JP6808830B2 - Electrical steel sheet and its manufacturing method - Google Patents

Electrical steel sheet and its manufacturing method Download PDF

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JP6808830B2
JP6808830B2 JP2019522885A JP2019522885A JP6808830B2 JP 6808830 B2 JP6808830 B2 JP 6808830B2 JP 2019522885 A JP2019522885 A JP 2019522885A JP 2019522885 A JP2019522885 A JP 2019522885A JP 6808830 B2 JP6808830 B2 JP 6808830B2
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steel sheet
weight
grain
electrical steel
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スゥ パク，チャン
スゥ パク，チャン
ハン，ギュソク
ドン ジュ，ヒョン
ドン ジュ，ヒョン
ソ，ジンウク
キム，ウシン
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Posco Holdings Inc
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • 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
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/005—Heat treatment of ferrous alloys containing Mn
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/008—Heat treatment of ferrous alloys containing Si
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0226—Hot rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0236—Cold rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • C21D8/0263—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment following hot rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets

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  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Soft Magnetic Materials (AREA)

Description

本発明は、方向性電磁鋼板およびその製造方法に係り、より詳しくは、Ｂ、Ｂａ、Ｙを一定量含ませて、結晶粒界に偏析させた方向性電磁鋼板およびその製造方法に関する。 The present invention relates to a grain-oriented electrical steel sheet and a method for producing the same, and more particularly to a grain-oriented electrical steel sheet obtained by containing a certain amount of B, Ba, and Y and segregating at grain boundaries and a method for producing the same.

方向性電磁鋼板は、鋼板の結晶方位が｛１１０｝＜００１＞である、別名、ゴス（Ｇｏｓｓ）方位を有する結晶粒からなる、圧延方向への磁気的特性に優れた軟磁性材料である。
一般に、磁気特性は、磁束密度と鉄損で表現され、高い磁束密度は、結晶粒の方位を｛１１０｝＜００１＞方位に正確に配列することにより得られる。磁束密度が高い電磁鋼板は、電気機器の鉄心材料の大きさを小さくできるだけでなく、履歴損失が低くなって電気機器の小型化と同時に高効率化を高めることができる。鉄損は、鋼板に任意の交流磁場を加えた時、熱エネルギーとして消費される電力損失であって、鋼板の磁束密度と板厚さ、鋼板中の不純物量、比抵抗、そして２次再結晶粒の大きさなどによって大きく変化し、磁束密度と比抵抗が高いほど、そして板厚さと鋼板中の不純物量が低いほど、鉄損が低くなって電気機器の効率が増加する。 The grain-oriented electrical steel sheet is a soft magnetic material having excellent magnetic properties in the rolling direction, which is composed of crystal grains having a crystal orientation of {110} <001>, also known as a Goss orientation.
Generally, the magnetic characteristics are expressed by the magnetic flux density and the iron loss, and the high magnetic flux density is obtained by accurately arranging the orientations of the crystal grains in the {110} <001> orientation. An electromagnetic steel sheet having a high magnetic flux density can not only reduce the size of the iron core material of an electric device, but also reduce the history loss, so that the electric device can be miniaturized and the efficiency can be improved at the same time. Iron loss is the power loss consumed as thermal energy when an arbitrary alternating magnetic field is applied to a steel plate, and is the magnetic flux density and thickness of the steel plate, the amount of impurities in the steel plate, the specific resistance, and the secondary recrystallization. It varies greatly depending on the grain size and the like, and the higher the magnetic flux density and specific resistance, and the lower the plate thickness and the amount of impurities in the steel plate, the lower the iron loss and the higher the efficiency of electrical equipment.

現在、全世界的にＣＯ２発生を低減することで地球温暖化に対処するために、エネルギー節約と共に高効率製品化を目指す傾向にあり、電気エネルギーを少なく使用する高効率化された電気機器の拡大普及に対する需要が増加するに伴い、より優れた低鉄損特性を有する方向性電磁鋼板の開発に対する社会的要求が増大している。
一般に、磁気特性に優れた方向性電磁鋼板は、鋼板の圧延方向に｛１１０｝＜００１＞方位のゴス組織（Ｇｏｓｓ ｔｅｘｔｕｒｅ）が強く発達しなければならず、このような集合組織を形成させるためには、ゴス方位の結晶粒が２次再結晶という異常な結晶粒成長を形成させなければならない。このような異常な結晶成長は、通常の結晶粒成長とは異なり、正常な結晶粒成長が析出物、介在物やあるいは固溶または粒界に偏析する元素によって正常に成長する結晶粒界の移動が抑制された時に発生する。このように結晶粒成長を抑制する析出物や介在物などを特に結晶粒成長抑制剤（ｉｎｈｉｂｉｔｏｒ）と呼び、｛１１０｝＜００１＞方位の２次再結晶による方向性電磁鋼板の製造技術に関する研究は、強い結晶粒成長抑制剤を用いて｛１１０｝＜００１＞方位に対する集積度が高い２次再結晶を形成して優れた磁気特性を確保するのに力を注いできた。 Currently, in order to deal with global warming by reducing CO 2 emissions worldwide, there is a tendency to aim for high-efficiency products as well as energy saving, and highly efficient electrical equipment that uses less electrical energy. As the demand for expansion and dissemination increases, the social demand for the development of grain-oriented electrical steel sheets having better low iron loss characteristics is increasing.
Generally, in a directional electromagnetic steel sheet having excellent magnetic properties, a Goss texture in the {110} <001> direction must be strongly developed in the rolling direction of the steel sheet, and in order to form such an aggregate structure. In order, the grains in the Goth orientation must form an abnormal grain growth called secondary recrystallization. Such abnormal crystal growth is different from normal grain growth, and the movement of grain boundaries in which normal grain growth normally grows due to precipitates, inclusions, or elements that segregate into solid solutions or grain boundaries. Occurs when is suppressed. Precipitates and inclusions that suppress grain growth in this way are particularly called grain growth inhibitors (inhibitors), and research on manufacturing technology for directional electromagnetic steel sheets by secondary recrystallization in the {110} <001> orientation. Has focused its efforts on forming secondary recrystallization with a high degree of integration with respect to the {110} <001> orientation using a strong grain growth inhibitor to ensure excellent magnetic properties.

既存の方向性電磁鋼板技術では、主に、ＡｌＮ、ＭｎＳ［Ｓｅ］などの析出物を結晶粒成長抑制剤として用いている。一例として、１回の強冷間圧延後、脱炭を実施した後に、アンモニアガスを用いた別途の窒化工程により、鋼板の内部に窒素を供給して強い結晶粒成長抑制効果を発揮するＡｌ系の窒化物によって２次再結晶を起こす製造方法がある。
しかし、高温焼鈍過程で炉内雰囲気による脱窒または復窒による析出物の不安定性の深刻化および高温で３０時間以上の長時間の純化焼鈍が必要であるという点は、製造工程上の複雑性とコスト負担を伴う。 In the existing grain-oriented electrical steel sheet technology, precipitates such as AlN and MnS [Se] are mainly used as a crystal grain growth inhibitor. As an example, after one strong cold rolling and decarburization, nitrogen is supplied to the inside of the steel sheet by a separate nitriding process using ammonia gas to exert a strong grain growth suppressing effect. There is a manufacturing method in which secondary recrystallization is caused by the nitride of the above.
However, the complexity of the manufacturing process is that the instability of the precipitate due to denitrification or renitrification due to the atmosphere in the furnace becomes serious in the high temperature annealing process, and that long-term purification annealing at high temperature for 30 hours or more is required. And cost burden.

このような理由から、最近、ＡｌＮ、ＭｎＳなどの析出物を結晶粒成長抑制剤として使用せずに方向性電磁鋼板を製造する方法が提案されている。一例として、バリウム（Ｂａ）およびイットリウム（Ｙ）などの粒界偏析元素を用いる製造方法がある。
ＢａおよびＹは、２次再結晶の形成が可能なほど結晶粒成長抑制効果に優れ、高温焼鈍過程で炉内雰囲気の影響を受けないなどの利点があるが、粒界の結合力を弱めるという欠点がある。したがって、強圧下が必要な冷間圧延過程で粒界クラックが多数発生して生産性の低下を避けられなくなる問題がある。 For this reason, recently, a method for producing grain-oriented electrical steel sheets without using precipitates such as AlN and MnS as a crystal grain growth inhibitor has been proposed. As an example, there is a production method using grain boundary segregation elements such as barium (Ba) and yttrium (Y).
Ba and Y are excellent in the effect of suppressing grain growth so that secondary recrystallization can be formed, and have advantages such as not being affected by the atmosphere in the furnace during the high temperature annealing process, but they are said to weaken the binding force of the grain boundaries. There are drawbacks. Therefore, there is a problem that a large number of grain boundary cracks are generated in the cold rolling process that requires strong reduction, and a decrease in productivity cannot be avoided.

本発明の目的とするところは、方向性電磁鋼板およびその製造方法を提供することにある。 An object of the present invention is to provide a grain-oriented electrical steel sheet and a method for producing the same.

本発明の一実施例による方向性電磁鋼板は、重量％で、Ｓｉ：１．０〜７．０％、Ｂ：０．００１〜０．１％、およびＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％含み、残部はＦｅおよびその他の不可避不純物を含むこと位を特徴とする。 The grain-oriented electrical steel sheet according to an embodiment of the present invention contains Si: 1.0 to 7.0%, B: 0.001 to 0.1%, and Ba and Y alone or in total in% by weight. It is characterized by containing 0.005% by weight to 0.5% by weight, and the balance containing Fe and other unavoidable impurities.

本発明の一実施例による方向性電磁鋼板は、下記式１を満足することができる。
［式１］
０．５≦（［Ｂａ］＋［Ｙ］）／（［Ｂ］＊１０）≦３
（ただし、式１中、［Ｂａ］、［Ｙ］、［Ｂ］は、それぞれＢａ、Ｙ、Ｂの含有量（重量％）を示す。）
Ｃ：０．００５％以下（０％を除く）、Ａｌ：０．００５％以下（０％を除く）、Ｎ：０．００５５％以下（０％を除く）、およびＳ：０．００５５％以下（０％を除く）をさらに含むことができる。 The grain-oriented electrical steel sheet according to an embodiment of the present invention can satisfy the following formula 1.
[Equation 1]
0.5 ≤ ([Ba] + [Y]) / ([B] * 10) ≤ 3
(However, in Formula 1, [Ba], [Y], and [B] indicate the contents (% by weight) of Ba, Y, and B, respectively.)
C: 0.005% or less (excluding 0%), Al: 0.005% or less (excluding 0%), N: 0.0055% or less (excluding 0%), and S: 0.0055% or less (Excluding 0%) can be further included.

Ｍｎ：０．０１％〜０．５％をさらに含むことができる。
２ｍｍ以上の粒径を有する結晶粒の平均粒径は、１０ｍｍ以上であること位が好ましい。
結晶粒界に偏析したＢ並びに、ＢａまたはＹを含むことができる。 Mn: 0.01% to 0.5% can be further contained.
The average particle size of the crystal grains having a particle size of 2 mm or more is preferably 10 mm or more.
B segregated at the grain boundaries and Ba or Y can be included.

本発明の一実施例による方向性電磁鋼板の製造方法は、重量％で、Ｓｉ：１．０〜７．０％、Ｂ：０．００１〜０．１％並びに、ＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％含み、残部はＦｅおよびその他の不可避不純物を含むスラブを加熱する段階、スラブを熱間圧延して熱延板を製造する段階、熱延板を冷間圧延して冷延板を製造する段階、冷延板を１次再結晶焼鈍する段階、および、１次再結晶焼鈍が完了した冷延板を２次再結晶焼鈍する段階、を含むことを特徴とする In the method for producing a directional electromagnetic steel sheet according to an embodiment of the present invention, Si: 1.0 to 7.0%, B: 0.001 to 0.1%, and Ba and Y are used alone or in% by weight, respectively. The total amount contains 0.005% by weight to 0.5% by weight, and the balance is the stage of heating a slab containing Fe and other unavoidable impurities, the stage of hot rolling the slab to produce a hot-rolled plate, and the stage of hot-rolled plate. Includes a step of cold rolling to produce a cold rolled plate, a step of primary recrystallization annealing of the cold rolled plate, and a step of secondary recrystallization annealing of the cold rolled plate for which the primary recrystallization annealing has been completed. Characterized by

スラブは、下記式１を満足することができる。
［式１］
０．５≦（［Ｂａ］＋［Ｙ］）／（［Ｂ］＊１０）≦３
（ただし、式１中、［Ｂａ］、［Ｙ］、［Ｂ］は、それぞれＢａ、Ｙ、Ｂの含有量（重量％）を示す。）
スラブは、Ｃ：０．００１〜０．１％、Ａｌ：０．０１％以下（０％を除く）、Ｎ：０．００５５％以下（０％を除く）、およびＳ：０．００５５％以下（０％を除く）をさらに含むことができる。 The slab can satisfy the following equation 1.
[Equation 1]
0.5 ≤ ([Ba] + [Y]) / ([B] * 10) ≤ 3
(However, in Formula 1, [Ba], [Y], and [B] indicate the contents (% by weight) of Ba, Y, and B, respectively.)
The slab has C: 0.001 to 0.1%, Al: 0.01% or less (excluding 0%), N: 0.0055% or less (excluding 0%), and S: 0.0055% or less. (Excluding 0%) can be further included.

スラブは、Ｍｎ：０．０１％〜０．５％をさらに含むことができる。
スラブを加熱する段階で、１０００〜１２８０℃に加熱することがよい。
熱延板を冷間圧延して冷延板を製造する段階で、最終圧下率が８０％以上になることが好ましい。
２次再結晶焼鈍する段階は、昇温段階および均熱段階を含み、均熱段階の温度は、９００〜１２５０℃になることがよい。 The slab can further contain Mn: 0.01% to 0.5%.
At the stage of heating the slab, it is preferable to heat it to 1000 to 1280 ° C.
At the stage of cold-rolling the hot-rolled plate to produce the cold-rolled plate, the final reduction ratio is preferably 80% or more.
The secondary recrystallization annealing step includes a temperature raising step and a heat soaking step, and the temperature of the heat soaking step is preferably 900 to 1250 ° C.

本発明の一実施例による方向性電磁鋼板は、ゴス結晶粒を安定的に形成させることによって、磁気的特性に優れている。
また、結晶粒成長抑制剤としてＡｌＮおよびＭｎＳを使用しないので、１３００℃以上の高温にスラブを加熱する必要がない。
さらに、結晶粒界強化効果によって、強冷間圧延下でも粒界クラックの発生が低減され、生産性の向上および製造費用が節減される。 The grain-oriented electrical steel sheet according to an embodiment of the present invention is excellent in magnetic properties by stably forming Goth crystal grains.
Moreover, since AlN and MnS are not used as the crystal grain growth inhibitor, it is not necessary to heat the slab to a high temperature of 1300 ° C. or higher.
Further, due to the effect of strengthening the grain boundaries, the occurrence of grain boundary cracks is reduced even under strong cold rolling, and the productivity is improved and the manufacturing cost is reduced.

試料番号２番の発明材の製造過程における冷延鋼板の写真である。It is a photograph of a cold-rolled steel sheet in the manufacturing process of the invention material of sample number 2. 試料番号１番の比較材の製造過程における冷延鋼板の写真である。It is a photograph of a cold-rolled steel sheet in the manufacturing process of the comparative material of sample number 1.

第１、第２および第３などの用語は、多様な部分、成分、領域、層および／またはセクションを説明するために使用されるが、これらに限定されない。これらの用語は、ある部分、成分、領域、層またはセクションを、他の部分、成分、領域、層またはセクションと区別するためにのみ使用される。したがって、以下に述べる第１部分、成分、領域、層またはセクションは、本発明の範囲を逸脱しない範囲内で第２部分、成分、領域、層またはセクションとして言及される。
ここで使用される専門用語は、単に特定の実施例を言及するためのものであり、本発明を限定することを意図しない。ここで使用される単数形態は、文言がこれと明確に反対の意味を示さない限り、複数形態も含む。明細書で使用される「含む」の意味は、特定の特性、領域、整数、段階、動作、要素および／または成分を具体化し、他の特性、領域、整数、段階、動作、要素および／または成分の存在や付加を除外させるわけではない。 Terms such as first, second and third are used to describe, but are not limited to, various parts, components, regions, layers and / or sections. These terms are used only to distinguish one part, component, area, layer or section from another part, component, area, layer or section. Therefore, the first part, component, region, layer or section described below is referred to as the second part, component, region, layer or section within the scope of the present invention.
The terminology used herein is merely to refer to a particular embodiment and is not intended to limit the invention. The singular form used herein also includes multiple forms, unless the wording has a clear opposite meaning. As used herein, the meaning of "contains" embodies a particular property, region, integer, stage, behavior, element and / or component, and other characteristics, region, integer, stage, behavior, element and / or. It does not exclude the presence or addition of ingredients.

ある部分が他の部分の「上に」あると言及する場合、これは、まさに他の部分の上にあるか、その間に他の部分が伴ってもよい。対照的にある部分が他の部分の「真上に」あると言及する場合、その間に他の部分が介在しない。
別途に定義しないものの、ここに使用される技術用語および科学用語を含むすべての用語は、本発明の属する技術分野における通常の知識を有する者が一般に理解する意味と同じ意味を有する。通常使用される辞書に定義された用語は、関連技術文献と現在開示された内容に符合する意味を有するものとして追加解釈され、定義されない限り、理想的または非常に公式的な意味で解釈されない。
また、特に言及しない限り、％は、重量％を意味し、１ｐｐｍは、０．０００１重量％である。 When referring to one part being "above" another part, this may be just above the other part, or with another part in between. In contrast, when one mentions that one part is "directly above" another, there is no other part in between.
Although not defined separately, all terms, including the technical and scientific terms used herein, have the same meaning as generally understood by those with ordinary knowledge in the technical field to which the present invention belongs. Terms defined in commonly used dictionaries are additionally interpreted as having a meaning consistent with the relevant technical literature and currently disclosed content, and are not interpreted in an ideal or very formal sense unless defined.
Further, unless otherwise specified,% means% by weight, and 1 ppm is 0.0001% by weight.

以下、本発明の実施例について、本発明の属する技術分野における通常の知識を有する者が容易に実施できるように詳細に説明する。しかし、本発明は種々の異なる形態で実現可能であり、ここで説明する実施例に限定されない。
既存の方向性電磁鋼板技術では、結晶粒成長抑制剤としてＡｌＮ、ＭｎＳなどのような析出物を使用しており、すべての工程が析出物の分布を厳格に制御し、２次再結晶された鋼板内に残留した析出物が除去されるようにするための条件によって工程条件が極めて限られていた。
反面、本発明の一実施例では、結晶粒成長抑制剤としてＡｌＮ、ＭｎＳなどのような析出物を使用しない。本発明の一実施例では、Ｂ並びに、ＢａまたはＹを結晶粒成長抑制剤として使用することによって、Ｇｏｓｓ結晶粒の分率を増加させ、磁性に優れた電磁鋼板を得ることができる。 Hereinafter, examples of the present invention will be described in detail so that a person having ordinary knowledge in the technical field to which the present invention belongs can easily carry out the examples. However, the present invention is feasible in a variety of different forms and is not limited to the examples described herein.
In the existing directional electromagnetic steel sheet technology, precipitates such as AlN and MnS are used as the crystal grain growth inhibitor, and all the steps strictly control the distribution of the precipitates and secondary recrystallization is performed. The process conditions were extremely limited by the conditions for removing the precipitates remaining in the steel sheet.
On the other hand, in one embodiment of the present invention, precipitates such as AlN and MnS are not used as the crystal grain growth inhibitor. In one embodiment of the present invention, by using B and Ba or Y as a crystal grain growth inhibitor, the fraction of Goss crystal grains can be increased and an electromagnetic steel sheet having excellent magnetism can be obtained.

本発明の一実施例による方向性電磁鋼板は、重量％で、Ｓｉ：１．０〜７．０％、Ｍｎ：０．０１％〜０．５％、Ｂ：０．００１〜０．１％並びに、ＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％含み、残部はＦｅおよびその他の不可避不純物を含む。
以下、各成分について具体的に説明する。 The grain-oriented electrical steel sheet according to an embodiment of the present invention is Si: 1.0 to 7.0%, Mn: 0.01% to 0.5%, B: 0.001 to 0.1% in weight%. In addition, Ba and Y are contained alone or in a combined amount of 0.005% by weight to 0.5% by weight, and the balance contains Fe and other unavoidable impurities.
Hereinafter, each component will be specifically described.

バリウム（Ｂａ）およびイットリウム（Ｙ）は、本発明の一実施例において、結晶粒成長抑制剤として作用し、２次再結晶焼鈍時、ゴス結晶粒以外の他の方位の結晶粒が成長するのを抑制して電磁鋼板の磁性を向上させる。ＢａおよびＹは、それぞれ単独で添加されるか、複合添加されてもよい。ＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％含むことができる。つまり、ＢａまたはＹがそれぞれ単独で添加される場合、ＢａまたはＹの含有量がそれぞれ０．００５重量％〜０．５重量％になってもよく、ＢａおよびＹが同時に添加される場合、ＢａおよびＹの含有量の合計が（つまり、合量が）０．００５重量％〜０．５重量％になってもよい。ＢａまたはＹまたはその合量が少なすぎると、十分な抑制力を発揮しにくく、ＢａまたはＹまたはその合量が多すぎると、鋼板の脆性が増加して、圧延時にクラックが発生することがある。 In one embodiment of the present invention, barium (Ba) and yttrium (Y) act as crystal grain growth inhibitors, and during secondary recrystallization annealing, crystal grains in directions other than Goth crystal grains grow. To improve the magnetism of the electromagnetic steel sheet. Ba and Y may be added individually or in combination. Ba and Y can be contained alone or in a combined amount of 0.005% by weight to 0.5% by weight, respectively. That is, when Ba or Y is added alone, the content of Ba or Y may be 0.005% by weight to 0.5% by weight, respectively, and when Ba and Y are added at the same time, Ba. And the total content of Y may be between 0.005% and 0.5% by weight (ie, the total amount). If the amount of Ba or Y or the total amount thereof is too small, it is difficult to exert a sufficient restraining force, and if the amount of Ba or Y or the total amount thereof is too large, the brittleness of the steel sheet increases and cracks may occur during rolling. ..

ホウ素（Ｂ、ボロン）は、粒界に偏析して粒界結合力を強化するので、圧延時のクラック発生および圧延回数を低減する役割を果たす。また、鋼中の窒素と反応してＢＮ析出物を一部形成するが、ＢＮは、高温安定性に優れていて、前述したＢａおよびＹと共に結晶粒成長を抑制する補助インヒビターの作用が可能である。Ｂの含有量は、０．００１〜０．１重量％になってもよい。Ｂが過度に少なく含まれると、ＢａおよびＹによる粒界脆性を緩和させるのに不足しうる。Ｂが過度に多く含まれると、ＢａおよびＹの粒界偏析を抑制し、高温焼鈍過程で介在物を多数形成して磁気特性が低下しうる。
Ｂは、ＢａおよびＹとの関係において下記式１を満足することができる。
［式１］
０．５≦（［Ｂａ］＋［Ｙ］）／（［Ｂ］＊１０）≦３
（ただし、式１中、［Ｂａ］、［Ｙ］、［Ｂ］は、それぞれＢａ、Ｙ、Ｂの含有量（重量％）を示す。）
式１の値が０．５未満の場合、ＢａおよびＹの粒界偏析を抑制し、高温焼鈍過程で介在物を多数形成して磁気特性が低下しうる。式１の値が３超過の場合、ＢａおよびＹによる粒界脆性を緩和させるのに不足しうる。 Boron (B, boron) segregates at the grain boundaries and strengthens the grain boundary bonding force, so that it plays a role of reducing crack generation during rolling and the number of rolling times. In addition, it reacts with nitrogen in steel to form a part of BN precipitate, but BN is excellent in high temperature stability and can act as an auxiliary inhibitor that suppresses crystal grain growth together with Ba and Y described above. is there. The content of B may be 0.001 to 0.1% by weight. If B is contained in an excessively small amount, it may be insufficient to alleviate the intergranular brittleness due to Ba and Y. If B is contained in an excessively large amount, the grain boundary segregation of Ba and Y can be suppressed, and a large number of inclusions can be formed in the high temperature annealing process to deteriorate the magnetic properties.
B can satisfy the following equation 1 in relation to Ba and Y.
[Equation 1]
0.5 ≤ ([Ba] + [Y]) / ([B] * 10) ≤ 3
(However, in Formula 1, [Ba], [Y], and [B] indicate the contents (% by weight) of Ba, Y, and B, respectively.)
When the value of Equation 1 is less than 0.5, the grain boundary segregation of Ba and Y can be suppressed, and a large number of inclusions can be formed in the high temperature annealing process to deteriorate the magnetic properties. If the value of Equation 1 exceeds 3, it may be insufficient to alleviate the intergranular brittleness due to Ba and Y.

シリコン（Ｓｉ）は、素材の比抵抗を増加させて鉄損を低くする役割を果たす。スラブおよび電磁鋼板においてＳｉ含有量が１．０重量％未満の場合、比抵抗が減少して鉄損特性が低下しうる。逆に、方向性電磁鋼板においてＳｉ含有量が７重量％を超える場合、変圧器の製造時に加工が難しいので、方向性電磁鋼板におけるＳｉ含有量は、７重量％以下であるのが良い。
炭素（Ｃ）は、オーステナイト安定化元素であって、０．００１重量％以上スラブ中に添加されて、連鋳過程で発生する粗大な柱状組織を微細化し、Ｓのスラブ中心偏析を抑制することができる。また、冷間圧延中に鋼板の加工硬化を促進して、鋼板内に｛１１０｝＜００１＞方位の２次再結晶の核生成を促進したりすることができる。しかし、０．１％を超えると、熱延中にエッジ−クラック（ｅｄｇｅ−ｃｒａｃｋ）が発生することがある。ただし、電磁鋼板の製造時に脱炭焼鈍を経るようになり、脱炭焼鈍後の最終電磁鋼板内のＣ含有量は、０．００５重量％以下であるのが良い。より具体的には０．００３重量％以下である。 Silicon (Si) plays a role of increasing the specific resistance of the material and lowering the iron loss. If the Si content of the slab and the electrical steel sheet is less than 1.0% by weight, the specific resistance may decrease and the iron loss characteristics may decrease. On the contrary, when the Si content of the grain-oriented electrical steel sheet exceeds 7% by weight, it is difficult to process it at the time of manufacturing the transformer. Therefore, the Si content of the grain-oriented electrical steel sheet is preferably 7% by weight or less.
Carbon (C) is an austenite stabilizing element, which is added to 0.001% by weight or more in the slab to refine the coarse columnar structure generated in the continuous casting process and suppress the segregation of S in the slab center. Can be done. Further, it is possible to promote work hardening of the steel sheet during cold rolling to promote nucleation of secondary recrystallization in the {110} <001> orientation in the steel sheet. However, if it exceeds 0.1%, edge-cracks may occur during hot spreading. However, the electrical steel sheet undergoes decarburization annealing during production, and the C content in the final electrical steel sheet after decarburization annealing is preferably 0.005% by weight or less. More specifically, it is 0.003% by weight or less.

本発明の一実施例において、ＡｌＮ、ＭｎＳなどの析出物を結晶粒成長抑制剤として使用しないので、アルミニウム（Ａｌ）、窒素（Ｎ）、硫黄（Ｓ）など一般的な方向性電磁鋼板で必須として使用される元素は、不純物範囲で管理される。つまり、不可避にＡｌ、Ｎ、Ｓなどをさらに含む場合、Ａｌを０．００５重量％以下、Ｓを０．００５５重量％以下、およびＮを０．００５５重量％以下でさらに含んでもよい。
本発明の一実施例では、ＡｌＮを結晶粒成長抑制剤として使用しなくてよいので、アルミニウム（Ａｌ）含有量を積極的に抑制することができる。したがって、本発明の一実施例では、方向性電磁鋼板内にＡｌは添加されなかったり、０．００５重量％以下に制御することができる。また、スラブでは、製造工程過程でＡｌが除去されるので、Ａｌを０．０１重量％以下で含むことができる。 In one embodiment of the present invention, since precipitates such as AlN and MnS are not used as a grain growth inhibitor, they are essential for general directional electromagnetic steel sheets such as aluminum (Al), nitrogen (N) and sulfur (S). The elements used as are controlled in the impurity range. That is, when Al, N, S and the like are inevitably further contained, Al may be further contained in 0.005% by weight or less, S in 0.0055% by weight or less, and N in 0.0055% by weight or less.
In one embodiment of the present invention, since AlN does not have to be used as a crystal grain growth inhibitor, the aluminum (Al) content can be positively suppressed. Therefore, in one embodiment of the present invention, Al is not added to the grain-oriented electrical steel sheet, or it can be controlled to 0.005% by weight or less. Further, in the slab, since Al is removed in the manufacturing process, Al can be contained in an amount of 0.01% by weight or less.

窒素（Ｎ）は、ＡｌＮ、（Ａｌ、Ｍｎ）Ｎ、（Ａｌ、Ｓｉ、Ｍｎ）Ｎ、Ｓｉ３Ｎ４、ＢＮなどの析出物を形成するので、本発明の一実施例では、Ｎは添加されなかったり、０．００５５重量％以下に制御することができる。より具体的には０．００３０重量％以下であってもよい。本発明の一実施例では、浸窒工程を省略できるので、スラブ内のＮ含有量と最終電磁鋼板内のＮ含有量とが実質的に同一であり得る。
硫黄（Ｓ）は、熱間圧延時、固溶温度が高くて偏析が激しい元素であるので、本発明の一実施例では、添加されなかったり、０．００５５重量％以下に制御することができる。より具体的には０．００３５重量％以下であってもよい。 Nitrogen (N) forms precipitates such as AlN, (Al, Mn) N, (Al, Si, Mn) N, Si3N4, and BN. Therefore, in one embodiment of the present invention, N is not added. , 0.0055% by weight or less can be controlled. More specifically, it may be 0.0030% by weight or less. In one embodiment of the present invention, since the nitrification step can be omitted, the N content in the slab and the N content in the final magnetic steel sheet can be substantially the same.
Sulfur (S) is an element that has a high solid solution temperature and severe segregation during hot rolling. Therefore, in one embodiment of the present invention, sulfur (S) may not be added or may be controlled to 0.0055% by weight or less. .. More specifically, it may be 0.0035% by weight or less.

本発明の一実施例では、ＭｎＳを結晶粒成長抑制剤として使用しないので、マンガン（Ｍｎ）を添加しなくてよい。ただし、Ｍｎは、比抵抗元素であって磁性を改善する効果があるので、スラブおよび電磁鋼板に任意成分として、追加的にさらに含まれてもよい。Ｍｎが追加的に含まれる場合、Ｍｎの含有量は、０．０１重量％以上であってもよい。しかし、０．５重量％を超える場合、２次再結晶後に相変態を起こして磁性が劣化することがある。本発明の一実施例において、追加元素をさらに含む場合、残部の鉄（Ｆｅ）を代替して添加されることが理解される。
また、その他の不可避不純物として、Ｔｉ、Ｍｇ、Ｃａのような成分は、鋼中で酸素と反応して酸化物を形成して、介在物として最終製品の磁区移動に妨害を与えて磁性劣化の原因になりうるので、強力抑制することが必要である。したがって、これらを不可避に含有する場合、それぞれの成分ごとに０．００５重量％以下で管理することができる。 In one embodiment of the present invention, since MnS is not used as a crystal grain growth inhibitor, manganese (Mn) does not have to be added. However, since Mn is a resistivity element and has an effect of improving magnetism, it may be additionally contained as an optional component in the slab and the electromagnetic steel sheet. When Mn is additionally contained, the content of Mn may be 0.01% by weight or more. However, if it exceeds 0.5% by weight, phase transformation may occur after secondary recrystallization and the magnetism may deteriorate. In one embodiment of the present invention, it is understood that when additional elements are further included, the remaining iron (Fe) is added in place of it.
In addition, as other unavoidable impurities, components such as Ti, Mg, and Ca react with oxygen in steel to form oxides, which interfere with the movement of magnetic domains in the final product as inclusions and cause magnetic deterioration. Since it can be a cause, it is necessary to strongly suppress it. Therefore, when these are unavoidably contained, each component can be controlled at 0.005% by weight or less.

本発明の一実施例による方向性電磁鋼板は、２ｍｍ以上の粒径を有する結晶粒の平均粒径が１０ｍｍ以上になる。２ｍｍ以上の粒径を有する結晶粒の平均粒径が１０ｍｍ未満の場合、結晶粒が十分に成長せずに磁性が低下しうる。本発明の一実施例において、結晶粒の粒径とは、円に相当する結晶粒に対する直径の長さを意味する。
本発明の一実施例による方向性電磁鋼板は、ゴス結晶粒を安定的に形成させることによって、磁気的特性に優れている。具体的には、本発明の一実施例による方向性電磁鋼板は、８００Ａ／ｍの磁場で測定した磁束密度のＢ８が１．８８Ｔ以上であってもよい。 In the grain-oriented electrical steel sheet according to an embodiment of the present invention, the average particle size of crystal grains having a particle size of 2 mm or more is 10 mm or more. When the average particle size of the crystal grains having a particle size of 2 mm or more is less than 10 mm, the crystal grains do not grow sufficiently and the magnetism may decrease. In one embodiment of the present invention, the grain size of the crystal grains means the length of the diameter with respect to the crystal grains corresponding to the circle.
The grain-oriented electrical steel sheet according to an embodiment of the present invention is excellent in magnetic properties by stably forming Goth crystal grains. Specifically, the grain-oriented electrical steel sheet according to the embodiment of the present invention may have a magnetic flux density of B8 of 1.88 T or more measured in a magnetic field of 800 A / m.

本発明の一実施例による方向性電磁鋼板の製造方法は、重量％で、Ｓｉ：１．０〜７．０％、Ｂ：０．００１〜０．１％並びに、ＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％含み、残部はＦｅおよびその他の不可避不純物を含むスラブを加熱する段階、スラブを熱間圧延して熱延板を製造する段階、熱延板を冷間圧延して冷延板を製造する段階、冷延板を１次再結晶焼鈍する段階、および、１次再結晶焼鈍が完了した冷延板を２次再結晶焼鈍する段階、を含む。 In the method for producing a directional electromagnetic steel sheet according to an embodiment of the present invention, Si: 1.0 to 7.0%, B: 0.001 to 0.1%, and Ba and Y are used alone or in% by weight, respectively. The total amount contains 0.005% by weight to 0.5% by weight, and the balance is the stage of heating the slab containing Fe and other unavoidable impurities, the stage of hot rolling the slab to produce a hot-rolled plate, and the hot-rolled plate. Includes a step of cold rolling to produce a cold rolled plate, a step of primary recrystallization annealing of the cold rolled plate, and a step of secondary recrystallization annealing of the cold rolled plate for which the primary recrystallization annealing has been completed. ..

以下、各段階ごとに方向性電磁鋼板の製造方法を具体的に説明する。
まず、スラブを加熱する。
スラブの組成については、電磁鋼板の組成に関連して具体的に説明したので、重複する説明は省略する。
スラブの加熱温度は制限されないが、スラブを１２８０℃以下の温度に加熱すると、スラブの柱状晶組織が粗大に成長するのを防止して、熱間圧延工程で板のクラックが発生するのを防止することができる。したがって、スラブの加熱温度は、１０００℃〜１２８０℃であってもよい。特に、本発明の一実施例では、結晶粒成長抑制剤としてＡｌＮおよびＭｎＳを使用しないので、１３００℃以上の高温にスラブを加熱する必要がない。 Hereinafter, the method for manufacturing the grain-oriented electrical steel sheet will be specifically described for each step.
First, the slab is heated.
Since the composition of the slab has been specifically described in relation to the composition of the electrical steel sheet, duplicate description will be omitted.
The heating temperature of the slab is not limited, but heating the slab to a temperature of 1280 ° C or lower prevents the columnar crystal structure of the slab from growing coarsely and prevents cracks in the plate during the hot rolling process. can do. Therefore, the heating temperature of the slab may be 1000 ° C. to 1280 ° C. In particular, in one embodiment of the present invention, since AlN and MnS are not used as the crystal grain growth inhibitors, it is not necessary to heat the slab to a high temperature of 1300 ° C. or higher.

次に、スラブを熱間圧延して熱延板を製造する。熱間圧延温度は制限されず、一実施例として９５０℃以下で熱延を終了することができる。この後、水冷して６００℃以下で巻取ることができる。
次に、必要に応じて、熱延板を熱延板焼鈍することができる。熱延板焼鈍を実施する場合、熱延組織を均一にするために、９００℃以上の温度に加熱し、均熱した後、冷却することができる。
次に、熱延板を冷間圧延して冷延板を製造する。冷間圧延は、リバース（Ｒｅｖｅｒｓｅ）圧延機あるいはタンデム（Ｔａｎｄｅｍ）圧延機を用いて、１回の冷間圧延、複数回の冷間圧延、または中間焼鈍を含む複数回の冷間圧延法で０．１ｍｍ〜０．５ｍｍの厚さの冷延板を製造することができる。
また、冷間圧延中に鋼板の温度を１００℃以上に維持する温間圧延を実施できる。
Next, the slab is hot-rolled to produce a hot-rolled plate. The hot rolling temperature is not limited, and as an example, hot rolling can be completed at 950 ° C. or lower. After that, it can be cooled with water and wound at 600 ° C. or lower.
Next, if necessary, the hot-rolled plate can be annealed. When the hot-rolled plate is annealed, it can be heated to a temperature of 900 ° C. or higher, equalized, and then cooled in order to make the hot-rolled structure uniform.
Next, the hot-rolled plate is cold-rolled to produce a cold-rolled plate. Cold rolling, using a reverse (Reverse) mill or a tandem (Tandem) rolling mill, one of the cold rolling, a plurality of times of cold rolling, or multiple cold rolling method including intermediate annealing 0 A cold rolled plate having a thickness of 1 mm to 0.5 mm can be produced.
In addition, warm rolling can be performed in which the temperature of the steel sheet is maintained at 100 ° C. or higher during cold rolling.

さらに、冷間圧延による最終圧下率は、８０％以上になってもよい。本発明の一実施例では、前述のように、スラブ成分内にＢを特定の含有量含むことによって、粒界に偏析して粒界結合力を強化するので、圧延時のクラック発生および圧延回数を低減することができ、最終圧下率を高めることができる。
次に、冷間圧延された冷延板を１次再結晶焼鈍する。１次再結晶焼鈍段階でゴス結晶粒の核が生成される１次再結晶が起こる。１次再結晶焼鈍段階で冷延板の脱炭が行われる。脱炭のために、８００℃〜９００℃の温度で焼鈍することができる。また、雰囲気は、水素および窒素の混合ガス雰囲気であってもよい。さらに、脱炭が完了すると、冷延板内の炭素含有量は、０．００５重量％以下になってもよい。本発明の一実施例では、ＡｌＮ結晶粒成長抑制剤を使用しないので、窒化工程を省略することができる。 Further, the final rolling reduction by cold rolling may be 80% or more. In one embodiment of the present invention, as described above, by including B in the slab component at a specific content, segregation occurs at the grain boundaries and the grain boundary bonding force is strengthened, so that cracks occur during rolling and the number of times of rolling. Can be reduced and the final rolling reduction rate can be increased.
Next, the cold-rolled cold-rolled sheet is first recrystallized and annealed. Primary recrystallization In the annealing step, primary recrystallization occurs in which nuclei of Goth grains are generated. The cold rolled plate is decarburized at the primary recrystallization annealing stage. For decarburization, it can be annealed at a temperature of 800 ° C to 900 ° C. Further, the atmosphere may be a mixed gas atmosphere of hydrogen and nitrogen. Further, when the decarburization is completed, the carbon content in the cold rolled plate may be 0.005% by weight or less. In one embodiment of the present invention, since the AlN crystal grain growth inhibitor is not used, the nitriding step can be omitted.

次に、１次再結晶焼鈍が完了した冷延板を２次再結晶焼鈍する。この時、１次再結晶焼鈍が完了した冷延板に焼鈍分離剤を塗布した後、２次再結晶焼鈍することができる。この時、焼鈍分離剤は特に制限せず、ＭｇＯを主成分として含む焼鈍分離剤を使用することができる。
２次再結晶焼鈍する段階は、昇温段階および均熱段階を含む。昇温段階は、１次再結晶焼鈍が完了した冷延板を均熱段階の温度まで昇温する段階である。均熱段階の温度は、９００℃〜１２５０℃であってもよい。９００℃未満であれば、ゴス結晶粒が十分に成長せずに磁性が低下し、１２５０℃超過時、結晶粒が粗大に成長して電磁鋼板の特性が低下しうる。昇温段階は水素および窒素の混合ガス雰囲気で、均熱段階は水素雰囲気で行われる。 Next, the cold-rolled plate for which the primary recrystallization annealing has been completed is subjected to the secondary recrystallization annealing. At this time, after applying the annealing separator to the cold-rolled plate for which the primary recrystallization annealing has been completed, the secondary recrystallization annealing can be performed. At this time, the annealing separator is not particularly limited, and an annealing separator containing MgO as a main component can be used.
The secondary recrystallization annealing step includes a heating step and a soaking step. The temperature raising step is a step of raising the temperature of the cold rolled sheet for which the primary recrystallization annealing has been completed to the temperature of the soaking step. The temperature of the soaking step may be 900 ° C to 1250 ° C. If it is less than 900 ° C., the Goth crystal grains do not grow sufficiently and the magnetism decreases, and if it exceeds 1250 ° C., the crystal grains grow coarsely and the characteristics of the electrical steel sheet may deteriorate. The heating step is performed in a mixed gas atmosphere of hydrogen and nitrogen, and the soaking step is performed in a hydrogen atmosphere.

本発明の一実施例による方向性電磁鋼板の製造方法では、ＡｌＮ、ＭｎＳの結晶粒成長抑制剤を使用しないので、２次再結晶焼鈍が完了した後、純化焼鈍工程を省略することができる。従来のＭｎＳ、ＡｌＮを結晶粒成長抑制剤として使用する方向性電磁鋼板の製造方法では、ＡｌＮおよびＭｎＳのような析出物を除去するための高温の純化焼鈍が必要であったが、本発明の一実施例による方向性電磁鋼板の製造方法では、純化焼鈍工程を必要としない。
この後、必要に応じて、方向性電磁鋼板の表面に絶縁被膜を形成したり、磁区微細化処理を行うことができる。本発明の一実施例において、方向性電磁鋼板の合金成分は、絶縁被膜などのコーティング層を除いた素地鋼板を意味する。
以下、実施例を通じて本発明をより詳細に説明する。しかし、このような実施例は単に本発明を例示するためのものであり、本発明がこれに限定されるものではない。 Since the method for producing grain grain growth inhibitor of AlN and MnS is not used in the method for producing grain grain growth inhibitor according to the embodiment of the present invention, the purification annealing step can be omitted after the secondary recrystallization annealing is completed. In the conventional method for producing grain-oriented electrical steel sheets using MnS and AlN as grain growth inhibitors, high-temperature purification annealing for removing precipitates such as AlN and MnS was required. The method for manufacturing grain-oriented electrical steel sheets according to one embodiment does not require a purification annealing step.
After that, if necessary, an insulating film can be formed on the surface of the grain-oriented electrical steel sheet, or a magnetic domain miniaturization treatment can be performed. In one embodiment of the present invention, the alloy component of the grain-oriented electrical steel sheet means a base steel sheet excluding a coating layer such as an insulating film.
Hereinafter, the present invention will be described in more detail through examples. However, such examples are merely for exemplifying the present invention, and the present invention is not limited thereto.

実施例１
重量％で、Ｓｉ：３．２％、Ｃ：０．０５％、Ｍｎ：０．０６％、Ｓ：０．００４８％、Ｎ：０．００３２％、および、Ａｌ：０．００５％を含み、バリウム（Ｂａ）、イットリウム（Ｙ）、およびボロン（Ｂ）を下記表１のように含有し、残部Ｆｅとその他不可避に混入する不純物からなるスラブを準備した。
スラブを１１５０℃の温度に９０分間加熱した後、熱間圧延して２．６ｍｍの厚さの熱延板を製造した。この熱延板を１０５０℃以上の温度に加熱した後、９１０℃で９０秒間維持し、水冷した後、酸洗した。次に、リバース（Ｒｅｖｅｒｓｅ）圧延機を用いて、計７回のパスを経て０．３０ｍｍの厚さまで冷間圧延した。各パスあたりの圧下率は、試験条件ごとに同一に適用した。冷間圧延された鋼板は、炉中で昇温した後、水素：５０体積％および窒素：５０体積％の混合ガス雰囲気、および、焼鈍温度８５０℃で１２０秒間維持して炭素濃度０．００２重量％まで脱炭と共に１次再結晶焼鈍を行った。この後、ＭｇＯを塗布した後、コイル状に巻取って２次再結晶焼鈍した。２次再結晶焼鈍は、窒素：２５体積％および水素：７５体積％の混合ガス雰囲気で１２００℃まで昇温し、１２００℃到達後には水素：１００体積％のガス雰囲気で２０時間維持後、炉冷した。 Example 1
By weight%, it contains Si: 3.2%, C: 0.05%, Mn: 0.06%, S: 0.0048%, N: 0.0032%, and Al: 0.005%. A slab containing barium (Ba), yttrium (Y), and boron (B) as shown in Table 1 below, and consisting of the balance Fe and other unavoidably mixed impurities was prepared.
The slab was heated to a temperature of 1150 ° C. for 90 minutes and then hot-rolled to produce a hot-rolled plate having a thickness of 2.6 mm. The hot-rolled plate was heated to a temperature of 1050 ° C. or higher, maintained at 910 ° C. for 90 seconds, cooled with water, and then pickled. Next, using a Reverse rolling mill, cold rolling was performed to a thickness of 0.30 mm through a total of 7 passes. The reduction rate per pass was applied the same for each test condition. After the temperature of the cold-rolled steel sheet is raised in the furnace, it is maintained at a mixed gas atmosphere of hydrogen: 50% by volume and nitrogen: 50% by volume and an annealing temperature of 850 ° C. for 120 seconds to have a carbon concentration of 0.002% by volume. Primary recrystallization annealing was performed along with decarburization to%. Then, after applying MgO, it was wound into a coil and annealed for secondary recrystallization. In the secondary recrystallization annealing, the temperature is raised to 1200 ° C. in a mixed gas atmosphere of nitrogen: 25% by volume and hydrogen: 75% by volume, and after reaching 1200 ° C., maintained in a gas atmosphere of hydrogen: 100% by volume for 20 hours, and then the furnace. It was chilled.

最終的に得られた鋼板を表面洗浄後、ｓｉｎｇｌｅ ｓｈｅｅｔ測定法を利用して、磁場の強さを８００Ａ／ｍの条件で磁束密度を測定した。
After surface cleaning of the finally obtained steel sheet, the magnetic flux density was measured under the condition of a magnetic field strength of 800 A / m using a single sheet measurement method.

表１から確認できるように、ＢａおよびＹの含有量に応じてＢの含有量が本発明の範囲内で制御された場合に、圧延クラックの発生がなく、比較材に比べて優れた磁性を得ることができた。
また、図１、および図２に、試料番号２番の発明材の製造工程中の冷延鋼板の写真、および試料番号１番の比較材の製造工程中の冷延鋼板の写真を示した。比較材の場合、圧延クラックが明確に現れることを確認できる。 As can be confirmed from Table 1, when the B content is controlled within the range of the present invention according to the Ba and Y contents, rolling cracks do not occur and the magnetism is superior to that of the comparative material. I was able to get it.
Further, FIGS. 1 and 2 show a photograph of a cold-rolled steel sheet during the manufacturing process of the invention material of Sample No. 2 and a photograph of the cold-rolled steel sheet during the manufacturing process of the comparative material of Sample No. 1. In the case of the comparative material, it can be confirmed that rolling cracks clearly appear.

実施例２
重量％で、Ｓｉ：３．２％、Ｃ：０．０４８％、Ｍｎ：０．１１％、Ｓ：０．００５１％、Ｎ：０．００２８％、および、Ａｌ：０．００８％を含み、バリウム（Ｂａ）、イットリウム（Ｙ）、およびボロン（Ｂ）を下記表２のように含有し、残部Ｆｅとその他不可避に混入する不純物からなるスラブを準備した。
スラブを１１５０℃の温度に９０分間加熱した後、熱間圧延して２．６ｍｍの厚さの熱延板を製造した。この熱延板を１０５０℃以上の温度に加熱した後、９１０℃で９０秒間維持し、水冷した後、酸洗した。次に、リバース（Ｒｅｖｅｒｓｅ）圧延機を用いて、計７回のパスを経て０．３０ｍｍの厚さまで冷間圧延した。各パスあたりの圧下率は、試験条件ごとに同一に適用した。冷間圧延された鋼板は、炉中で昇温した後、水素：５０体積％および窒素：５０体積％の混合ガス雰囲気、および、焼鈍温度８５０℃で１２０秒間維持して炭素濃度０．００３重量％まで脱炭と共に１次再結晶焼鈍を行った。この後、ＭｇＯを塗布した後、コイル状に巻取って２次再結晶焼鈍した。２次再結晶焼鈍は、窒素：２５体積％および水素：７５体積％の混合ガス雰囲気で１２００℃まで昇温し、１２００℃到達後には水素：１００体積％のガス雰囲気で２０時間維持後、炉冷した。 Example 2
By weight%, it contains Si: 3.2%, C: 0.048%, Mn: 0.11%, S: 0.0051%, N: 0.0028%, and Al: 0.008%. A slab containing barium (Ba), yttrium (Y), and boron (B) as shown in Table 2 below, and consisting of the balance Fe and other unavoidably mixed impurities was prepared.
The slab was heated to a temperature of 1150 ° C. for 90 minutes and then hot-rolled to produce a hot-rolled plate having a thickness of 2.6 mm. The hot-rolled plate was heated to a temperature of 1050 ° C. or higher, maintained at 910 ° C. for 90 seconds, cooled with water, and then pickled. Next, using a Reverse rolling mill, cold rolling was performed to a thickness of 0.30 mm through a total of 7 passes. The reduction rate per pass was applied the same for each test condition. After the temperature of the cold-rolled steel sheet is raised in the furnace, it is maintained at a mixed gas atmosphere of hydrogen: 50% by volume and nitrogen: 50% by volume and an annealing temperature of 850 ° C. for 120 seconds to have a carbon concentration of 0.003% by volume. Primary recrystallization annealing was performed along with decarburization to%. Then, after applying MgO, it was wound into a coil and annealed for secondary recrystallization. In the secondary recrystallization annealing, the temperature is raised to 1200 ° C. in a mixed gas atmosphere of nitrogen: 25% by volume and hydrogen: 75% by volume, and after reaching 1200 ° C., maintained in a gas atmosphere of hydrogen: 100% by volume for 20 hours, and then the furnace. It was chilled.

最終的に得られた鋼板を表面洗浄後、ｓｉｎｇｌｅ ｓｈｅｅｔ測定法を利用して、磁場の強さを８００Ａ／ｍの条件で磁束密度を測定した。また、結晶粒の粒径は６０℃に加熱された塩酸に５分間浸漬して表面のコーティング層を除去した後、面積に応じた平均値で計算した。
表２を参照すれば、本発明の一実施例による電磁鋼板において、２ｍｍ以上の粒径を有する結晶粒の平均粒径は１０ｍｍ以上となり、磁性に優れていることが明らかになった。 After surface cleaning of the finally obtained steel sheet, the magnetic flux density was measured under the condition of a magnetic field strength of 800 A / m using a single sheet measurement method. The grain size of the crystal grains was calculated by immersing in hydrochloric acid heated to 60 ° C. for 5 minutes to remove the coating layer on the surface, and then calculating the average value according to the area.
With reference to Table 2, in the electromagnetic steel sheet according to the embodiment of the present invention, the average particle size of the crystal grains having a particle size of 2 mm or more was 10 mm or more, and it was clarified that the magnetic steel sheet was excellent in magnetism.

本発明は、上記の実施例に限定されるものではなく、互いに異なる多様な形態で製造可能であり、本発明の属する技術分野における通常の知識を有する者は、本発明の技術的な思想や必須の特徴を変更することなく他の具体的な形態で実施可能であることを理解するであろう。そのため、以上に述べた実施例はあらゆる面で例示的なものであり、限定的ではないと理解しなければならない。 The present invention is not limited to the above-mentioned examples, and can be produced in various forms different from each other, and a person having ordinary knowledge in the technical field to which the present invention belongs may consider the technical idea of the present invention. You will understand that it can be implemented in other concrete forms without changing the essential features. Therefore, it should be understood that the above-described embodiments are exemplary in all respects and are not limiting.

Claims (9)

重量％で、Ｓｉ：１．０〜７．０％、Ｂ：０．００１〜０．１％、ＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％、Ｃ：０．００５％以下（０％を除く）、Ａｌ：０．００５％以下（０％を除く）、Ｎ：０．００５５％以下（０％を除く）、およびＳ：０．００５５％以下（０％を除く）含み、残部はＦｅおよびその他不可避に混入する不純物からなり、下記式１を満足することを特徴とする方向性電磁鋼板。
［式１］
０．５≦（［Ｂａ］＋［Ｙ］）／（［Ｂ］＊１０）≦３
（ただし、式１中、［Ｂａ］、［Ｙ］、［Ｂ］は、それぞれＢａ、Ｙ、Ｂの含有量（重量％）を示す。） By weight%, Si: 1.0 to 7.0%, B: 0.001 to 0.1 %, Ba and Y alone or in total, 0.005% by weight to 0.5% by weight , C: 0.005% or less (excluding 0%) , Al: 0.005% or less (excluding 0%), N: 0.0055% or less (excluding 0%), and S: 0.0055% or less (0) % excluding) wherein, the balance being impurities mixed in Fe and other unavoidable, oriented electrical steel sheet satisfies the following formula 1.
[Equation 1]
0.5 ≤ ([Ba] + [Y]) / ([B] * 10) ≤ 3
(However, in Formula 1, [Ba], [Y], and [B] indicate the contents (% by weight) of Ba, Y, and B, respectively.) Ｍｎ：０．０１％〜０．５％をさらに含むことを特徴とする請求項１に記載の方向性電磁鋼板。 The grain-oriented electrical steel sheet according to claim 1, further comprising Mn: 0.01% to 0.5%. ２ｍｍ以上の粒径を有する結晶粒の平均粒径は、１０ｍｍ以上であることを特徴とする請求項１または請求項２に記載の方向性電磁鋼板。 The grain-oriented electrical steel sheet according to claim 1 or 2, wherein the average particle size of the crystal grains having a particle size of 2 mm or more is 10 mm or more. 結晶粒界に偏析したＢ並びに、ＢａまたはＹを含むことを特徴とする請求項１乃至請求項３のいずれか一項に記載の方向性電磁鋼板。 The grain-oriented electrical steel sheet according to any one of claims 1 to 3 , which contains B segregated at the grain boundaries and Ba or Y. 重量％で、Ｓｉ：１．０〜７．０％、Ｂ：０．００１〜０．１％、ＢａおよびＹをそれぞれ単独または合量で０．００５重量％〜０．５重量％、Ｃ：０．００１〜０．１％、Ａｌ：０．０１％以下（０％を除く）、Ｎ：０．００５５％以下（０％を除く）、およびＳ：０．００５５％以下（０％を除く）含み、残部はＦｅおよびその他不可避に混入する不純物からなり、下記式１を満足する、スラブを加熱する段階；
前記スラブを熱間圧延して熱延板を製造する段階；
前記熱延板を冷間圧延して冷延板を製造する段階；
前記冷延板を１次再結晶焼鈍する段階；および；
前記１次再結晶焼鈍が完了した前記冷延板を２次再結晶焼鈍する段階；を含むことを特徴とする方向性電磁鋼板の製造方法。
［式１］
０．５≦（［Ｂａ］＋［Ｙ］）／（［Ｂ］＊１０）≦３
（ただし、式１中、［Ｂａ］、［Ｙ］、［Ｂ］は、それぞれＢａ、Ｙ、Ｂの含有量（重量％）を示す。） By weight%, Si: 1.0 to 7.0%, B: 0.001 to 0.1 %, Ba and Y alone or in total, 0.005% by weight to 0.5% by weight , C: 0.001 to 0.1%, Al: 0.01% or less (excluding 0%), N: 0.0055% or less (excluding 0%), and S: 0.0055% or less (excluding 0%) ) wherein, the balance being impurities mixed in Fe and other unavoidable, satisfies the following formula 1, heating the slab stage;
A stage in which the slab is hot-rolled to produce a hot-rolled plate;
A stage in which the hot-rolled plate is cold-rolled to produce a cold-rolled plate;
The stage of primary recrystallization annealing of the cold rolled plate; and;
A method for producing a grain-oriented electrical steel sheet, which comprises a step of secondary recrystallization annealing of the cold-rolled sheet for which the primary recrystallization annealing has been completed.
[Equation 1]
0.5 ≤ ([Ba] + [Y]) / ([B] * 10) ≤ 3
(However, in Formula 1, [Ba], [Y], and [B] indicate the contents (% by weight) of Ba, Y, and B, respectively.) 前記スラブは、Ｍｎ：０．０１％〜０．５％をさらに含むことを特徴とする請求項５に記載の方向性電磁鋼板の製造方法。 The method for producing a grain-oriented electrical steel sheet according to claim 5, wherein the slab further contains Mn: 0.01% to 0.5%. 前記スラブを加熱する段階で、１０００〜１２８０℃に加熱することを特徴とする請求項５または請求項６に記載の方向性電磁鋼板の製造方法。 The method for manufacturing a grain-oriented electrical steel sheet according to claim 5 or 6, wherein the slab is heated to 1000 to 1280 ° C. at the stage of heating. 前記熱延板を冷間圧延して冷延板を製造する段階で、最終圧下率が８０％以上であることを特徴とする請求項５乃至請求項７のいずれか一項に記載の方向性電磁鋼板の製造方法。 The direction according to any one of claims 5 to 7 , wherein the final reduction rate is 80% or more at the stage of cold-rolling the hot-rolled sheet to produce the cold-rolled sheet. Manufacturing method of electromagnetic steel sheet. 前記２次再結晶焼鈍する段階は、昇温段階および均熱段階を含み、前記均熱段階の温度は、９００〜１２５０℃であることを特徴とする請求項５乃至請求項８のいずれか一項に記載の方向性電磁鋼板の製造方法。 Any one of claims 5 to 8 , wherein the secondary recrystallization annealing step includes a temperature raising step and a heat soaking step, and the temperature of the heat soaking step is 900 to 1250 ° C. The method for manufacturing a directional electromagnetic steel plate according to the section.
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