JP2011208188A - Method for manufacturing grain-oriented electromagnetic steel sheet - Google Patents
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本発明は、主として変圧器や発電機、回転機の鉄心等に用いられる方向性電磁鋼板の製造方法に関し、詳しくは、連続焼鈍を用いた仕上焼鈍で二次再結晶させる方向性電磁鋼板の製造方法に関するものである。 The present invention relates to a method for producing a grain-oriented electrical steel sheet mainly used for transformers, generators, iron cores of rotating machines, and the like, and more specifically, the production of grain-oriented electrical steel sheet that is secondarily recrystallized by finish annealing using continuous annealing. It is about the method.
方向性電磁鋼板は、結晶方位が（１１０）＜００１＞方位（以下、「Ｇｏｓｓ方位」とも称する）に強く集積し、磁化容易軸が圧延方向に強く配向しているため、圧延方向へ励磁する際のエネルギーロスが非常に小さいという優れた特長がある。しかし、上記方向性電磁鋼板を製造するには、Ｇｏｓｓ方位を持つ結晶粒を優先的に成長させる必要があるため、極めて高温長時間の仕上焼鈍が必要である。具体的には、仕上焼鈍には、コイルフォームでのバッチ焼鈍法を用いるのが一般的であるが、通常、９００〜１２００℃の温度域で数十時間の加熱が必要とされているため、膨大なエネルギーと時間を要するコストの高い処理となっている。したがって、この仕上焼鈍を、短時間で焼鈍が可能な連続焼鈍に置き換えることができれば、優れた磁気特性を有する方向性電磁鋼板を安価にかつ大量に提供することが可能となる。 In the grain-oriented electrical steel sheet, the crystal orientation is strongly accumulated in the (110) <001> orientation (hereinafter also referred to as “Goss orientation”), and the easy magnetization axis is strongly oriented in the rolling direction, so that it is excited in the rolling direction. There is an excellent feature that the energy loss is very small. However, in order to manufacture the grain-oriented electrical steel sheet, it is necessary to preferentially grow crystal grains having Goss orientation, and therefore, finishing annealing at an extremely high temperature for a long time is required. Specifically, it is common to use a batch annealing method with coil foam for finish annealing, but usually heating in the temperature range of 900 to 1200 ° C. is required for several tens of hours. It is a costly process that requires enormous energy and time. Therefore, if this finish annealing can be replaced with continuous annealing capable of annealing in a short time, it becomes possible to provide a large amount of grain-oriented electrical steel sheets having excellent magnetic properties.
斯かる技術としては、例えば、特許文献１には、インヒビターとしてＭｎ（Ｓｅ，Ｓ）を用い、インヒビターを完全固溶させない温度でスラブ加熱を行い、さらに二次再結晶焼鈍前にスキンパス圧延を行うことで、連続焼鈍法で二次再結晶を発現させる技術が提案されている。また、特許文献２には、インヒビターとしてＡｌＮ＋Ｍｎ（Ｓｅ，Ｓ）を用い、熱延板焼鈍温度と冷間圧延温度を制御することにより、連続焼鈍法で二次再結晶を発現させる技術が提案されている。また、特許文献３には、インヒビター成分を極力排除し、冷延２回法を利用することで、連続焼鈍法で平均粒径が０．１５〜２．０ｍｍの微細Ｇｏｓｓ組織を発現させる技術が提案されている。また、特許文献４には、インヒビターとして金属間化合物を利用し、連続焼鈍法で二次再結晶を起こさせることで、通常の方向性電磁鋼板と同等以上の磁気特性を備えた電磁鋼板を製造する方法が提案されている。 As such a technique, for example, in Patent Document 1, Mn (Se, S) is used as an inhibitor, slab heating is performed at a temperature at which the inhibitor is not completely dissolved, and skin pass rolling is performed before secondary recrystallization annealing. Therefore, a technique for expressing secondary recrystallization by a continuous annealing method has been proposed. Patent Document 2 proposes a technique for expressing secondary recrystallization by a continuous annealing method using AlN + Mn (Se, S) as an inhibitor and controlling the hot-rolled sheet annealing temperature and the cold rolling temperature. ing. Patent Document 3 discloses a technique for expressing a fine Goss structure having an average particle diameter of 0.15 to 2.0 mm by a continuous annealing method by eliminating an inhibitor component as much as possible and utilizing a cold rolling twice method. Proposed. Patent Document 4 uses an intermetallic compound as an inhibitor to produce secondary recrystallization by a continuous annealing method, thereby producing an electrical steel sheet having magnetic properties equal to or higher than that of a normal grain oriented electrical steel sheet. A method has been proposed.
ところで、連続焼鈍法を用いて工業的に方向性電磁鋼板の生産するためには、仕上焼鈍での焼鈍温度を約１０２０℃以下とし、かつ均熱時間を長くとも２〜３分程度として、二次再結晶を完了させることが望ましい。というのは、焼鈍温度が１０２０℃を超えると鋼板上に形成されるＳｉ酸化物などがハースロールの表面に付着・堆積し、鋼板に押し疵（デンツ）を発生させるため、ロール交換を頻繁に行う必要があり、生産性や歩留りが大きく低下する。また、均熱時間が２〜３分より長くなると、低速焼鈍せざるを得ず、やはり生産性の低下や焼鈍コストの増大を招くことになるからである。 By the way, in order to produce a grain-oriented electrical steel sheet industrially using the continuous annealing method, the annealing temperature in the finish annealing is set to about 1020 ° C. or less, and the soaking time is set to about 2 to 3 minutes at the longest. It is desirable to complete the next recrystallization. This is because when the annealing temperature exceeds 1020 ° C., Si oxides and the like formed on the steel sheet adhere to and accumulate on the surface of the hearth roll, and the steel sheet generates dents. This has to be done and the productivity and yield are greatly reduced. In addition, if the soaking time is longer than 2 to 3 minutes, low-speed annealing is unavoidable, which also causes a decrease in productivity and an increase in annealing cost.
発明者らは、上記観点から、特許文献１〜４で提案された技術について検討を行った。
その結果、特許文献１の技術は、一次再結晶組織が残留しやすく、連続焼鈍法で二次再結晶させるには、安定性の点で難があることが明らかとなった。これは、比較的ピン止め力の弱いＭｎ（Ｓｅ，Ｓ）をインヒビターとして用いていることと、未固溶のインヒビター成分が多く、分散が不均一であることに原因があると推定された。さらに、スキンパス圧延を利用すると、そのまま二次再結晶させる場合に比べて配向性が大きく低下しやすいという問題がある。また、特許文献２の技術は、二次再結晶を完了させるために、高温もしくは長時間の仕上焼鈍が必要であり、例えば、１０００℃で二次再結晶を完了させるためには６〜１０分間の均熱時間が必要とされているため実用的な技術ではない。
Inventors examined the technique proposed by patent documents 1-4 from the said viewpoint.
As a result, it has been clarified that the technique of Patent Document 1 has a difficulty in terms of stability in that the primary recrystallization structure tends to remain and secondary recrystallization by the continuous annealing method is difficult. This was presumed to be caused by the fact that Mn (Se, S), which has a relatively weak pinning force, was used as an inhibitor and that there were many undissolved inhibitor components and the dispersion was uneven. Furthermore, when skin pass rolling is used, there is a problem that the orientation tends to be greatly reduced as compared with the case where secondary recrystallization is performed as it is. Further, the technique of Patent Document 2 requires high-temperature or long-time finish annealing in order to complete secondary recrystallization. For example, in order to complete secondary recrystallization at 1000 ° C., it takes 6 to 10 minutes. This is not a practical technique because it requires soaking time.
また、特許文献３の技術は、Ｇｏｓｓ方位粒発達の安定性・再現性に難がある。というのは、この技術は、鋼中のインヒビター成分を極力低減して粒成長を促進させた上で、集合組織によるインヒビション効果でＧｏｓｓ方位粒を選択成長させることに特徴がある。しかし、インヒビター成分を排除しているため、Ｇｏｓｓ方位の選択性が集合組織変動の影響を受けやすくなり、その結果、安定してＧｏｓｓ方位を発達させることが難しくなるためと考えられる。つまり、Ｇｏｓｓ組織を安定して成長させるためには、ある程度のインヒビターの存在が必要であると考えられる。また、特許文献４の技術は、高価な合金元素を多量に添加する必要があるため、原料コストが高くなるという問題がある。
以上説明したように、上記従来技術はいずれも、製造コストや生産性、二次再結晶の安定性の点で工業的に実用可能な技術とは言い難いものでしかなかった。
Moreover, the technique of patent document 3 has difficulty in stability and reproducibility of Goss orientation grain development. This is because this technique is characterized in that the inhibitor component in steel is reduced as much as possible to promote grain growth, and the Goss oriented grains are selectively grown by the inhibition effect by the texture. However, since the inhibitor component is excluded, the selectivity of the Goss orientation is likely to be affected by the texture variation, and as a result, it is considered difficult to develop the Goss orientation stably. That is, it is considered that the presence of a certain amount of inhibitor is necessary in order to stably grow the Goss tissue. Moreover, since the technique of patent document 4 needs to add an expensive alloy element in large quantities, there exists a problem that raw material cost becomes high.
As described above, any of the above prior arts is hardly a technically practical technique in terms of manufacturing cost, productivity, and stability of secondary recrystallization.
そこで、本発明の目的は、連続焼鈍法を用いた比較的低温・短時間の仕上焼鈍で、安定的に二次再結晶を起こさせることができる方向性電磁鋼板の有利な製造方法を提案することにある。 Therefore, an object of the present invention is to propose an advantageous method for producing a grain-oriented electrical steel sheet that can cause secondary recrystallization stably by finish annealing at a relatively low temperature and in a short time using a continuous annealing method. There is.
発明者らは、上記課題の解決に向けて鋭意検討を重ねた。その結果、適正な微量インヒビターを含有する熱延鋼板を、熱延板焼鈍を施すことなくあるいは低温で熱延板焼鈍を施した後、低温中間焼鈍を挟む２回以上でかつ最終冷延圧下率を適正範囲に制御した冷間圧延により最終板厚の冷延板とし、その後、低温・短時間の仕上焼鈍を施すことにより、二次再結晶を安定して起こさせることができ、ひいては、Ｇｏｓｓ方位に高度に集積した方向性電磁鋼板を安価かつ大量に製造し得ることを見出し、本発明を完成させた。 The inventors have intensively studied to solve the above problems. As a result, the hot-rolled steel sheet containing an appropriate trace amount of inhibitor is subjected to hot-rolled sheet annealing without performing hot-rolled sheet annealing or at a low temperature, and then the final cold-rolling reduction ratio at least twice with the low-temperature intermediate annealing interposed therebetween. The secondary recrystallization can be caused stably by forming a cold-rolled sheet having a final thickness by cold rolling controlled to an appropriate range, followed by a low-temperature, short-time finish annealing. The inventors have found that grain oriented electrical steel sheets that are highly integrated in the orientation can be manufactured in a large amount at low cost, and have completed the present invention.
すなわち、本発明は、Ｃ：０．１２ｍａｓｓ％以下、Ｓｉ：２．０〜４．５ｍａｓｓ％、Ｍｎ：０．００５〜０．３ｍａｓｓ％、Ａｌ：０．００５〜０．０１２ｍａｓｓ％、Ｎ：０．００３０〜０．０１０ｍａｓｓ％、残部がＦｅおよび不可避的不純物からなる成分組成を有する鋼スラブを熱間圧延し、中間焼鈍を挟む２回以上の冷間圧延で最終板厚の冷延板とし、その後、仕上焼鈍として１回以上の連続焼鈍を施す方向性電磁鋼板の製造方法において、上記中間焼鈍を７５０〜９５０℃の温度とし、最終冷間圧延を３０〜８０％の圧下率として行った後、連続焼鈍で二次再結晶させることを特徴とする方向性電磁鋼板の製造方法である。 That is, the present invention is C: 0.12 mass% or less, Si: 2.0-4.5 mass%, Mn: 0.005-0.3 mass%, Al: 0.005-0.012 mass%, N: 0 .0030-0.010 mass%, hot-rolling a steel slab having a composition composed of Fe and inevitable impurities in the balance, and forming a cold-rolled sheet having a final thickness by two or more cold-rolling sandwiching intermediate annealing, Thereafter, in the method for producing a grain-oriented electrical steel sheet that is subjected to one or more continuous annealings as finish annealing, the intermediate annealing is performed at a temperature of 750 to 950 ° C., and the final cold rolling is performed at a rolling reduction of 30 to 80%. , A method for producing a grain-oriented electrical steel sheet, characterized by performing secondary recrystallization by continuous annealing.
本発明の方向性電磁鋼板の製造方法は、熱間圧延後、９５０℃以下の温度で熱延板焼鈍を施すことを特徴とする。 The method for producing a grain-oriented electrical steel sheet according to the present invention is characterized by performing hot-rolled sheet annealing at a temperature of 950 ° C. or lower after hot rolling.
また、本発明の方向性電磁鋼板の製造方法における上記鋼スラブは、上記成分組成に加えてさらに、Ｓｂ：０．００５〜０．２ｍａｓｓ％、Ｓｎ：０．００５〜０．２ｍａｓｓ％、Ｃｕ：０．０１〜０．２ｍａｓｓ％、Ｓ：０．００１〜０．０２ｍａｓｓ％、Ｓｅ：０．００１〜０．０２ｍａｓｓ％およびＢ：０．０００１〜０．００５ｍａｓｓ％のうちから選ばれる１種または２種以上を含有することを特徴とする。 In addition to the above component composition, the steel slab in the method for producing a grain-oriented electrical steel sheet according to the present invention further includes Sb: 0.005-0.2 mass%, Sn: 0.005-0.2 mass%, Cu: One or two selected from 0.01 to 0.2 mass%, S: 0.001 to 0.02 mass%, Se: 0.001 to 0.02 mass%, and B: 0.0001 to 0.005 mass% It contains more than seeds.
本発明によれば、低温・短時間の連続焼鈍を用いた仕上焼鈍でも、二次再結晶を安定して発現させることができるので、磁気特性に優れる方向性電磁鋼板を、低コストで大量に提供することが可能となる。したがって、本発明は、省エネルギーや温暖化の防止にも貢献することができる。 According to the present invention, secondary recrystallization can be stably expressed even in finish annealing using low-temperature and short-time continuous annealing. Therefore, a large amount of grain-oriented electrical steel sheets with excellent magnetic properties can be obtained at low cost. It becomes possible to provide. Therefore, the present invention can also contribute to energy saving and prevention of global warming.
先ず、本発明を開発する契機となった実験について説明する。
表１に示した成分組成からなるＡ〜Ｄの鋼を実験室的に溶製し、鋼素材とし、１２００℃に加熱後、熱間圧延し、板厚２．７ｍｍの熱延板とし、その後、上記熱延板を２分割し、そのうちの一方については、熱延板焼鈍を施すことなく、また、残りの一方については、乾燥窒素中で１０００℃×６０ｓｅｃの熱延板焼鈍を施した後、冷間圧延して最終板厚０．３５ｍｍの冷延板とした。なお、上記冷間圧延は、１回の冷間圧延で最終板厚まで圧延する条件（中間焼鈍なし）と、１回目の冷間圧延で中間厚０．４〜２．０ｍｍまで圧延し、８００℃×６０ｓｅｃの中間焼鈍を施した後、２回目の冷間圧延（最終冷間圧延）で最終板厚とする条件で行った。その後、上記最終冷延後の冷延板に、１０００℃×２ｍｉｎの連続焼鈍（仕上焼鈍）を施し、製品板とした。
First, an experiment that triggered the development of the present invention will be described.
The steels A to D having the composition shown in Table 1 were melted in a laboratory, made into a steel material, heated to 1200 ° C., hot-rolled to obtain a hot-rolled sheet having a thickness of 2.7 mm, and thereafter The hot-rolled sheet is divided into two parts, one of which is not subjected to hot-rolled sheet annealing, and the other is subjected to hot-rolled sheet annealing at 1000 ° C. × 60 sec in dry nitrogen. Then, it was cold-rolled to obtain a cold-rolled sheet having a final sheet thickness of 0.35 mm. The cold rolling is performed under the condition of rolling to the final sheet thickness by one cold rolling (without intermediate annealing) and by rolling to the intermediate thickness of 0.4 to 2.0 mm by the first cold rolling, 800 After performing the intermediate annealing of ° C. × 60 sec, it was performed under the condition that the final thickness was obtained by the second cold rolling (final cold rolling). Thereafter, the cold-rolled sheet after the final cold-rolling was subjected to continuous annealing (finish annealing) at 1000 ° C. for 2 minutes to obtain a product sheet.
斯くして得られた仕上焼鈍後の鋼板からエプスタイン試験片を採取し、５０００Ａ／ｍで磁化したときの圧延方向の磁束密度Ｂ５０を測定した。次いで、上記焼鈍後の鋼板をマクロエッチングし、鋼板のマクロ組織を肉眼で観察したところ、Ｂ５０が１．９０Ｔを超える鋼板では、平均結晶粒径が２ｍｍ以上の二次再結晶粒で覆われており、二次再結晶が完了していることが確認できた。 An Epstein specimen was collected from the steel sheet after finish annealing thus obtained, and the magnetic flux density B 50 in the rolling direction when magnetized at 5000 A / m was measured. Then, the steel sheet after the annealing macro etching, observation of the macrostructure of the steel sheet with the naked eye, in the steel sheet B 50 is more than 1.90T, the average crystal grain size is covered with more secondary recrystallized grains 2mm The secondary recrystallization was confirmed to be complete.
図１に、上記各試験片のＢ５０と最終冷延圧下率との関係を示した。図１から、インヒビター成分であるＡｌを０．００５ｍａｓｓ％以上、Ｎを０．００３ｍａｓｓ％以上含有する熱延板を、熱延板焼鈍を施さず、かつ、中間焼鈍後の最終冷延圧下率を３０〜８０％の範囲として冷間圧延した場合には、圧延方向の磁束密度Ｂ５０を著しく高めることができることがわかる。 Figure 1 shows the relationship between the B 50 and the final cold rolling reduction ratio of each specimen. From FIG. 1, the hot-rolled sheet containing 0.005 mass% or more of Al as an inhibitor component and 0.003 mass% or more of N is not subjected to hot-rolled sheet annealing, and the final cold rolling reduction ratio after intermediate annealing is shown. when cold rolling as a range of 30% to 80%, it can be seen that can significantly enhance the rolling direction of the magnetic flux density B 50.
次に、上記実験で高い磁束密度を示した表１の鋼Ｂの素材を１２００℃に加熱後、熱間圧延し、板厚２．７ｍｍの熱延板とし、その後、１回目の冷間圧延で中間厚０．８５ｍｍの冷延板とし、次いで、焼鈍温度を７００〜１０００℃に変化させ、保持時間を６０ｓｅｃとした中間焼鈍を施した後、最終冷間圧延して、最終板厚０．３５ｍｍの冷延板とし、その後、この冷延板に、１０００℃×２ｍｉｎの連続焼鈍（仕上焼鈍）を施し、製品板とした。 Next, the steel B material shown in Table 1 that showed high magnetic flux density in the above experiment was heated to 1200 ° C. and hot-rolled to obtain a hot-rolled sheet having a thickness of 2.7 mm, and then the first cold-rolling Then, a cold-rolled sheet having an intermediate thickness of 0.85 mm is obtained. Next, the annealing temperature is changed to 700 to 1000 ° C., an intermediate annealing with a holding time of 60 sec is performed, and then final cold rolling is performed to obtain a final sheet thickness of 0. A 35 mm cold-rolled sheet was formed, and then this cold-rolled sheet was subjected to continuous annealing (finish annealing) at 1000 ° C. for 2 minutes to obtain a product sheet.
斯くして得られた仕上焼鈍後の鋼板からエプスタイン試験片を採取し、上記実験と同様にして、圧延方向の磁束密度Ｂ５０を測定した。図２に、各試験片のＢ５０と中間焼鈍温度との関係を示した。この結果から、中間焼鈍温度を７５０〜９５０℃の範囲とした場合に、圧延方向の磁束密度Ｂ５０を著しく高めることができることがわかる。 Epstein test pieces were sampled from thus to the steel sheet after annealing finish obtained in the same manner as above experiment, the rolling direction of the magnetic flux density B 50. Figure 2 shows the relationship between the B 50 and the intermediate annealing temperature of each specimen. From this result, it can be seen that the magnetic flux density B 50 in the rolling direction can be remarkably increased when the intermediate annealing temperature is in the range of 750 to 950 ° C.
以上の実験結果から、インヒビター成分としてＡｌを０．００５ｍａｓｓ％以上、Ｎを０．００３ｍａｓｓ％以上含有する熱延鋼板を、熱延板焼鈍を施すことなく、７５０〜９５０℃の温度範囲の中間焼鈍を挟む２回以上でかつ最終冷延圧下率を３０〜８０％の範囲とする冷間圧延することで、短時間の連続焼鈍でも容易に二次再結晶を発現させることができることが明らかとなった。 From the above experimental results, intermediate annealing of a hot rolled steel sheet containing 0.005 mass% or more of Al and 0.003 mass% or more of N as an inhibitor component in a temperature range of 750 to 950 ° C. without performing hot rolling sheet annealing. It becomes clear that secondary recrystallization can be easily expressed even in a short time of continuous annealing by performing cold rolling at least twice with a final cold rolling reduction in the range of 30 to 80%. It was.
上記の条件を満たした場合に二次再結晶が容易となる理由については次のように推定される。
まず、連続焼鈍法で二次再結晶させる場合には、バッチ焼鈍法に比べて焼鈍温度が高くなるため、ＡｌＮが固溶してピン止め力（インヒビター効果）が低下するのを防ぐためには、最低限のＡｌとＮが必要と考えられ、０．００５ｍａｓｓ％以上のＡｌ、Ｎ：０．００３ｍａｓｓ％以上のＮがその下限値であると考えられる。
また、短時間の連続焼鈍（仕上焼鈍）で安定して二次再結晶を起こさせるためには、熱間圧延中もしくは中間焼鈍で微細析出したＡｌＮをできるだけ粗大化させずにおくことが必要であると考えられる。したがって、熱延板焼鈍しないこと、および中間焼鈍温度を９５０℃以下とすることは、ＡｌＮの粗大化を防止する効果があると考えられる。
The reason why secondary recrystallization becomes easy when the above conditions are satisfied is estimated as follows.
First, when secondary recrystallization is performed by the continuous annealing method, since the annealing temperature is higher than the batch annealing method, in order to prevent AlN from forming a solid solution and reducing the pinning force (inhibitor effect), The minimum Al and N are considered necessary, and Al of 0.005 mass% or more and N: N of 0.003 mass% or more are considered to be the lower limit values.
In addition, in order to cause secondary recrystallization stably by short-term continuous annealing (finish annealing), it is necessary to keep AlN finely precipitated during hot rolling or intermediate annealing as coarse as possible. It is believed that there is. Therefore, it is considered that not hot-rolled sheet annealing and setting the intermediate annealing temperature to 950 ° C. or less have an effect of preventing AlN from becoming coarse.
また、熱延で形成されるバンド組織は、Ｇｏｓｓ方位粒に蚕食され難く、冷延板まで残留すると、仕上焼鈍での二次再結晶粒の発達を阻害するため、その前に完全に破壊しておく必要があるが、中間焼鈍を７５０℃以上の温度で行うことは、圧延加工組織の再結晶を促進すること以外に、上記バンド組織を破壊する効果があると考えられる。ここで、バンド組織の破壊を、熱延板焼鈍で行わずに中間焼鈍で行う理由は、熱延板は、冷延板に比べて転位が少なく再結晶が起こり難いため、低温の熱延板焼鈍ではバンド組織を十分に破壊することができないためである。また、低温での中間焼鈍は、ＡｌＮの粗大化を防止し、連続焼鈍法で二次再結晶を発現させる上でも好ましいことである。 In addition, the band structure formed by hot rolling is not easily eroded by Goss orientation grains, and if it remains up to the cold-rolled sheet, it inhibits the development of secondary recrystallized grains during finish annealing. However, it is considered that performing the intermediate annealing at a temperature of 750 ° C. or more has an effect of destroying the band structure in addition to promoting recrystallization of the rolled structure. Here, the reason why the band structure is destroyed by intermediate annealing rather than by hot-rolled sheet annealing is that hot-rolled sheets have fewer dislocations and are less likely to recrystallize compared to cold-rolled sheets. This is because annealing cannot sufficiently destroy the band structure. Moreover, the intermediate annealing at a low temperature is preferable for preventing coarsening of AlN and causing secondary recrystallization by a continuous annealing method.
また、最終冷延圧下率を３０〜８０％の範囲とすることは、一次再結晶集合組織にＧｏｓｓ方位粒を増やす効果があると考えられる。Ｇｏｓｓ方位粒は、二次再結晶粒発生までに必要な時間が短くなるため、Ｇｏｓｓ方位粒が多いほど短時間で完全な二次再結晶組織を得ることが可能となる。 Moreover, it is thought that making the final cold rolling reduction ratio in the range of 30 to 80% has an effect of increasing Goss orientation grains in the primary recrystallization texture. The Goss orientation grains shorten the time required until the generation of secondary recrystallized grains. Therefore, the more Goss orientation grains, the more complete secondary recrystallized structure can be obtained in a short time.
すなわち、適切な量のＡｌＮを鋼板中に極微細に分散析出させ、低温の中間焼鈍で熱延バンド組織を破壊し、冷延圧下率を適正に制御して一次再結晶集合組織のＧｏｓｓ方位粒を増やしてやることが、低温・短時間の連続焼鈍で安定して二次再結晶を発現させる上で重要である。本発明は、上記知見に基き、さらに検討を加えて開発したものである。 That is, an appropriate amount of AlN is finely dispersed and precipitated in the steel sheet, the hot-rolled band structure is destroyed by low-temperature intermediate annealing, and the cold rolling reduction ratio is appropriately controlled to goss-oriented grains of the primary recrystallized texture. Increasing the amount is important in order to stably develop secondary recrystallization by low-temperature, short-time continuous annealing. The present invention was developed based on the above findings and further studies.
次に、本発明の方向性電磁鋼板の鋼素材（スラブ）の成分組成について説明する。
Ｃ：０．１２ｍａｓｓ％以下
Ｃは、熱間圧延時のα／γ変態によって結晶組織を均一化する効果がある。また、冷間圧延時の変形帯の形成を促進し、一次再結晶組織中のＧｏｓｓ方位粒を増やすことで、二次再結晶を安定して起こさせる効果がある。しかし、製品鋼板中のＣが０．００５ｍａｓｓ％を超えると、磁気時効を起こして磁気特性が経時劣化する。そのため、鋼素材にＣが０．００５ｍａｓｓ％を超えて含まれる場合には、中間焼鈍や仕上焼鈍で脱炭除去することが望ましい。なお、脱炭処理は、コスト増加の原因となるため、Ｃの添加は必須ではない。一方、Ｃの含有量が０．１２ｍａｓｓ％を超えると、上記脱炭処理で０．００５ｍａｓｓ％以下に低減することが困難となる。よって、Ｃの含有量は０．１２ｍａｓｓ％以下とするが、好ましくは０．０６ｍａｓｓ％以下の範囲である。なお、Ｃは、脱炭焼鈍を行う場合は０．００５ｍａｓｓ％超えでもよいが、行わない場合は０．００５ｍａｓｓ％以下とするのが好ましい。
Next, the component composition of the steel material (slab) of the grain-oriented electrical steel sheet of the present invention will be described.
C: 0.12 mass% or less C has an effect of making the crystal structure uniform by α / γ transformation during hot rolling. In addition, the formation of deformation bands during cold rolling is promoted, and by increasing the number of Goss orientation grains in the primary recrystallization structure, there is an effect of causing secondary recrystallization stably. However, if C in the product steel plate exceeds 0.005 mass%, magnetic aging occurs and the magnetic properties deteriorate over time. Therefore, when C is contained in the steel material exceeding 0.005 mass%, it is desirable to decarburize and remove by intermediate annealing or finish annealing. In addition, since a decarburization process causes a cost increase, addition of C is not essential. On the other hand, when the content of C exceeds 0.12 mass%, it is difficult to reduce the content to 0.005 mass% or less by the decarburization treatment. Therefore, the content of C is set to 0.12 mass% or less, but is preferably in the range of 0.06 mass% or less. In addition, although C may be over 0.005 mass% when performing decarburization annealing, it is preferable to make it 0.005 mass% or less when not performing it.
Ｓｉ：２．０〜４．５ｍａｓｓ％
Ｓｉは、鋼の比抵抗を高めて鉄損を改善する効果があり、この効果を得るためには２．０ｍａｓｓ％以上の添加が必要である。一方、４．５ｍａｓｓ％を超えて添加すると、冷間圧延することが困難となる。よって、Ｓｉの含有量は２．０〜４．５ｍａｓｓ％の範囲とする。好ましくは２．８〜３．８ｍａｓｓ％の範囲である。
Si: 2.0 to 4.5 mass%
Si has an effect of improving the iron loss by increasing the specific resistance of the steel. In order to obtain this effect, addition of 2.0 mass% or more is necessary. On the other hand, when it exceeds 4.5 mass%, it will become difficult to cold-roll. Therefore, the Si content is in the range of 2.0 to 4.5 mass%. Preferably it is the range of 2.8-3.8 mass%.
Ｍｎ：０．００５〜０．３ｍａｓｓ％
Ｍｎは、Ｓによる熱間圧延時の割れを防止する効果がある。また、微細なＳ化合物、Ｓｅ化合物を形成して一次再結晶組織の成長を阻害して、二次再結晶を促進する効果（インヒビター効果）もある。しかし、Ｍｎ含有量が０．００５ｍａｓｓ％以下では上記効果は小さく、一方、０．３ｍａｓｓ％を超えて添加しても上記効果が飽和するだけである。よって、Ｍｎの含有量は０．００５〜０．３ｍａｓｓ％の範囲とする。好ましくは０．０２〜０．１ｍａｓｓ％の範囲である。
Mn: 0.005 to 0.3 mass%
Mn has an effect of preventing cracking during hot rolling due to S. In addition, there is an effect (inhibitor effect) of forming a fine S compound or Se compound to inhibit the growth of the primary recrystallization structure to promote secondary recrystallization. However, when the Mn content is 0.005 mass% or less, the above effect is small. On the other hand, adding more than 0.3 mass% only saturates the above effect. Therefore, the Mn content is in the range of 0.005 to 0.3 mass%. Preferably it is the range of 0.02-0.1 mass%.
Ａｌ：０．００５〜０．０１２ｍａｓｓ％
Ａｌは、Ｎと微細なＡｌＮを形成し、一次再結晶組織の成長を阻害するインヒビター効果のある本発明における重要な元素である。しかし、Ａｌが０．００５ｍａｓｓ％未満では十分なインヒビター効果が得られない。一方、Ａｌが０．０１２ｍａｓｓ％を超えると、ＡｌＮの微細分散が困難となるので、Ａｌは０．００５〜０．０１２ｍａｓｓ％の範囲とする。好ましくは０．００６〜０．０９ｍａｓｓ％の範囲である。
Al: 0.005-0.012 mass%
Al is an important element in the present invention having an inhibitor effect that forms fine AlN with N and inhibits the growth of the primary recrystallized structure. However, if the Al content is less than 0.005 mass%, a sufficient inhibitor effect cannot be obtained. On the other hand, if Al exceeds 0.012 mass%, it becomes difficult to finely disperse AlN, so Al is set in the range of 0.005 to 0.012 mass%. Preferably it is the range of 0.006-0.09 mass%.
Ｎ：０．００３０〜０．０１０ｍａｓｓ％
Ｎは、Ａｌと微細なＡｌＮを形成し、一次再結晶組織の成長を阻害するインヒビター効果のある本発明における重要な元素である。しかし、Ｎが０．００３０ｍａｓｓ％未満では十分なインヒビター効果が得られない。一方、Ｎが０．０１２ｍａｓｓ％を超えると、ブリスターとよばれる表面欠陥が発生するようになる。よって、Ｎは０．００３０〜０．０１２ｍａｓｓ％の範囲とする。好ましくは０．００３５〜０．００６０ｍａｓｓ％の範囲である。
N: 0.0030 to 0.010 mass%
N is an important element in the present invention having an inhibitor effect that forms fine AlN with Al and inhibits the growth of the primary recrystallized structure. However, if N is less than 0.0030 mass%, a sufficient inhibitor effect cannot be obtained. On the other hand, when N exceeds 0.012 mass%, surface defects called blisters are generated. Therefore, N is set to a range of 0.0030 to 0.012 mass%. Preferably it is the range of 0.0035-0.0060mass%.
本発明の方向性電磁鋼板に用いる鋼素材は、上記成分の他に、以下の元素を含有していてもよい。
Ｓｂ：０．００５〜０．２ｍａｓｓ％、Ｓｎ：０．００５〜０．２ｍａｓｓ％
ＳｂおよびＳｎは、一次再結晶集合組織を改善し、二次再結晶を安定化する効果がある。また、焼鈍中の酸化を防止して、磁気特性の劣化を防ぐ効果もある。このような効果を得るためには、それぞれ０．００５ｍａｓｓ％以上添加するのが好ましい。しかし、０．２ｍａｓｓ％を超えて添加すると、鋼板が脆化するようになる。よって、ＳｂおよびＳｎを添加する場合は、それぞれ０．００５〜０．２ｍａｓｓ％の範囲とする。より好ましくは０．０１〜０．１ｍａｓｓ％の範囲である。
The steel material used for the grain-oriented electrical steel sheet of the present invention may contain the following elements in addition to the above components.
Sb: 0.005-0.2 mass%, Sn: 0.005-0.2 mass%
Sb and Sn have an effect of improving the primary recrystallization texture and stabilizing the secondary recrystallization. It also has the effect of preventing oxidation during annealing and preventing deterioration of magnetic properties. In order to acquire such an effect, it is preferable to add 0.005 mass% or more, respectively. However, if added over 0.2 mass%, the steel sheet becomes brittle. Therefore, when adding Sb and Sn, it is set as the range of 0.005-0.2 mass%, respectively. More preferably, it is the range of 0.01-0.1 mass%.
Ｃｕ：０．０１〜０．２ｍａｓｓ％、Ｓ：０．００１〜０．０２ｍａｓｓ％、Ｓｅ：０．００１〜０．０２ｍａｓｓ％、Ｂ：０．０００１〜０．００５ｍａｓｓ％
Ｃｕ，Ｓ，ＳｅおよびＢは、いずれも微細な析出物を形成して一次再結晶組織の成長を阻害するインヒビター効果のある元素であり、補助的なインヒビター元素として添加することができる。しかし、Ｃｕ：０．０１ｍａｓｓ％未満、Ｓ：０．００１ｍａｓｓ％未満、Ｓｅ：０．００１％未満およびＢ：０．０００１ｍａｓｓ％未満では、十分なインヒビター効果が得られず、一方、Ｃｕ：０．２ｍａｓｓ％超え、Ｓ：０．０２ｍａｓｓ％超え、Ｓｅ：０．０２ｍａｓｓ％超えおよびＢ：０．００５ｍａｓｓ％超えでは、析出物の微細分散が困難となる。よって、Ｃｕ，Ｓ，ＳｅおよびＢは、それぞれ上記範囲で添加するのが好ましい。より好ましい範囲は、それぞれＣｕ：０．０２〜０．１ｍａｓｓ％、Ｓ：０．００２〜０．０１ｍａｓｓ％、Ｓｅ：０．００２〜０．０１ｍａｓｓ％およびＢ：０．０００２〜０．００２ｍａｓｓ％の範囲である。
Cu: 0.01-0.2 mass%, S: 0.001-0.02 mass%, Se: 0.001-0.02 mass%, B: 0.0001-0.005 mass%
Cu, S, Se, and B are all elements having an inhibitory effect that inhibits the growth of the primary recrystallized structure by forming fine precipitates, and can be added as auxiliary inhibitor elements. However, when Cu is less than 0.01 mass%, S is less than 0.001 mass%, Se is less than 0.001%, and B is less than 0.0001 mass%, a sufficient inhibitory effect cannot be obtained, while Cu = 0. If it exceeds 2 mass%, S: exceeds 0.02 mass%, Se: exceeds 0.02 mass%, and B: exceeds 0.005 mass%, fine dispersion of the precipitate becomes difficult. Therefore, Cu, S, Se, and B are preferably added in the above ranges. More preferable ranges are Cu: 0.02-0.1 mass%, S: 0.002-0.01 mass%, Se: 0.002-0.01 mass%, and B: 0.0002-0.002 mass%, respectively. It is a range.
次に、本発明の方向性電磁鋼板の製造方法について説明する。
本発明に適合する上記成分組成に調整した鋼を溶製し、連続鋳造法または造塊−分塊圧延法を用いて所定厚みの鋼素材（スラブ）とした後、このスラブを再加熱し、熱間圧延して熱延板とする。上記熱間圧延前のスラブ加熱は、インヒビターの固溶温度以上で行うのが好ましいが、生産性や製造コストの観点から、１２５０℃以下で行うのが好ましい。なお、スラブ加熱温度は、低温ほど熱延板のバンド組織の発達が抑制されるため、二次再結晶を安定化させる観点からも、低温度で行うのが好ましい。また、熱間圧延条件は、通常公知の条件であればよく、特に制限はない。
Next, the manufacturing method of the grain-oriented electrical steel sheet of this invention is demonstrated.
After melting the steel adjusted to the above component composition suitable for the present invention and using a continuous casting method or ingot-bundling rolling method to obtain a steel material (slab) of a predetermined thickness, the slab is reheated, Hot rolled into hot rolled sheets. The slab heating before the hot rolling is preferably performed at a temperature equal to or higher than the solid solution temperature of the inhibitor, but is preferably performed at 1250 ° C. or less from the viewpoint of productivity and manufacturing cost. In addition, since the development of the band structure of a hot-rolled sheet is suppressed as the slab heating temperature is lower, it is preferably performed at a lower temperature from the viewpoint of stabilizing secondary recrystallization. Further, the hot rolling conditions may be any generally known conditions and are not particularly limited.
熱間圧延した鋼板は、一般的な方向性電磁鋼板の製造方法では、熱延板焼鈍を施すことが多い。しかし、インヒビターの粗大化を防止する観点からは好ましくないので、本発明においては、熱延板焼鈍は必須の工程ではない。したがって、熱延板焼鈍を行う場合には、インヒビターを粗大化させないため、９５０℃以下の温度で行う必要がある。好ましい熱延板焼鈍温度は８８０℃以下である。なお、９５０℃以下の熱延板焼鈍では、バンド組織を完全には破壊できないため、後述する中間焼鈍は必須の工程である。 The hot-rolled steel sheet is often subjected to hot-rolled sheet annealing in a general method for producing a grain-oriented electrical steel sheet. However, since it is not preferable from the viewpoint of preventing the coarsening of the inhibitor, hot-rolled sheet annealing is not an essential process in the present invention. Therefore, when hot-rolled sheet annealing is performed, it is necessary to perform the annealing at a temperature of 950 ° C. or lower in order not to coarsen the inhibitor. A preferable hot-rolled sheet annealing temperature is 880 ° C. or less. In addition, in the hot-rolled sheet annealing at 950 ° C. or lower, the band structure cannot be completely destroyed, and therefore the intermediate annealing described later is an essential process.
上記熱間圧延後、あるいは、熱延板焼鈍後の熱延板は、その後、中間焼鈍を挟む２回以上の冷間圧延を行って所定の最終板厚の冷延板とし、連続焼鈍炉で仕上焼鈍し、必要に応じて絶縁コーティングを施して製品板とする。 The hot-rolled sheet after the hot rolling or after the hot-rolled sheet annealing is then cold-rolled to a predetermined final thickness by performing cold rolling at least twice with the intermediate annealing in a continuous annealing furnace. Finish annealing, and if necessary, apply an insulating coating to make a product plate.
ここで、上記中間焼鈍の温度は７５０〜９５０℃、最終冷間圧延の圧下率（最終冷延圧下率）は３０〜８０％の範囲とすることが必要である。中間焼鈍温度が７５０℃未満では、熱間圧延したときのバンド組織が残留しやすく、二次再結晶が不安定化となる。一方、中間焼鈍温度が９５０℃を超えると、ＡｌＮが粗大化し、十分なピン止め力（インヒビター効果）が得られない。また、最終冷延圧下率が３０〜８０％から外れると、一次再結晶集合組織中にＧｏｓｓ方位粒が少なくなり、二次再結晶が不安定化する。好ましい中間焼鈍温度は７８０〜８８０℃、最終冷延圧下率は５０〜７０％の範囲である。
なお、２回以上の中間焼鈍を行う場合、すなわち、３回以上の冷間圧延を行う場合には、磁気特性を向上させる観点から、最終冷間圧延に限らず全ての冷延圧下率を３０〜８０％とするのが好ましく、５０〜７０％とするのがより好ましい。
Here, the temperature of the intermediate annealing is required to be in the range of 750 to 950 ° C., and the reduction ratio of the final cold rolling (final cold rolling reduction ratio) is in the range of 30 to 80%. When the intermediate annealing temperature is less than 750 ° C., the band structure when hot rolled tends to remain, and the secondary recrystallization becomes unstable. On the other hand, if the intermediate annealing temperature exceeds 950 ° C., AlN becomes coarse and sufficient pinning force (inhibitor effect) cannot be obtained. On the other hand, if the final cold rolling reduction falls from 30 to 80%, the number of Goss orientation grains decreases in the primary recrystallization texture, and the secondary recrystallization becomes unstable. The preferred intermediate annealing temperature is 780 to 880 ° C., and the final cold rolling reduction is in the range of 50 to 70%.
In addition, when performing the intermediate annealing 2 times or more, that is, when performing the cold rolling 3 times or more, from the viewpoint of improving the magnetic properties, not only the final cold rolling but all the cold rolling reduction ratios are 30. It is preferable to set it to -80%, and it is more preferable to set it as 50-70%.
冷間圧延に続く連続焼鈍法を用いた仕上焼鈍は、製造性やエネルギーコスト等の観点から、均熱温度１０２０℃以下、均熱時間３分以下の条件で行うことが好ましい。前述したように、１０２０℃を超える均熱温度は、連続焼鈍炉への通板性が悪化したり、押し疵発生の原因となったり、焼鈍炉の負荷が大きくなったりし、また、３分以上の均熱時間は、生産性を低下させたり、製造コストの上昇を招いたりするからである。
なお、鋼素材のＣが０．００５ｍａｓｓ％超えである場合には、湿潤Ｈ２／Ｎ２雰囲気中で８５０℃程度の温度で脱炭焼鈍を施してから、上記仕上焼鈍して二次再結晶させるのが好ましい。
Finish annealing using the continuous annealing method subsequent to cold rolling is preferably performed under conditions of a soaking temperature of 1020 ° C. or less and a soaking time of 3 minutes or less from the viewpoints of manufacturability and energy costs. As described above, a soaking temperature exceeding 1020 ° C. deteriorates the plate-passability to the continuous annealing furnace, causes the occurrence of pressing iron, and increases the load on the annealing furnace. This is because the soaking time described above decreases the productivity and increases the manufacturing cost.
When C of the steel material exceeds 0.005 mass%, decarburization annealing is performed at a temperature of about 850 ° C. in a wet H 2 / N 2 atmosphere, and then the above-described finish annealing is performed to perform secondary recrystallization. It is preferable to do so.
なお、上記仕上焼鈍は、複数回行ってもよい。また、連続焼鈍で二次再結晶させた後、さらに焼鈍を行ってもよく、例えば、二次再結晶焼鈍後に浸珪処理を行い、Ｓｉ含有量を６．５ｍａｓｓ％程度まで増加させることは、鉄損や騒音の低減に効果的である。また、二次再結晶焼鈍と浸珪処理を同時に行ってもよい。 The finish annealing may be performed a plurality of times. Further, after secondary recrystallization by continuous annealing, further annealing may be performed, for example, performing a siliconization treatment after secondary recrystallization annealing, and increasing the Si content to about 6.5 mass%, Effective for reducing iron loss and noise. Moreover, you may perform a secondary recrystallization annealing and a siliconization process simultaneously.
上記に説明したように、本発明の製造方法は、低温・短時間の仕上焼鈍でも安定して二次再結晶を起こさせることができるので、磁気特性（磁束密度Ｂ５０）に優れる方向性電磁鋼板を、安価にかつ大量に提供することができるところに特長がある。なお、本発明により得られる鋼板の二次再結晶組織は、従来のコイルフォームでバッチ焼鈍して得られる一般的な方向性電磁鋼板に比較して配向性の面で劣る傾向にある。しかし、Ｇｏｓｓ方位の圧延方向への配向性が高度に高まると、逆に圧延直角方向に励磁し難くなるため、ある程度の配向性の優劣は、回転機やＥＩコアの性能に及ぼす影響は小さいと考えられる。 As described above, the production method of the present invention can cause secondary recrystallization stably even at a low-temperature and short-time finish annealing, so that the directional electromagnetic excellent in magnetic characteristics (magnetic flux density B 50 ). It is characterized in that steel sheets can be provided at low cost and in large quantities. In addition, the secondary recrystallization structure of the steel sheet obtained by the present invention tends to be inferior in terms of orientation as compared with a general grain-oriented electrical steel sheet obtained by batch annealing with a conventional coil foam. However, if the orientation of the Goss orientation in the rolling direction is highly enhanced, it becomes difficult to excite in the direction perpendicular to the rolling direction. Therefore, a certain degree of orientation has little effect on the performance of the rotating machine or EI core. Conceivable.
表２に示した成分組成を有するＡ〜Ｎの鋼を溶製し、連続鋳造して鋼素材（スラブ）とした後、このスラブを１２００℃に加熱後、熱間圧延して板厚２．７ｍｍの熱延板とした。次いで、１回目の冷間圧延で板厚０．８５ｍｍの冷延板とし、乾燥窒素雰囲気で８１０℃×５０秒の中間焼鈍を施した後、最終冷間圧延で最終板厚０．３５ｍｍの冷延板とした。その後、上記冷延板を、連続焼鈍炉を用いて、Ｈ２：３０ｖｏｌ％＋Ｎ２：７０ｖｏｌ％、露点：３０℃の雰囲気中で８５０℃×６０秒の脱炭焼鈍を兼ねた一次再結晶焼鈍した後、連続焼鈍炉を用いて、Ｈ２：２０ｖｏｌ％＋Ｎ２：８０ｖｏｌ％の乾燥雰囲気中で９９５℃×１２０秒の仕上焼鈍を施し、製品板とした。 The steels A to N having the composition shown in Table 2 were melted and continuously cast to obtain a steel material (slab), which was then heated to 1200 ° C. and hot-rolled to obtain a plate thickness of 2. A 7 mm hot-rolled sheet was used. Next, a cold-rolled sheet having a thickness of 0.85 mm was obtained by the first cold rolling, subjected to intermediate annealing at 810 ° C. for 50 seconds in a dry nitrogen atmosphere, and then cooled to a final thickness of 0.35 mm by final cold rolling. It was a sheet. Then, the above-mentioned cold-rolled sheet is subjected to primary recrystallization annealing that also serves as decarburization annealing at 850 ° C. for 60 seconds in an atmosphere of H 2 : 30 vol% + N 2 : 70 vol% and dew point: 30 ° C. using a continuous annealing furnace. Then, using a continuous annealing furnace, finish annealing was performed at 995 ° C. for 120 seconds in a dry atmosphere of H 2 : 20 vol% + N 2 : 80 vol% to obtain a product plate.
斯くして得られた製品板から、エプスタイン試験片を採取し、圧延方向の磁束密度Ｂ５０を測定した。また、上記試験片をマクロエッチングし、肉眼で二次再結晶粒が確認できたものについては、その平均結晶粒径を測定した。
上記の結果を表２に併記して示した。この結果から、ＡｌおよびＮを本発明の範囲で含有する鋼から製造された製品板は、粗大な二次再結晶粒が発現しており、優れた磁束密度Ｂ５０が得られていることがわかる。
From the product plate thus obtained, an Epstein test piece was collected and the magnetic flux density B 50 in the rolling direction was measured. Moreover, the said test piece was macroetched and the average crystal grain diameter was measured about what could confirm the secondary recrystallized grain with the naked eye.
The above results are shown together in Table 2. From this result, the product plate manufactured from the steel containing Al and N within the scope of the present invention expresses coarse secondary recrystallized grains, and an excellent magnetic flux density B50 is obtained. Recognize.
Ｃ：０．００２ｍａｓｓ％、Ｓｉ：３．３９ｍａｓｓ％、Ｍｎ：０．０７ｍａｓｓ％、Ａｌ：０．００７９ｍａｓｓ％、Ｎ：０．００４１ｍａｓｓ％、Ｓ：０．００１８ｍａｓｓ％、Ｃｕ：０．０２ｍａｓｓ％、残部がＦｅおよび不可避不純物からなる成分組成を有するスラブを１２００℃に加熱後、熱間圧延して板厚２．６ｍｍの熱延板とした後、表３に示した温度で、乾燥窒素雰囲気中で均熱時間６０秒の熱延板焼鈍を施した後、あるいは熱延板焼鈍を施さずに、１回目の冷間圧延で中間厚とし、その後、同じく表３に示した温度で、乾燥窒素雰囲気中で均熱時間６０秒の中間焼鈍を施した後、あるいは中間焼鈍を施さずに、２回目の冷間圧延（最終冷間圧延）して最終板厚０．３５ｍｍの冷延板とした。その後、この冷延板を、連続焼鈍炉を用いて、Ｈ２：２０ｖｏｌ％＋Ｎ２：８０ｖｏｌ％の乾燥雰囲気中で１００５℃×１１０秒の仕上焼鈍を施し、製品板とした。 C: 0.002 mass%, Si: 3.39 mass%, Mn: 0.07 mass%, Al: 0.0079 mass%, N: 0.0041 mass%, S: 0.0018 mass%, Cu: 0.02 mass%, balance After heating a slab having a composition composed of Fe and inevitable impurities to 1200 ° C. and hot rolling to obtain a hot-rolled sheet having a thickness of 2.6 mm, in a dry nitrogen atmosphere at the temperature shown in Table 3 After performing hot-rolled sheet annealing with a soaking time of 60 seconds, or without performing hot-rolled sheet annealing, an intermediate thickness is obtained by the first cold rolling, and then a dry nitrogen atmosphere at the same temperature shown in Table 3 After performing intermediate annealing with a soaking time of 60 seconds in the middle or without intermediate annealing, the second cold rolling (final cold rolling) was performed to obtain a cold rolled sheet having a final sheet thickness of 0.35 mm. Then, this cold-rolled sheet was subjected to finish annealing at 1005 ° C. × 110 seconds in a dry atmosphere of H 2 : 20 vol% + N 2 : 80 vol% using a continuous annealing furnace to obtain a product sheet.
斯くして得られた製品板から、エプスタイン試験片を採取し、圧延方向の磁束密度Ｂ５０を測定した。また、上記試験片をマクロエッチングし、肉眼で二次再結晶粒が確認できたものについては、その平均結晶粒径を測定した。
上記の結果を製造条件と共に表３に示した。この結果から、熱延板焼鈍温度、中間焼鈍温度および最終冷延圧下率が本発明の条件を満たして製造された鋼板は、いずれも粗大な二次再結晶粒が発現しており、優れたＢ５０が得られていることがわかる。
From the product plate thus obtained, an Epstein test piece was collected and the magnetic flux density B 50 in the rolling direction was measured. Moreover, the said test piece was macroetched and the average crystal grain diameter was measured about what could confirm the secondary recrystallized grain with the naked eye.
The results are shown in Table 3 together with the production conditions. From this result, the steel sheet produced by satisfying the conditions of the present invention in which the hot-rolled sheet annealing temperature, the intermediate annealing temperature, and the final cold rolling reduction rate satisfy the conditions of the present invention, all expressed coarse secondary recrystallized grains. it can be seen that B 50 is obtained.
Ｃ：０．０１２ｍａｓｓ％、Ｓｉ：３．１８ｍａｓｓ％、Ｍｎ：０．１１ｍａｓｓ％、Ａｌ：０．００８５ｍａｓｓ％、Ｎ：０．００４３ｍａｓｓ％、Ｓｂ：０．０２ｍａｓｓ％、残部がＦｅおよび不可避不純物からなる成分組成を有するスラブを１２１０℃に加熱後、熱間圧延して板厚２．４ｍｍの熱延板とし、乾燥窒素雰囲気中で所定の温度で均熱時間６０秒の熱延板焼鈍を施し、あるいは熱延板焼鈍を施さずに、１回目の冷間圧延して所定の中間板厚とし、その後、乾燥窒素雰囲気中で所定の温度で均熱時間６０秒の１回目の中間焼鈍し、あるいは中間焼鈍せずに、２回目の冷間圧延して所定の中間板厚とし、その後さらに、乾燥窒素雰囲気中で所定の温度で均熱時間６０秒の２回目の中間焼鈍を施し、あるいは中間焼鈍せずに、所定の圧下率で３回目の冷間圧延（最終冷間圧延）して最終板厚０．１ｍｍの冷延板とした。その後、この冷延板を、連続焼鈍炉を用いて、Ｈ２：３０ｖｏｌ％＋Ｎ２：７０ｖｏｌ％、露点：３０℃の雰囲気中で８５０℃×６０秒の脱炭焼鈍を兼ねた一次再結晶焼鈍した後、連続焼鈍炉を用いて、Ｈ２：２０ｖｏｌ％＋Ｎ２：８０ｖｏｌ％の乾燥雰囲気中で９９８℃×１３０秒の仕上焼鈍を施し、製品板とした。 C: 0.012 mass%, Si: 3.18 mass%, Mn: 0.11 mass%, Al: 0.0085 mass%, N: 0.0043 mass%, Sb: 0.02 mass%, the balance being Fe and inevitable impurities After heating the slab having the component composition to 1210 ° C., it is hot-rolled to form a hot-rolled sheet having a thickness of 2.4 mm, and subjected to hot-rolled sheet annealing at a predetermined temperature in a dry nitrogen atmosphere for 60 seconds, Alternatively, without performing hot-rolled sheet annealing, the first cold rolling is performed to a predetermined intermediate sheet thickness, and then the first intermediate annealing is performed at a predetermined temperature in a dry nitrogen atmosphere at a predetermined temperature of 60 seconds, or Without intermediate annealing, the second cold rolling is performed to a predetermined intermediate sheet thickness, and then a second intermediate annealing is performed in a dry nitrogen atmosphere at a predetermined temperature for a soaking time of 60 seconds, or intermediate annealing is performed. Without prescribed Third cold rolling at a reduction ratio (final cold rolling) to the cold rolled sheet having a final thickness of 0.1 mm. Then, this cold-rolled sheet was subjected to primary recrystallization annealing that also served as decarburization annealing at 850 ° C. for 60 seconds in an atmosphere of H 2 : 30 vol% + N 2 : 70 vol%, dew point: 30 ° C., using a continuous annealing furnace. Then, using a continuous annealing furnace, finish annealing was performed at 998 ° C. for 130 seconds in a dry atmosphere of H 2 : 20 vol% + N 2 : 80 vol% to obtain a product plate.
斯くして得られた製品板から、エプスタイン試験片を採取し、圧延方向の磁束密度Ｂ５０を測定した。また、上記試験片をマクロエッチングし、肉眼で二次再結晶粒が確認できたものについては、その平均結晶粒径を測定した。
上記の結果を、製造条件と共に表４に示した。この結果から、熱延板焼鈍温度、中間焼鈍温度および最終冷延圧下率が本発明の条件を満たして製造された鋼板は、いずれも粗大な二次再結晶粒が発現しており、優れたＢ５０が得られていることがわかる。
From the product plate thus obtained, an Epstein test piece was collected and the magnetic flux density B 50 in the rolling direction was measured. Moreover, the said test piece was macroetched and the average crystal grain diameter was measured about what could confirm the secondary recrystallized grain with the naked eye.
The results are shown in Table 4 together with the production conditions. From this result, the steel sheet produced by satisfying the conditions of the present invention in which the hot-rolled sheet annealing temperature, the intermediate annealing temperature, and the final cold rolling reduction rate satisfy the conditions of the present invention, all expressed coarse secondary recrystallized grains. it can be seen that B 50 is obtained.
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| JP2023508029A (en) * | 2019-12-20 | 2023-02-28 | ポスコホールディングス インコーポレーティッド | Grain-oriented electrical steel sheet and manufacturing method thereof |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |