の冷却は最大でも６００℃までの時間が１５０秒を超えないことである。高温からの冷却によってＡｌＮは析出するが、この際時間をかけて徐々に冷却すればＡｌＮは時間の経過と共に粗大化し極端な場合には１μm 程度のサイズとなり本発明の目的には全く意味の無い形態になってしまう。完全に固溶した状態のＡｌＮが６００℃まで１５０秒を超えない時間で冷却されると、析出サイズは略１０nm前後となり本発明に好ましい状態となる。 In summary, the hot rolling conditions for producing an excellent high magnetic flux density grain-oriented silicon steel sheet by utilizing the effect of suppressing crystal growth by AlN are as follows.
(1) When hot rolling a medium thickness bar in which AlN is completely dissolved in a silicon steel material containing 2.95 to 4% Si, the bar is heated to the holding temperature after casting or extraction from a heating furnace. Accordingly, when the temperature is 1250 ° C. or higher, the hot rolling is started by reaching the inlet of the hot finishing mill within 500 seconds at the longest, and preferably when the temperature is higher than 1200 ° C. within 150 seconds.
(2) The cooling after the end of the hot rolling is that the time to 600 ° C. does not exceed 150 seconds at the maximum. AlN is precipitated by cooling from a high temperature. At this time, if it is gradually cooled over time, the AlN coarsens with the passage of time and becomes about 1 μm in an extreme case, and has no meaning for the purpose of the present invention. It becomes a form. When AlN in a completely solid solution is cooled to 600 ° C. for a time not exceeding 150 seconds, the precipitation size becomes approximately 10 nm, which is a preferable state for the present invention.

以下に本発明を実施例に基づいて説明する。
［実施例１］
質量％で、０．０４５％Ｃ，３．０５％Ｓｉ，０．０３２％Ａｌを含み残部Ｆｅ及び不可避的不純物からなる（残部規定は以下の実施例も同じにつき記述省略）珪素鋼溶鋼を連続鋳造機（以下ＣＣ機という）で６０mm厚のバーとし、直ちに仕上熱延して３．０mm厚とした。仕上熱延入口温度はバー頭部が１２１０℃、尻部が１２０５℃であった。熱延板のＣ量は０．０４１％で僅かに脱炭が起こっている。これを先ず圧下率３０％の冷延をして２．１mm厚とし次いで１１００℃で２分間窒素中で焼鈍した後ジェット気流を吹き当てて冷却した。冷却速度は１１００℃から８５０℃までが約１８秒、８５０℃から４００℃までが約２７秒であった。この焼鈍後のＡｌＮは０．００５５％（ＮａｓＡｌＮ）と分析された。次にこれを８３．３％の圧延率で冷延して０．３５mm厚とした後８００℃で３分間水素中で脱炭した後１２００℃で２０時間焼鈍した。製品の圧延方向におけるＢ10特性は１．９３Ｔ，Ｗ17/50は１．１５Ｗ／kgであった。
［比較例］実施例１と同じ成分のバーを仕上熱延機入口の前でほぼ４０秒間放置した後、仕上げ熱延を開始した。その際のバーの仕上圧延開始温度はバー頭部が１１５０℃、尻部が１１２０℃であった。その後実施例１と同様に処理し、最修成品の２次再結晶率発生率を調べたところ、ほぼ５０％であり、成品には成らなかった。 The present invention will be described below based on examples.
[Example 1]
Containing 0.045% C, 3.05% Si, 0.032% Al, the balance being Fe and unavoidable impurities (the remainder is omitted in the following examples as well), and silicon steel molten steel is continuously used. The bar was 60 mm thick with a casting machine (hereinafter referred to as “CC machine”) and immediately finished and hot rolled to a thickness of 3.0 mm. The finishing hot rolling inlet temperature was 1210 ° C. at the bar head and 1205 ° C. at the bottom. The amount of C in the hot-rolled sheet is 0.041%, and decarburization is slightly occurring. This was first cold-rolled at a reduction rate of 30% to a thickness of 2.1 mm, then annealed at 1100 ° C. for 2 minutes in nitrogen, and then cooled by blowing a jet stream. The cooling rate was about 18 seconds from 1100 ° C. to 850 ° C. and about 27 seconds from 850 ° C. to 400 ° C. The annealed AlN was analyzed to be 0.0055% (NasAlN). Next, this was cold rolled at a rolling rate of 83.3% to a thickness of 0.35 mm, decarburized at 800 ° C. for 3 minutes in hydrogen, and then annealed at 1200 ° C. for 20 hours. The B10 characteristic in the rolling direction of the product was 1.93 T, and W17 / 50 was 1.15 W / kg.
[Comparative Example] A bar having the same components as in Example 1 was allowed to stand for about 40 seconds in front of the finishing hot rolling machine inlet, and then finishing hot rolling was started. The finishing rolling start temperature of the bar at that time was 1150 ° C. at the bar head and 1120 ° C. at the bottom. Thereafter, the treatment was carried out in the same manner as in Example 1, and the secondary recrystallization rate occurrence rate of the most repaired product was examined.

［実施例２］
質量％で、０．０４８％Ｃ，３．１３％Ｓｉ，０．１０％Ｍｎ，０．０２９％Ａｌ，０．０２９％Ｓ、含有し残部Ｆｅ及び不可避的不純物からなる（残部規定は以下の実施例も同じにつき記述省略）珪素鋼溶鋼を該ＣＣ機で５０mm厚のバーとし、直ちに仕上熱延して２．８mm厚とした。仕上熱延入口温度はバー頭部が１２１０℃、尻部が１２００℃であり、それぞれ１０秒後、５０秒後に熱延を終了し、その際の温度は１０１０℃、１０００℃であった。約７５秒後には巻取を完了した。熱延後のＣは０．０４０％，ＡｌＮは０．００４０％（ＮａｓＡｌＮ）と分析された。この熱延板を酸洗後８７．５％の圧延率で冷延して０．３５mm厚の最終ゲージとし、８５０℃で３分間湿水素中で脱炭した後水素中１２００℃で１５時間焼鈍した。製品の圧延方向におけるＢ10特性は夫々１．９２Ｔ，Ｗ17/50 は１．０５Ｗ／kgであった。 [Example 2]
Containing 0.048% C, 3.13% Si, 0.10% Mn, 0.029% Al, 0.029% S, and the balance Fe and unavoidable impurities (the balance is defined as follows) The description of the examples is also omitted. The silicon steel molten steel was made into a bar having a thickness of 50 mm by the CC machine, and immediately finished and hot rolled to a thickness of 2.8 mm. The finishing hot rolling inlet temperature was 1210 ° C. at the bar head and 1200 ° C. at the bottom, and after 10 seconds and 50 seconds, the hot rolling was finished, and the temperatures at that time were 1010 ° C. and 1000 ° C. The winding was completed after about 75 seconds. C after hot rolling was analyzed to be 0.040%, and AlN was analyzed to be 0.0040% (NasAlN). This hot-rolled sheet is pickled and cold-rolled at a rolling rate of 87.5% to obtain a final gauge of 0.35 mm thickness, decarburized in wet hydrogen at 850 ° C. for 3 minutes, and then annealed in hydrogen at 1200 ° C. for 15 hours. did. The B10 characteristics in the rolling direction of the product were 1.92 T and W17 / 50 was 1.05 W / kg, respectively.

［実施例３］
質量％で、０．０５０％Ｃ，３．１８％Ｓｉ，０．０７５％Ｍｎ，０．０２１％Ａｌ，０．０３５％Ｓを含有する珪素鋼溶鋼を該ＣＣ機で４０mm厚のバーとし、直ちに仕上熱延して３．０mm厚とした。仕上熱延入口温度はバー頭部が１２１０℃、尻部が１２０５℃であり、それぞれ１２秒後、５３秒後に熱延を終了した。その際の温度は夫々１０２０℃、９９０℃であった。約８０秒後には巻取を完了した。
これを１１００℃で１分間窒素雰囲気中で連続焼鈍した後、炉の出口にある窒素ガス吹きつけ装置によって強制冷却して９３０℃とし、更にラミナーフロー装置によって２００℃まで急速冷却した。この時のＣは０．０４５％，ＡｌＮは０．００４０％（ＮａｓＡｌＮ）と分析された。これを酸洗後８８．３％圧延率で冷延して０．３５mm厚の最終ゲージとし、８５０℃で３分間湿水素中で脱炭した後水素中１２００℃で１５時間焼鈍した。製品の圧延方向における磁気特性はＢ10が1.９２Ｔ，Ｗ17/50は１．０５Ｗ／kgであった。
［比較例］実施例３と同じ成分のバーを仕上熱延機入口の前でほぼ１５０秒間放置した後、仕上げ熱延を開始した。その際のバーの仕上圧延開始温度はバー頭部が９５０℃、尻部が９３０℃であった。その後、上記実施例３と同様一条件で最終製品まで処理した結果、２次再結晶率発生率を調べたところ、２０％であり、成品には成らなかった。 [Example 3]
A silicon steel molten steel containing 0.050% C, 3.18% Si, 0.075% Mn, 0.021% Al, 0.035% S in mass% is made into a 40 mm thick bar with the CC machine, Immediately, it was hot rolled to a thickness of 3.0 mm. The finishing hot rolling inlet temperature was 1210 ° C. at the bar head and 1205 ° C. at the bottom, and the hot rolling was finished after 12 seconds and 53 seconds, respectively. The temperatures at that time were 1020 ° C. and 990 ° C., respectively. The winding was completed after about 80 seconds.
This was continuously annealed at 1100 ° C. for 1 minute in a nitrogen atmosphere, then forcedly cooled to 930 ° C. by a nitrogen gas blowing device at the outlet of the furnace, and further rapidly cooled to 200 ° C. by a laminar flow device. At this time, C was analyzed as 0.045%, and AlN was analyzed as 0.0040% (NasAlN). This was pickled and cold rolled at a rolling rate of 88.3% to obtain a final gauge having a thickness of 0.35 mm, decarburized in wet hydrogen at 850 ° C. for 3 minutes, and then annealed in hydrogen at 1200 ° C. for 15 hours. The magnetic properties in the rolling direction of the product were 1.92 T for B10 and 1.05 W / kg for W17 / 50.
[Comparative Example] A bar having the same components as in Example 3 was allowed to stand for about 150 seconds in front of the finishing hot rolling machine inlet, and then finishing hot rolling was started. The finishing rolling start temperature of the bar at that time was 950 ° C. at the bar head and 930 ° C. at the bottom. Thereafter, the final product was processed under the same conditions as in Example 3 and as a result, the secondary recrystallization rate occurrence rate was examined. As a result, it was 20%, and it was not a product.

［実施例４］
質量％で、０．０５０％Ｃ，３．１２％Ｓｉ，０．０４１％Ａｌ，０．０３０％Ｓ，０．０５０％Ｓｅ，０．０３０％Ｔｅを含む珪素鋼溶鋼を該ＣＣ機で６０mm厚のバーとし、直ちに仕上熱延して３．０mm厚とした。仕上熱延入口温度はバー頭部が１２３０℃、尻部が１２１０℃であり、それぞれ１５秒後、６０秒後に熱延を終了した。その際の温度は夫々１０５０℃、１０２０℃であった。約９０秒後には巻取を完了した。
これを１１００℃で２分間窒素雰囲気中で連続焼鈍した後、５０％冷延し、次いで１分間１次再結晶のための焼鈍をし、更に８４．７％の圧延率で０．２３mmとした。これを脱炭焼鈍後、脱Ｓｅ、脱Ｔｅ、脱Ｓを伴う１２００℃で２０時間の仕上焼鈍をした。製品の磁気特性は、Ｂ10が１．９３Ｔ、Ｗ17/50は１．０５Ｗ／kgであった。 [Example 4]
Silicon steel molten steel containing 0.050% C, 3.12% Si, 0.041% Al, 0.030% S, 0.050% Se, 0.030% Te in mass% is 60 mm with the CC machine. A thick bar was formed and immediately finished and hot rolled to a thickness of 3.0 mm. The finishing hot rolling inlet temperature was 1230 ° C. at the bar head and 1210 ° C. at the bottom, and the hot rolling was finished after 15 seconds and 60 seconds, respectively. The temperatures at that time were 1050 ° C. and 1020 ° C., respectively. The winding was completed after about 90 seconds.
This was continuously annealed at 1100 ° C. for 2 minutes in a nitrogen atmosphere, then cold-rolled by 50%, then annealed for 1 minute for primary recrystallization, and further reduced to 0.23 mm at a rolling rate of 84.7%. . After decarburization annealing, this was subjected to finish annealing at 1200 ° C. for 20 hours with removal of Se, removal of Te, and removal of S. The magnetic properties of the product were 1.93 T for B10 and 1.05 W / kg for W17 / 50.

［実施例５］
質量％で、０．０４６％Ｃ，３．２０％Ｓｉ，０．０３１％Ａｌ，０．０２５％Ｓを含有する珪素鋼溶鋼を該ＣＣ機で５０mm厚のバーとし、直ちに仕上熱延して２．５mm厚とした。仕上熱延入り口温度はバー頭部が１２２０℃、尻部が１２０５℃であり、それぞれ１２秒後、５０秒後に熱延を終了した。その際の温度は夫々１００５℃、９９０℃であった。約８５秒後には巻取を完了した。
これを１１３０℃で２分間連続焼鈍した後、酸洗いし最終板厚０．２３mmに冷延した後８５０℃で２分間湿水素中で脱炭焼鈍した。この鋼板に重量でＭｇＯ：１００に対してＴｉＯ2 ：１０，ＭｎＯ2 ：５の割合で配合し、更に硼酸０．１〜３％添加の焼鈍分離剤と、硼酸添加しない焼鈍分離剤とを区別して塗布した後１２００℃で２０時間水素中で焼鈍した。
下表に示す通り、このＭｇＯへの硼酸添加によってＢ10特性が向上すると同時に鉄損値が低下し、また夫々のバラツキも少なくなり、方向性珪素鋼板として非常に重要なグラスフィルムの性状が良好となった。
硼酸添 磁束密度，B10(T) 鉄損値，W17/50（W/kg） 備考，
加量,% 最低 最大 平均値 差 最低 最大 平均値 差 TiO2，MnO2添加
0 1.88 1.92 1.905 0.04 1.15 1.32 1.235 0.17 なし
0.1 1.89 1.94 1.915 0.05 0.99 1.12 1.055 0.13
0.5 1.90 1.93 1.915 0.03 0.96 1.08 1.020 0.12 あり
1.0 1.91 1.93 1.920 0.02 0.94 0.98 0.960 0.04
3.0 1.88 1.91 1.895 0.03 1.02 1.17 1.095 0.15 [Example 5]
A silicon steel molten steel containing 0.046% C, 3.20% Si, 0.031% Al, 0.025% S in mass% is made into a 50 mm-thick bar with the CC machine, and immediately finished hot rolled. The thickness was 2.5 mm. The finish hot rolling entrance temperature was 1220 ° C. at the bar head and 1205 ° C. at the bottom, and the hot rolling was finished after 12 seconds and 50 seconds, respectively. The temperatures at that time were 1005 ° C. and 990 ° C., respectively. The winding was completed after about 85 seconds.
This was continuously annealed at 1130 ° C. for 2 minutes, then pickled, cold-rolled to a final thickness of 0.23 mm, and then decarburized and annealed in wet hydrogen at 850 ° C. for 2 minutes. The steel sheet is mixed with TiO 2 : 10 and MnO 2 : 5 by weight with respect to MgO: 100, and further, an annealing separator containing 0.1 to 3% boric acid and an annealing separator not containing boric acid are separated. After separately coating, it was annealed in hydrogen at 1200 ° C. for 20 hours.
As shown in the table below, the addition of boric acid to MgO improves the B10 characteristics and at the same time reduces the iron loss value, and also reduces each variation, and the glass film, which is very important as a grain-oriented silicon steel sheet, has good properties. became.
Boric acid-added magnetic flux density, B10 (T) Iron loss value, W17 / 50 (W / kg) Remarks,
Addition,% Minimum Maximum Average Difference Minimum Maximum Average Difference TiO 2 , MnO 2 added
0 1.88 1.92 1.905 0.04 1.15 1.32 1.235 0.17 None
0.1 1.89 1.94 1.915 0.05 0.99 1.12 1.055 0.13
0.5 1.90 1.93 1.915 0.03 0.96 1.08 1.020 0.12 Yes
1.0 1.91 1.93 1.920 0.02 0.94 0.98 0.960 0.04
3.0 1.88 1.91 1.895 0.03 1.02 1.17 1.095 0.15

［実施例６］
質量％で、０．０４％Ｃ，３．３０％Ｓｉ，０．０２９％Ａｌを含む珪素鋼溶鋼を該ＣＣ機で６０mm厚のバーとし、直ちに仕上熱延して２．３mm厚とした。仕上熱延入口温度はバー頭部が１２３０℃、尻部が１２０５℃であり、それぞれ１２秒後、４５秒後に熱延を終了した。その際の温度は夫々１０１０℃、９９５℃であった。約８５秒後には巻取を完了した。
この熱延板を１１５０℃で２分間連続焼鈍した後、急速冷却した後酸洗いし、最終板厚０．２７mmに冷延した後８５０℃で水素中で脱炭焼鈍を行い１２００℃で最終焼鈍した。冷延を行うに当たっては５通りの異なる温度での時効処理を行いながら、同一のパススケジュール（１．６mm，１．２mm，１．０mm，０．８mm，０．６mm，０．４５mmの６パス）で通板した。即ち、その条件と磁気特性との関係は下表に示す通りである。
これから２００℃前後でのパス間時効が効果的であることが分かる。
(1).冷延パス毎に 50 ℃×5 分熱処理 ・・Ｂ10=1.920（T)，Ｗ17/50=1.024 （Ｗ/kg)
(2).冷延パス毎に150 ℃×5 分熱処理 ・・Ｂ10=1.944（T)，Ｗ17/50=1.001 （W/kg）
(3).冷延パス毎に200 ℃×5 分熱処理 ・・Ｂ10=1.951（T)，Ｗ17/50=0.998 （W/kg）
(4).冷延パス毎に350 ℃×5 分熱処理 ・・Ｂ10=1.925（T)，Ｗ17/50=1.012 （W/kg）
(5).冷延パス毎に500 ℃×5 分熱処理 ・・Ｂ10=1.880（T)，Ｗ17/50=1.195 （W/kg） [Example 6]
A silicon steel molten steel containing 0.04% C, 3.30% Si and 0.029% Al in mass% was made into a bar having a thickness of 60 mm by the CC machine, and immediately finished by hot rolling to a thickness of 2.3 mm. The finishing hot rolling inlet temperature was 1230 ° C. at the bar head and 1205 ° C. at the bottom, and the hot rolling was finished after 12 seconds and 45 seconds, respectively. The temperatures at that time were 1010 ° C. and 995 ° C., respectively. The winding was completed after about 85 seconds.
This hot-rolled sheet was continuously annealed at 1150 ° C. for 2 minutes, then rapidly cooled and pickled, cold-rolled to a final sheet thickness of 0.27 mm, decarburized and annealed in hydrogen at 850 ° C., and finally annealed at 1200 ° C. did. When performing cold rolling, the same pass schedule (6 passes of 1.6mm, 1.2mm, 1.0mm, 0.8mm, 0.6mm, 0.45mm), with aging treatment at 5 different temperatures ). That is, the relationship between the conditions and the magnetic characteristics is as shown in the table below.
This shows that aging between passes at around 200 ° C. is effective.
(1). Heat treatment at 50 ℃ for 5 minutes for each cold rolling pass ・ ・ B10 = 1.920 (T), W17 / 50 = 1.024 (W / kg)
(2). Heat treatment at 150 ℃ for 5 minutes for each cold rolling pass ・ ・ B10 = 1.944 (T), W17 / 50 = 1.001 (W / kg)
(3). Heat treatment at 200 ℃ for 5 minutes for each cold rolling pass ・ ・ B10 = 1.951 (T), W17 / 50 = 0.998 (W / kg)
(4). Heat treatment at 350 ℃ for 5 minutes for each cold rolling pass ・ ・ B10 = 1.925 (T), W17 / 50 = 1.012 (W / kg)
(5). Heat treatment at 500 ℃ for 5 minutes for each cold rolling pass ・ ・ B10 = 1.880 (T), W17 / 50 = 1.195 (W / kg)

［実施例７］
質量％で、０．０８５％Ｃ，３．２０％Ｓｉ，０．０７３％Ｍｎ，０．０２５％Ｓ，０．０２５％酸可溶性Ａｌ，０．００８５％Ｎ，０．０８％Ｓｎ，０．０７％Ｃｕを含有する珪素鋼溶鋼を該ＣＣ機で６０mm厚のバーとし、直ちに仕上熱延して２．０mmとした。仕上熱延入り口温度はバー頭部が１２２０℃、尻部が１２０１℃であり、それぞれ１５秒後、５５秒後に熱延を終了した。その際の温度は夫々９９０℃、９８５℃であった。約９０秒後には巻取を完了した。
この熱延板を１１３０℃で２分間連続焼鈍した後、１００℃の湯の中に急速冷却して析出熱処理を行い、酸洗いし、次いで２５０℃×５分間のパス間時効処理を施しながら最終板厚０．２２mmに冷延した。次いで８５０℃で２分間Craced−ＮＨ3 中，露点６２℃の雰囲気中で脱炭焼鈍を行い、更にＭｇＯとＴｉＯ2 を混合した焼鈍分離剤を塗布し１２００℃で最終焼鈍した。最終焼鈍後に張力コーティングを施した。
製品の磁気特性と結晶粒度は、Ｂ10＝１．９２（Ｔ），Ｗ17/50＝０．８８Ｗ/kg，ＡＳＴＭ Ｎｏ．５であった。Ｓｎ及びＣｕを添加しない場合には、Ｂ10＝１．９２ （Ｔ），Ｗ17/50 ＝０．９５Ｗ/kg ，ＡＳＴＭ Ｎｏ．３であった。 [Example 7]
In mass%, 0.085% C, 3.20% Si, 0.073% Mn, 0.025% S, 0.025% acid-soluble Al, 0.0085% N, 0.08% Sn, 0.005%. Silicon steel molten steel containing 07% Cu was made into a 60 mm thick bar by the CC machine, and immediately finished hot rolled to 2.0 mm. The finishing hot rolling entrance temperature was 1220 ° C. at the bar head and 1201 ° C. at the bottom, and the hot rolling was finished after 15 seconds and 55 seconds, respectively. The temperatures at that time were 990 ° C. and 985 ° C., respectively. The winding was completed after about 90 seconds.
This hot-rolled sheet was continuously annealed at 1130 ° C. for 2 minutes, then rapidly cooled in hot water at 100 ° C., subjected to precipitation heat treatment, pickled, and then subjected to final aging treatment at 250 ° C. for 5 minutes. The sheet was cold-rolled to a thickness of 0.22 mm. Next, decarburization annealing was performed in an atmosphere of dew point of 62 ° C. in Craced-NH 3 for 2 minutes at 850 ° C., and an annealing separator mixed with MgO and TiO 2 was applied and final annealing was performed at 1200 ° C. A tension coating was applied after the final annealing.
The magnetic properties and grain size of the product are B10 = 1.92 (T), W17 / 50 = 0.88 W / kg, ASTM No. It was 5. When Sn and Cu are not added, B10 = 1.92 (T), W17 / 50 = 0.95 W / kg, ASTM No. 3.

［実施例８］ 質量％で、０．０５％Ｃ，３．０５％Ｓｉ，０．０７％Ｍｎ，０．０３％Ｓ，０．０２６％酸可溶性Ａｌ，を含有する珪素鋼溶鋼を該ＣＣ機で４０mm厚のバーとして鋳造した。鋳造後単体のバーに切断しその際のバー温度は１２５５℃であった。これを１２５０℃以下に降温しないように加熱装置による温度保持を続けながら約３００で秒仕上熱延機の入口に到達せしめ、直ちに熱延を開始し３０mm厚さとした。仕上熱延入口温度は１２２０〜１２３０℃であり、熱延板の先端及び後端は夫々１５秒、６０秒後に熱延を完了した。その際の温度は夫々１０３０℃，１０２０℃であり、約７０秒後には巻取を完了した。
この熱延板を１１３０℃で３分間連続焼鈍した後、炉の出口にある沸騰水の入った槽を潜らせる強制冷却下後酸洗し、９０％の圧下率で冷延して０．３mm厚さとした。これを脱炭焼鈍した後１２００℃で約２０時間Ｈ2中で最終焼鈍した。
製品の圧延方向における磁気特性は、Ｂ10＝１．９３（Ｔ），Ｗ17/50＝１．０１Ｗ/kg であった。
［比較例］上記実施例８と同じ成分のバーを鋳造後、加熱装置による温度保持をすることなく仕上熱延機入口へ搬送したものは、温度が１１００℃に低下しており、これを直ちに仕上げ熱延した熱延板を上記実施例３と同様一条件で最終製品まで処理し、２次再結晶粒率発生率を調べたところ、コイル全体で３０％以下であり、成品にはなりえなかった。 [Example 8] A silicon steel molten steel containing 0.05% C, 3.05% Si, 0.07% Mn, 0.03% S, and 0.026% acid-soluble Al in mass% is obtained as the CC. Machined as a 40mm thick bar. After casting, it was cut into a single bar and the bar temperature at that time was 1255 ° C. While maintaining the temperature by the heating device so as not to lower the temperature to 1250 ° C. or less, the temperature reached the inlet of the finishing hot rolling machine at about 300 seconds, and immediately started hot rolling to a thickness of 30 mm. The finish hot rolling inlet temperature was 1220-1230 ° C., and the hot rolling was completed after 15 seconds and 60 seconds at the front and rear ends of the hot rolled sheet, respectively. The temperatures at that time were 1030 ° C. and 1020 ° C., respectively, and the winding was completed after about 70 seconds.
This hot-rolled sheet was continuously annealed at 1130 ° C. for 3 minutes, then forced-cooled to immerse the bath containing boiling water at the outlet of the furnace, pickled, cold-rolled at a rolling reduction of 90%, and 0.3 mm Thickness. This was decarburized and annealed at 1200 ° C. for about 20 hours in H 2 .
The magnetic properties of the product in the rolling direction were B10 = 1.93 (T) and W17 / 50 = 1.01 W / kg.
[Comparative example] After the bar having the same composition as in Example 8 was cast and conveyed to the finishing hot rolling machine inlet without holding the temperature by the heating device, the temperature dropped to 1100 ° C. The finished hot-rolled sheet was processed to the final product under the same conditions as in Example 3 and the secondary recrystallized grain ratio occurrence rate was examined. The coil was 30% or less, and it could be a finished product. There wasn't.

［実施例９］ 質量％で、０．０５５％Ｃ，３．２０％Ｓｉ，０．０２５％Ｓ，０．３０％酸可溶性Ａｌ，を含有する珪素鋼溶鋼を該ＣＣ機で３０mm厚のバーとして鋳造した。鋳造後単体のバーに切断しその際のバー温度は１１５０℃であった。このバーを直ちに１３３０℃に加熱した加熱炉に挿入してサイドＡｌＮを固溶させた後、炉から抽出し、約１２０秒仕上熱延機の入口に到達せしめ、直ちに熱延を開始し２５mm厚さとした。仕上熱延入口温度は１２１０〜１２２０℃であり、熱延板の先端及び後端は夫々１６秒、５０秒後に熱延を完了した。その際の温度は夫々１０１０℃，９９８℃であり、約７０秒後には巻取を完了した。
この熱延板を１１３０℃で２分間連続焼鈍した後、炉の出口にある霧吹き装置で強制冷却し、酸洗し、冷延して０．３mm厚にした後。８３５℃で３分間湿水素中で脱炭焼鈍した。この鋼板にＢを８００ppm 含むＭｇＯをスラリーとして塗布し、コイルに巻いて１２００℃で２０時間水素中で焼鈍した。
製品の圧延方向における磁気特性は、Ｂ10＝１．９２（Ｔ），Ｗ17/50＝０．８９Ｗ/kg であった。
［比較例］上記実施例８と同じ成分のバーを鋳造後、直ちに仕上熱延機入口に搬送したものは、温度はさらに降下して１０８０℃まで低下していた。これを直ちに仕上げ熱延した熱延板を上記実施例３と同一条件で最終製品まで処理し、２次再結晶率発生率を調べたところ、僅か２０％しか発生せず、成品にはなりえなかった。 [Example 9] A silicon steel molten steel containing 0.055% C, 3.20% Si, 0.025% S, and 0.30% acid-soluble Al in mass% is bar-shaped 30 mm thick with the CC machine. As cast. After casting, it was cut into a single bar and the bar temperature at that time was 1150 ° C. This bar was immediately inserted into a heating furnace heated to 1330 ° C. to dissolve the side AlN, and then extracted from the furnace, reached the inlet of the finishing hot rolling machine for about 120 seconds, immediately started hot rolling, and had a thickness of 25 mm. Say it. The finish hot rolling inlet temperature was 1210 to 1220 ° C., and the hot rolling was completed after 16 seconds and 50 seconds at the front end and the rear end of the hot rolled plate, respectively. The temperatures at that time were 1010 ° C. and 998 ° C., respectively, and the winding was completed after about 70 seconds.
After this hot-rolled sheet was continuously annealed at 1130 ° C. for 2 minutes, it was forcibly cooled with a sprayer at the outlet of the furnace, pickled, and cold-rolled to a thickness of 0.3 mm. Decarburization annealing was performed in wet hydrogen at 835 ° C. for 3 minutes. This steel sheet was coated with MgO containing 800 ppm of B as a slurry, wound around a coil, and annealed in hydrogen at 1200 ° C. for 20 hours.
The magnetic properties of the product in the rolling direction were B10 = 1.92 (T), W17 / 50 = 0.89 W / kg.
[Comparative Example] After the bar having the same composition as in Example 8 was cast and immediately conveyed to the finishing hot rolling machine inlet, the temperature further decreased to 1080 ° C. The hot-rolled sheet that was immediately finished and hot-rolled was processed to the final product under the same conditions as in Example 3, and the secondary recrystallization rate occurrence rate was examined. As a result, only 20% was generated and it could be a finished product. There wasn't.

連続鋳造−熱間圧延連続設備の一例を示す模式図。The schematic diagram which shows an example of continuous casting-hot rolling continuous equipment. 連続鋳造−熱間圧延連続設備の他の例を示す模式図。The schematic diagram which shows the other example of continuous casting-hot rolling continuous equipment. ＡｌＮ固溶処理後の保持温度及び時間が磁気特性に及ぼす影響（３．２０％Ｓｉ）を示す図。The figure which shows the influence (3.20% Si) which the holding temperature and time after an AlN solid solution process have on magnetic characteristics. ＡｌＮ固溶処理後の熱間圧延における典型的な熱履歴曲線（３．１０％Ｓｉ）を示す図。The figure which shows the typical thermal history curve (3.10% Si) in the hot rolling after an AlN solid solution process. ＡｌＮ固溶処理後の熱間圧延における急冷（タンデム圧延）開始温度と磁気特性との関係（３．１０％Ｓｉ）を示す図。The figure which shows the relationship (3.10% Si) of the rapid cooling (tandem rolling) start temperature and magnetic characteristic in the hot rolling after an AlN solid solution process. ＡｌＮ固溶処理後の冷却曲線とＡｌＮの析出に及ぼすＳｉ量の影響を示す図。The figure which shows the influence of the amount of Si on the cooling curve after AlN solid solution processing, and precipitation of AlN.

Claims (4)

質量で
Ｃ ：０．０１０〜０．０７５％，
Ｓｉ：２．９５〜４．０％，
酸可溶性Ａｌ：０．０１０〜０．０４０％，
Ｎ：０．００１０〜０．０１５０％
Ｓ或いはＳｅを単独または双方で０．００５〜０．１％
を含み、残部Ｆｅおよび不可避的不純物からなる溶鋼を連続的に鋳造して厚さ２０〜７０mmの中肉厚バーを製造し、該バーを鋳造後或いは加熱炉より抽出後（加熱炉の在炉時間を含めて）１２００℃超の温度間に、かつ５００秒以内に熱間仕上圧延機の入口に到達せしめて熱間連続圧延を開始し、該熱延で１．５mm〜５mm厚の熱延板とし、熱延終了後６００℃に達するまでの冷却時間を１５０秒以下とすることを特徴とし、以下通常の冷延、中間焼鈍、脱炭焼鈍、仕上焼鈍等を行う高磁束密度方向性珪素鋼板の製造方法。 By mass C: 0.010 to 0.075%,
Si: 2.95 to 4.0%,
Acid-soluble Al: 0.010 to 0.040%,
N: 0.0010 to 0.0150%
0.005 to 0.1% of S or Se alone or both
A molten steel consisting of the remaining Fe and unavoidable impurities is continuously cast to produce a medium-thickness bar having a thickness of 20 to 70 mm. After the bar is cast or extracted from a heating furnace (in-furnace of the heating furnace) (Including the time) The hot finish rolling is started by reaching the inlet of the hot finishing mill within a temperature of over 1200 ° C. and within 500 seconds, and the hot rolling with a thickness of 1.5 mm to 5 mm is performed. A high magnetic flux density directional silicon which is made into a plate and has a cooling time of 150 seconds or less after completion of hot rolling until it reaches 600 ° C., and which performs normal cold rolling, intermediate annealing, decarburization annealing, finish annealing, etc. A method of manufacturing a steel sheet. 上記溶鋼中に、さらに粒界に偏析して結晶成長を抑制する，Ｓｂ：０．００５〜０．２％，Ｎｂ：０．００５〜０．２％、Ｍｏ：０．００３〜０．１、Ｃｕ：０．０２〜０．２％、Ｓｎ：０．０２〜０．３％の群から選ばれた少なくとも１種を含有することを特徴とする請求項１に記載の高磁束密度方向性珪素鋼板の製造方法。 In the molten steel, further segregation at grain boundaries to suppress crystal growth, Sb: 0.005 to 0.2%, Nb: 0.005 to 0.2%, Mo: 0.003 to 0.1, The high magnetic flux density directional silicon according to claim 1, comprising at least one selected from the group consisting of Cu: 0.02 to 0.2% and Sn: 0.02 to 0.3%. A method of manufacturing a steel sheet. 前記中肉厚バーが１２５０℃以上の温度を保持している場合には最長でも５００秒以内に、１２００℃以上の温度を保持している場合には１５０秒以内に熱間仕上圧延機の入口に到達せしめることを特徴とする請求項１に記載の高磁束密度方向性珪素鋼板の製造方法。 When the intermediate thickness bar holds a temperature of 1250 ° C. or higher, the hot finish rolling mill entrance is within 500 seconds at the longest, and when it maintains a temperature of 1200 ° C. or higher, within 150 seconds. The method for producing a high magnetic flux density directional silicon steel sheet according to claim 1, wherein: 連続鋳造で製造した中肉厚バーを熱間仕上圧延機の入口に到達せしめて熱間連続圧延を開始するまでの所用時間が２００秒を超える場合、或いは該バーの温度が１０００℃のように低温である場合には、これらのバーを１３００〜１３５０℃の温度に保持するための加熱炉を通すことを特徴とする請求項１に記載の高磁束密度方向性珪素鋼板の製造方法。 When it takes more than 200 seconds to reach the entrance of the hot finishing mill after the medium thickness bar manufactured by continuous casting exceeds 200 seconds, or the temperature of the bar is 1000 ° C. 2. The method for producing a high magnetic flux density grain-oriented silicon steel sheet according to claim 1, wherein when the temperature is low, the bar is passed through a heating furnace for maintaining the bar at a temperature of 1300 to 1350 ° C. 3.
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