JP5923881B2 - Oriented electrical steel sheet and manufacturing method thereof - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 229910000976 Electrical steel Inorganic materials 0.000 title claims description 5
- 238000000137 annealing Methods 0.000 claims description 69
- 229910000831 Steel Inorganic materials 0.000 claims description 47
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- 229910052839 forsterite Inorganic materials 0.000 claims description 44
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 44
- 238000000576 coating method Methods 0.000 claims description 42
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- 239000012298 atmosphere Substances 0.000 claims description 23
- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 230000005381 magnetic domain Effects 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 238000005261 decarburization Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 46
- 229910052742 iron Inorganic materials 0.000 description 21
- 238000000034 method Methods 0.000 description 21
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 9
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005097 cold rolling Methods 0.000 description 4
- 238000005098 hot rolling Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
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- 229910052804 chromium Inorganic materials 0.000 description 2
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- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 229960002261 magnesium phosphate Drugs 0.000 description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 2
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- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、トランスなどの鉄心材料に用いる方向性電磁鋼板およびその製造方法に関するものである。 The present invention relates to a grain-oriented electrical steel sheet used for a core material such as a transformer and a method for manufacturing the same.
方向性電磁鋼板は、主にトランスの鉄心として利用される材料である。トランスの高効率化、低騒音化の観点から、方向性電磁鋼板の材料特性としては低鉄損、低磁歪が求められている。
そのためには、鋼板中の二次再結晶粒を、(110)[001]方位（いわゆる、ゴス方位）に高度に揃えることが重要である。しかし、配向性が高すぎると逆に鉄損が増加してしまうことが知られている。そこで、この欠点を解消するため、鋼板の表面に歪や溝を導入し、磁区の幅を細分化して鉄損を低減する技術、すなわち磁区細分化技術が開発されている。
A grain-oriented electrical steel sheet is a material mainly used as an iron core of a transformer. Low iron loss and low magnetostriction are demanded as material properties of grain-oriented electrical steel sheets from the viewpoint of high efficiency and low noise of the transformer.
For that purpose, it is important to highly align the secondary recrystallized grains in the steel sheet in the (110) [001] orientation (so-called Goth orientation). However, it is known that if the orientation is too high, the iron loss increases. Therefore, in order to eliminate this defect, a technique of introducing a strain or a groove on the surface of the steel sheet to subdivide the magnetic domain width to reduce iron loss, that is, a magnetic domain subdivision technique has been developed.
例えば、特許文献１には、最終製品板にレーザーを照射し、鋼板表層に高転位密度領域を導入し、磁区幅を狭くすることで、鋼板の鉄損を低減する技術が提案されている。また、レーザー照射を用いる磁区細分化技術は、その後改良され（特許文献２、特許文献３および特許文献４などを参照）鉄損特性が良好な方向性電磁鋼板が得られるようになってきている。 For example, Patent Document 1 proposes a technique for reducing the iron loss of a steel sheet by irradiating the final product plate with a laser, introducing a high dislocation density region into the steel sheet surface layer, and narrowing the magnetic domain width. Further, the magnetic domain fragmentation technology using laser irradiation has been improved thereafter (see Patent Document 2, Patent Document 3, and Patent Document 4), and grain oriented electrical steel sheets having good iron loss characteristics have been obtained. .
さらに、フォルステライト被膜の改良による鉄損の低減を図るために、Tiをフォルステライト被膜中にTiNとして固定する技術が特許文献５に開示されている。また、同じく、鉄損の低減を図るために、フォルステライト被膜中のTi,Ｂ,Al量をそれぞれ規定する技術が特許文献６に開示されている。 Furthermore, Patent Document 5 discloses a technique for fixing Ti as TiN in a forsterite coating in order to reduce iron loss by improving the forsterite coating. Similarly, Patent Document 6 discloses a technique for defining the amounts of Ti, B, and Al in the forsterite film in order to reduce iron loss.
しかしながら、上掲したレーザー照射による磁区細分化には、いずれも鋼板の磁歪が増加し、その結果、トランス騒音が増大するという問題があった。特許文献２〜４ではこの問題を解決する手段が提案されているが、効果は十分ではなくトランス騒音の増加を抑えることはできていなかった。
また、特許文献５には、Ｂ元素の添加についてに何ら記載がなく、また、レーザー照射をした際の磁歪特性に関して何ら考慮が払われていない。すなわち、この技術ではレーザー照射部における被膜の局所破壊を抑えることはできず、磁歪が増加すると考えられる。
さらに、特許文献６に記載の技術は、磁束密度が1.0Ｔ程度の低磁場の鉄損特性の改善を図ったものであり、フォルステライトの強度向上には何ら考慮が払われていない。従って、この技術では、レーザー照射部における被膜の局所破壊を抑えることはできず、やはり、磁歪の増加が免れないと考えられる。
However, the above-mentioned magnetic domain subdivision by laser irradiation has a problem that the magnetostriction of the steel sheet increases, and as a result, transformer noise increases. Patent Documents 2 to 4 propose means for solving this problem, but the effect is not sufficient and an increase in transformer noise cannot be suppressed.
Further, Patent Document 5 has no description about the addition of B element, and no consideration is given to the magnetostriction characteristics when laser irradiation is performed. That is, it is considered that this technique cannot suppress local destruction of the coating film in the laser irradiation portion and increases magnetostriction.
Furthermore, the technique described in Patent Document 6 is intended to improve the iron loss characteristics of a low magnetic field with a magnetic flux density of about 1.0 T, and no consideration is given to the improvement of the strength of forsterite. Therefore, with this technique, it is considered that local destruction of the coating film in the laser irradiation portion cannot be suppressed, and an increase in magnetostriction is unavoidable.
本発明は、上記した現状に鑑み開発されたもので、実機トランスに組上げた場合に、優れた低騒音性および低鉄損特性を得ることができる方向性電磁鋼板を、その有利な製造方法と共に提供することを目的とする。 The present invention has been developed in view of the above-described present situation, and a grain-oriented electrical steel sheet capable of obtaining excellent low noise and low iron loss characteristics when assembled in an actual transformer, together with its advantageous manufacturing method. The purpose is to provide.
すなわち、本発明の要旨構成は次のとおりである。
１．表面にフォルステライト被膜をそなえ、レーザー照射による磁区細分化済みの方向性電磁鋼板であって、該フォルステライト被膜中に、１〜20mass％のTiと、0.02〜0.4mass％のＢを含有し、これらの被膜中Ｎに対する物質量比（Ti＋Ｂ）/Ｎが0.7〜1.3の範囲を満足し、かつ前記レーザー照射の照射領域におけるフォルステライト被膜の剥離率が70％以下であることを特徴とする方向性電磁鋼板。
That is, the gist configuration of the present invention is as follows.
1. It is a grain-oriented electrical steel sheet that has a forsterite coating on the surface and has been magnetically subdivided by laser irradiation, and contains 1-20 mass% Ti and 0.02-0.4 mass% B in the forsterite coating, object mass ratio of these coatings N (Ti + B) / N is within the ranges of 0.7 to 1.3, and the peeling rate of the forsterite film in the irradiated area of the laser irradiation, characterized in der Rukoto 70% or less Oriented electrical steel sheet.
２．方向性電磁鋼板用スラブを、熱間圧延し、ついで必要に応じて熱延板焼鈍を施したのち、１回または中間焼鈍を挟む２回以上の冷間圧延を施して、最終板厚に仕上げたのち、脱炭焼鈍を施し、ついで鋼板表面にMgOを主成分とする焼鈍分離剤を塗布してから、最終仕上げ焼鈍を行った後、レーザー照射による磁区細分化を施す一連の工程により方向性電磁鋼板を製造するに際し、
(1) 上記焼鈍分離剤中に、該焼鈍分離剤中のMgO：100質量部に対してTiO2：１〜30質量部を含有させる、
(2) 上記焼鈍分離剤の鋼板表面に対する塗布量を、目付量（両面）で８〜20g/m2とする、
(3) 上記焼鈍分離剤中のＢと鋼中のＢの合計量が鋼質量に対して0.0002〜0.002mass％の範囲とする、
(4) 上記最終仕上げ焼鈍を、窒素濃度が15vol％以上の非酸化性雰囲気中にて、1050℃以上、２時間以上の条件で行う、
(5) ついで、窒素濃度が２vol%以下の水素雰囲気中にて、1150〜1250℃の温度範囲に少なくとも２時間保持する
ことを特徴とする方向性電磁鋼板の製造方法。
2 . The slab for grain-oriented electrical steel sheet is hot-rolled and then subjected to hot-rolled sheet annealing as necessary, and then cold-rolled at least once with one or more intermediate annealings to the final thickness. Then, after decarburization annealing, and then applying an annealing separator mainly composed of MgO to the steel sheet surface, after final finishing annealing, the direction of the magnetic domain is subdivided by laser irradiation. When manufacturing electrical steel sheets,
(1) In the annealing separator, TiO 2 : 1 to 30 parts by mass with respect to 100 parts by mass of MgO in the annealing separator,
(2) The amount of the annealing separator applied to the steel sheet surface is 8 to 20 g / m 2 in basis weight (both sides).
(3) The total amount of B in the annealing separator and B in the steel is in the range of 0.0002 to 0.002 mass% with respect to the steel mass.
(4) The final finish annealing is performed in a non-oxidizing atmosphere with a nitrogen concentration of 15 vol% or more under conditions of 1050 ° C. or more and 2 hours or more.
(5) Next, a method for producing a grain-oriented electrical steel sheet, wherein the steel sheet is kept in a temperature range of 1150 to 1250 ° C. for at least 2 hours in a hydrogen atmosphere having a nitrogen concentration of 2 vol% or less.
本発明によれば、レーザーを用いた磁区細分化による鉄損低減効果が、実機トランスにおいても効果的に維持されるため、実機トランスにおいて優れた低騒音性および低鉄損特性を発現することができる。 According to the present invention, since the iron loss reduction effect due to magnetic domain subdivision using a laser is effectively maintained even in an actual transformer, it is possible to express excellent low noise and low iron loss characteristics in the actual transformer. it can.
以下、本発明について具体的に説明する。
上記した実機トランスの騒音問題に対して、発明者らによる種々の調査の結果、フォルステライト被膜（以下、単に被膜ともいう）の組成がトランスの騒音に大きな影響を及ぼしていることが判明した。すなわち、フォルステライト被膜の組成がある所定の範囲から外れた場合に、磁歪の高調波成分が増加し、その結果、トランス騒音が増大するのである。
この現象は、レーザー照射により照射部周辺のフォルステライト被膜が破壊されるためではないかと推定している。すなわち、フォルステライト被膜の破壊が起ることによって、レーザー照射領域（部）周辺に形成された被膜の応力状態が変化し、還流磁区が不安定となるために、交流励磁中の磁区構造が変化しやすくなり、その結果として磁歪の高調波成分が増加してしまうものと考えられる。
Hereinafter, the present invention will be specifically described.
As a result of various investigations by the inventors with respect to the above-mentioned noise problem of the actual transformer, it has been found that the composition of the forsterite coating (hereinafter also simply referred to as coating) has a great influence on the noise of the transformer. That is, when the composition of the forsterite film deviates from a predetermined range, the harmonic component of magnetostriction increases, and as a result, transformer noise increases.
This phenomenon is presumed to be due to the destruction of the forsterite film around the irradiated area by laser irradiation. That is, when the forsterite film breaks, the stress state of the film formed around the laser irradiation region (part) changes and the reflux magnetic domain becomes unstable, so the magnetic domain structure changes during AC excitation. As a result, it is considered that the harmonic component of magnetostriction increases.
そこで、発明者らは、被膜の組成とトランス騒音の関係を詳細に調査した。その結果、フォルステライト被膜中のTi量を１〜20mass％で、Ｂ量を0.02〜0.4mass％とし、（Ti＋Ｂ）/Ｎを物質量比で0.7〜1.3の範囲に制御すればよいことが分かった。
これは、フォルステライト被膜中に適切な量のTiNやBNが含まれていると、レーザー照射による熱衝撃を受けても被膜が破壊されにくくなり、鋼板の磁歪特性が良好なままに維持されるからと考えられる。
また、上記の効果はTiN単体では得られず、適切な量のBNと共存させることが必要である。なお、BNはフォルステライトの結晶粒界、フォルステライト-TiN界面、被膜-地鉄界面などに偏析し、被膜に耐熱衝撃性を付与していると考えられる。
Therefore, the inventors investigated in detail the relationship between the coating composition and transformer noise. As a result, it is understood that the Ti amount in the forsterite film should be 1 to 20 mass%, the B amount should be 0.02 to 0.4 mass%, and (Ti + B) / N should be controlled within the range of 0.7 to 1.3 in terms of the amount of substance. It was.
This means that if the forsterite film contains an appropriate amount of TiN or BN, the film will not be destroyed even when subjected to thermal shock by laser irradiation, and the magnetostrictive properties of the steel sheet will remain good. It is thought from.
In addition, the above effect cannot be obtained with TiN alone, and it is necessary to coexist with an appropriate amount of BN. BN segregates at the grain boundaries of forsterite, the forsterite-TiN interface, the coating-steel interface, etc., and is considered to impart thermal shock resistance to the coating.
ここに、本発明では、フォルステライト被膜の成分組成を上記の範囲に制御することにより、鋼板表面のレーザー照射部におけるフォルステライト被膜の剥離率が70％以下に抑制される。 Here, in the present invention, by controlling the component composition of the forsterite film within the above range, the peeling rate of the forsterite film at the laser irradiated portion on the steel sheet surface is suppressed to 70% or less.
本発明において、フォルステライト被膜の成分を制御する製造法上のポイントは、以下の４つである。
(a) 脱炭焼鈍後、焼鈍分離剤を塗布する際に、焼鈍分離剤中Ｂと鋼中Ｂとの合計量を鋼質量に対して、0.0002〜0.002mass％の範囲に調整する。
(b) 焼鈍分離剤中のMgO：100質量部に対してTiO2：１〜30質量部を含有させる。
(c) 仕上げ焼鈍において、1050℃以上の温度範囲で少なくとも２時間は窒素濃度が15vol％以上の非酸化性雰囲気とする。
(d) さらに仕上げ焼鈍において、1150〜1250℃の温度範囲で少なくとも２時間は窒素濃度が２vol%以下の水素雰囲気とする。
In the present invention, there are the following four points in the production method for controlling the components of the forsterite film.
(a) When applying the annealing separator after decarburization annealing, the total amount of B in the annealing separator and B in the steel is adjusted to a range of 0.0002 to 0.002 mass% with respect to the steel mass.
(b) TiO 2 : 1 to 30 parts by mass with respect to 100 parts by mass of MgO in the annealing separator.
(c) In the finish annealing, a non-oxidizing atmosphere having a nitrogen concentration of 15 vol% or more is set in a temperature range of 1050 ° C. or more for at least 2 hours.
(d) Further, in the finish annealing, a hydrogen atmosphere having a nitrogen concentration of 2 vol% or less is set in the temperature range of 1150 to 1250 ° C. for at least 2 hours.
上記した(a)について、本発明では、焼鈍分離剤中Ｂを、鋼中Ｂと等価にみて、鋼質量に対するＢ濃度の値を求める式でその値を規定することが重要である。すなわち、（焼鈍分離剤中Ｂ量＋鋼中Ｂ量）／鋼質量の式で求めた値を、鋼質量に対するＢ比率として、0.0002〜0.002mass％の範囲に調整することが肝要である。
ここに、焼鈍分離剤中Ｂ量は、焼鈍分離剤の塗布量や、MgO中のＢ濃度、副剤として添加するＢ化合物量などを調整することで制御することができる。
なお、焼鈍分離剤にその他の化合物を添加する場合、当該化合物中の不純物Ｂ量を管理する必要がある。
Regarding the above (a), in the present invention, it is important to define B in the annealing separator equivalent to B in steel, and to define the value by an equation for determining the value of B concentration relative to the steel mass. That is, it is important to adjust the value obtained by the formula of (B amount in annealing separator + B amount in steel) / steel mass to a range of 0.0002 to 0.002 mass% as a B ratio to steel mass.
Here, the amount of B in the annealing separator can be controlled by adjusting the coating amount of the annealing separator, the B concentration in MgO, the amount of B compound added as an auxiliary agent, and the like.
In addition, when adding another compound to an annealing separator, it is necessary to manage the amount of impurities B in the compound.
以下、本発明における成分組成などの限定理由、および好適範囲について述べる。
フォルステライト被膜中のTi量：１〜20mass％
Tiは被膜の耐熱衝撃性を向上させる効果がある。１mass％未満の場合は、添加効果が得られない。一方、20mass％より多く含まれる場合は、被膜の外観や密着性が劣化する。そのためTi量は１〜20mass％に限定する。さらに好ましくは２〜10mass％である。また、Tiは主にTiNとして被膜に含まれることが有利である。好ましくはTi化合物の70％以上がTiNである。
ここに、TiNは熱的に非常に安定な物質であり、被膜に耐熱衝撃性を付与すると考えられるが、前述したようにTiN単体では所望の被膜改善効果が得られないため、以下のＢとの共存が必須である。
Hereinafter, the reason for limitation such as the component composition in the present invention and the preferred range will be described.
Ti amount in forsterite coating: 1 to 20 mass%
Ti has the effect of improving the thermal shock resistance of the coating. If it is less than 1 mass%, the effect of addition cannot be obtained. On the other hand, when it contains more than 20 mass%, the external appearance and adhesiveness of a film will deteriorate. Therefore, the Ti amount is limited to 1 to 20 mass%. More preferably, it is 2-10 mass%. In addition, it is advantageous that Ti is mainly contained in the coating as TiN. Preferably, 70% or more of the Ti compound is TiN.
Here, TiN is a thermally stable material and is considered to impart thermal shock resistance to the coating. However, as described above, the desired coating improvement effect cannot be obtained with TiN alone, so the following B and Coexistence is essential.
フォルステライト被膜中のＢ量：0.02〜0.4mass％
ＢもTiと同様、被膜の強度および耐熱衝撃性を向上させる効果がある。0.02mass％未満の場合は添加効果が得られず、一方0.4mass％より多く含まれる場合は被膜性状が損なわれてしまう。そのためＢ量は0.02〜0.4mass％に限定する。好ましい範囲は0.2〜0.4mass％である。被膜に含まれる微量Ｂは、フォルステライト結晶粒界やフォルステライト-TiN界面、または被膜-地鉄界面に偏析し、フォルステライト被膜に耐熱衝撃性を付与していると考えられる。なお、本発明では、上述したように、TiN単体では所望の効果は得られないため、上記Ｂとの共存が必須である。
B content in forsterite film: 0.02 to 0.4 mass%
B, like Ti, has the effect of improving the strength and thermal shock resistance of the coating. When the amount is less than 0.02 mass%, the effect of addition cannot be obtained. On the other hand, when the amount is more than 0.4 mass%, the film properties are impaired. Therefore, the amount of B is limited to 0.02 to 0.4 mass%. A preferable range is 0.2 to 0.4 mass%. It is considered that the trace amount B contained in the coating is segregated at the forsterite crystal grain boundary, the forsterite-TiN interface, or the coating-base metal interface, and imparts thermal shock resistance to the forsterite coating. In addition, in this invention, since a desired effect is not acquired with TiN single-piece | unit as mentioned above, coexistence with said B is essential.
（Ti＋Ｂ）/Ｎ：0.7〜1.3
本発明において、Ti,Ｂは主に窒化物として被膜中に固定させる必要がある。(Ti+Ｂ)/Ｎの値が0.7未満の場合は過剰な窒素が鋼中に侵入し、磁気特性が損なわれる。一方1.3より高い場合は、TiN,BNが不足し被膜の耐熱衝撃性が損なわれるため、0.7〜1.3の範囲に限定する。好ましくは0.8〜1.2の範囲である。
なお、被膜中のＮ量は0.3〜10mass％とすることが好ましい。0.3mass％を下回ると被膜の耐熱衝撃性が不足し、10mass％を超えると被膜の外観や密着性が低下する。
(Ti + B) / N: 0.7 to 1.3
In the present invention, Ti and B need to be fixed in the film mainly as nitrides. When the value of (Ti + B) / N is less than 0.7, excess nitrogen penetrates into the steel and the magnetic properties are impaired. On the other hand, when it is higher than 1.3, TiN and BN are insufficient and the thermal shock resistance of the coating is impaired, so the range is limited to 0.7 to 1.3. Preferably it is the range of 0.8-1.2.
In addition, it is preferable that N amount in a film shall be 0.3-10 mass%. If it is less than 0.3 mass%, the thermal shock resistance of the coating is insufficient, and if it exceeds 10 mass%, the appearance and adhesion of the coating are reduced.
フォルステライト被膜の剥離率：70％以下
フォルステライト被膜の成分組成を、上記した範囲に制御して、フォルステライト被膜の耐熱衝撃性を向上させることにより、鋼板表面のレーザー照射領域におけるフォルステライト被膜の剥離率は、70％以下に抑制される。フォルステライト被膜の剥離率が70％以下の場合、フォルステライト被膜の局所破壊が抑制され、トランス特性を改善させることができる。より好ましい範囲は50％以下、さらに好ましい範囲は35％以下である。
Forsterite film peeling rate: 70% or less By controlling the forsterite film component composition to the above range and improving the thermal shock resistance of the forsterite film, the forsterite film in the laser irradiation area of the steel sheet surface The peeling rate is suppressed to 70% or less. When the peeling rate of the forsterite film is 70% or less, local destruction of the forsterite film is suppressed, and transformer characteristics can be improved. A more preferred range is 50% or less, and a further preferred range is 35% or less.
また、上述したように、フォルステライト被膜の局所破壊を抑制することで、レーザー照射後のコーティング塗布工程を省略できるというメリットがある。なお、コーティング塗布工程を省略する場合には、本発明に記載のフォルステライト被膜とした上で、さらにレーザー出力を下げる条件とすることが好ましい。 Further, as described above, there is an advantage that the coating application process after laser irradiation can be omitted by suppressing local destruction of the forsterite film. In the case where the coating application step is omitted, it is preferable that the forsterite film described in the present invention is used and the laser output is further reduced.
フォルステライト被膜の剥離率は、レーザー照射部の中心部を線分法で評価すればよい。
具体的に、フォルステライト被膜の剥離率（％）は、レーザー照射部の中心部に線分を引き、当該線分の長さＡと、当該線分がフォルステライト被膜剥離部を横切る部分の合計長さＢとから、Ｂ／Ａ×100の式で決定できる。
なお、上記線分法を行うに際しては、煮沸した苛性ソーダなどでリン酸塩コーティングを除去して評価してもよい。また、フォルステライト被膜の剥離の有無は、光学顕微鏡やSEMを用いることで容易に判断できるので、合計で１cm程度の長さのレーザー照射領域を評価すれば、当該レーザー照射領域の剥離率が推定でき、その結果を、レーザー照射の条件に反映することで、フォルステライト被膜の剥離のばらつきを、十分に低減することができる。
The peeling rate of the forsterite film may be evaluated by the line segment method at the center of the laser irradiation part.
Specifically, the forsterite film peeling rate (%) is the sum of the length A of the line segment and the portion where the line segment crosses the forsterite film peeling part. From the length B, it can be determined by the formula B / A × 100.
In addition, when performing the said line segment method, you may evaluate by removing a phosphate coating with the boiling caustic soda. In addition, since the presence or absence of peeling of the forsterite film can be easily determined by using an optical microscope or SEM, if the laser irradiation area having a total length of about 1 cm is evaluated, the peeling rate of the laser irradiation area is estimated. By reflecting the result on the laser irradiation conditions, it is possible to sufficiently reduce the variation in peeling of the forsterite film.
次に、本発明に従う方向性電磁鋼板の製造条件に関して具体的に説明する。
本発明において、方向性電磁鋼板用スラブの成分組成は、二次再結晶が生じる成分組成であればよい。
また、インヒビターを利用する場合、例えばAlN系インヒビターを利用する場合であればAlおよびＮを、またMnS・MnSe系インヒビターを利用する場合であればMnとSeおよび／またはＳを適量含有させればよい。勿論、両インヒビターを併用してもよい。この場合におけるAl、Ｎ、ＳおよびSeの好適含有量はそれぞれ、Al：0.012〜0.05mass％、Ｎ：0.004〜0.012mass％、ＳおよびSeから選んだ１種もしくは２種の合計：0.010〜0.040mass％である。
Next, the manufacturing conditions of the grain-oriented electrical steel sheet according to the present invention will be specifically described.
In the present invention, the component composition of the slab for grain-oriented electrical steel sheet may be a component composition that causes secondary recrystallization.
Further, when using an inhibitor, for example, when using an AlN-based inhibitor, Al and N, and when using an MnS / MnSe-based inhibitor, an appropriate amount of Mn and Se and / or S should be contained. Good. Of course, both inhibitors may be used in combination. The preferred contents of Al, N, S and Se in this case are Al: 0.012 to 0.05 mass%, N: 0.004 to 0.012 mass%, and one or two total selected from S and Se: 0.010 to 0.040. mass%.
さらに、本発明は、Al、Ｎ、Ｓ、Seの含有量を制限した、インヒビターを使用しない方向性電磁鋼板にも適用することができる。
この場合には、Al、Ｎ、ＳおよびSe量はそれぞれ、Al：100massppm以下、Ｎ：50massppm以下、Ｓ：50massppm以下、Se：50massppm以下に抑制することが好ましい。
Furthermore, the present invention can also be applied to grain-oriented electrical steel sheets in which the contents of Al, N, S, and Se are limited and no inhibitor is used.
In this case, the amounts of Al, N, S, and Se are preferably suppressed to Al: 100 massppm or less, N: 50 massppm or less, S: 50 massppm or less, and Se: 50 massppm or less, respectively.
本発明の方向性電磁鋼板用スラブの基本成分および任意添加成分について具体的に述べると次のとおりである。
Ｃ：0.08mass％以下
Ｃは、熱延板組織の改善のために添加をするが、0.08mass％を超えると製造工程中に磁気時効の起こらない50massppm以下までＣを低減することが困難になるため、0.08mass％以下とすることが好ましい。なお、下限に関しては、Ｃを含まない素材でも二次再結晶が可能であるので特に設ける必要はない。
The basic components and optional components of the slab for grain-oriented electrical steel sheets according to the present invention are specifically described as follows.
C: 0.08 mass% or less C is added to improve the hot-rolled sheet structure, but if it exceeds 0.08 mass%, it becomes difficult to reduce C to 50 massppm or less at which no magnetic aging occurs during the manufacturing process. Therefore, it is preferable to set it as 0.08 mass% or less. In addition, regarding the lower limit, since a secondary recrystallization is possible even for a material not containing C, there is no need to provide it.
Si：2.0〜8.0mass％
Siは、鋼の電気抵抗を高め、鉄損を改善するのに有効な元素であるが、含有量が2.0mass％に満たないと十分な鉄損低減効果が達成達成しにくく、一方、8.0mass％を超えると加工性が著しく低下し、また磁束密度も低下するおそれがあるため、Si量は2.0〜8.0mass％の範囲とすることが好ましい。
Si: 2.0-8.0mass%
Si is an element effective in increasing the electrical resistance of steel and improving iron loss, but if the content is less than 2.0 mass%, it is difficult to achieve a sufficient iron loss reduction effect, while 8.0 mass If it exceeds 50%, the workability is remarkably lowered and the magnetic flux density may also be lowered. Therefore, the Si content is preferably in the range of 2.0 to 8.0 mass%.
Mn：0.005〜1.0mass％
Mnは、熱間加工性を良好にする上で必要な元素であるが、含有量が0.005mass％未満ではその添加効果に乏しく、一方1.0mass％を超えると製品板の磁束密度が低下するため、Mn量は0.005〜1.0mass％の範囲とすることが好ましい。
Mn: 0.005 to 1.0 mass%
Mn is an element necessary for improving the hot workability, but if the content is less than 0.005 mass%, the effect of addition is poor, while if it exceeds 1.0 mass%, the magnetic flux density of the product plate decreases. The Mn content is preferably in the range of 0.005 to 1.0 mass%.
上記の基本成分以外に、磁気特性改善成分として、次に述べる元素を適宜含有させることができる。
Ni：0.03〜1.50mass％、Sn：0.01〜1.50mass％、Sb：0.005〜1.50mass％、Cu：0.03〜3.0mass％、Ｐ：0.03〜0.50mass％、Mo：0.005〜0.10mass％およびCr：0.03〜1.50mass％のうちから選んだ少なくとも１種
Niは、熱延板組織を改善して磁気特性を向上させるために有用な元素である。しかしながら、含有量が0.03mass％未満では磁気特性の向上効果が小さく、一方1.5mass％を超えると二次再結晶が不安定になり磁気特性が劣化する。そのため、Ni量は0.03〜1.5mass％の範囲とするのが好ましい。
In addition to the above basic components, the following elements can be appropriately contained as magnetic property improving components.
Ni: 0.03-1.50 mass%, Sn: 0.01-1.50 mass%, Sb: 0.005-1.50 mass%, Cu: 0.03-3.0 mass%, P: 0.03-0.50 mass%, Mo: 0.005-0.10 mass% and Cr: At least one selected from 0.03 to 1.50 mass%
Ni is an element useful for improving the magnetic properties by improving the hot-rolled sheet structure. However, if the content is less than 0.03 mass%, the effect of improving the magnetic properties is small, whereas if it exceeds 1.5 mass%, the secondary recrystallization becomes unstable and the magnetic properties are deteriorated. Therefore, the amount of Ni is preferably in the range of 0.03 to 1.5 mass%.
また、Sn、Sb、Cu、Ｐ、MoおよびCrはそれぞれ磁気特性の向上に有用な元素であるが、いずれも上記した各成分の下限に満たないと、磁気特性の向上効果が小さく、一方、上記した各成分の上限量を超えると、二次再結晶粒の発達が阻害されるため、それぞれ上記の範囲で含有させることが好ましい。
さらに、製品板の被膜中Ｂを制御するために、スラブに0.002mass%以下のＢを含有させてもよい。
なお、上記成分以外の残部は、製造工程において混入する不可避不純物およびFeである。
Sn, Sb, Cu, P, Mo and Cr are elements useful for improving the magnetic properties, respectively, but if any of them is less than the lower limit of each component described above, the effect of improving the magnetic properties is small, If the upper limit amount of each component described above is exceeded, the development of secondary recrystallized grains is hindered.
Furthermore, in order to control B in the coating on the product plate, 0.002 mass% or less of B may be contained in the slab.
The balance other than the above components is inevitable impurities and Fe mixed in the manufacturing process.
次いで、上記した成分組成を有するスラブは、常法に従い加熱して熱間圧延に供するが、鋳造後、加熱せずに直ちに熱間圧延してもよい。薄鋳片の場合には熱間圧延しても良いし、熱間圧延を省略してそのまま以後の工程に進んでもよい。 Next, the slab having the above-described component composition is heated and subjected to hot rolling according to a conventional method, but may be immediately hot rolled after casting without being heated. In the case of a thin slab, hot rolling may be performed, or the hot rolling may be omitted and the process may proceed as it is.
さらに、必要に応じて熱延板焼鈍を施す。この時、ゴス組織を製品板において高度に発達させるためには、熱延板焼鈍温度として800〜1100℃の範囲が好適である。熱延板焼鈍温度が800℃未満であると、熱間圧延でのバンド組織が残留し、整粒した一次再結晶組織を実現することが困難になり、二次再結晶の発達が阻害されるおそれがある。一方、熱延板焼鈍温度が1100℃を超えると、熱延板焼鈍後の粒径が粗大化しすぎるために、整粒した一次再結晶組織の実現が困難となる。 Furthermore, hot-rolled sheet annealing is performed as necessary. At this time, in order to develop a goth structure at a high level in the product plate, a range of 800 to 1100 ° C. is preferable as the hot-rolled sheet annealing temperature. When the hot-rolled sheet annealing temperature is less than 800 ° C, the band structure in hot rolling remains, making it difficult to achieve a sized primary recrystallization structure and inhibiting the development of secondary recrystallization. There is a fear. On the other hand, if the hot-rolled sheet annealing temperature exceeds 1100 ° C., the grain size after the hot-rolled sheet annealing becomes too coarse, and it becomes difficult to realize a sized primary recrystallized structure.
熱延板焼鈍後は、１回または中間焼鈍を挟む２回以上の冷間圧延を施した後、再結晶焼鈍を行い、MgOを主体とする焼鈍分離剤を、鋼板の両面に８〜20g/m2の目付量で塗布する。目付量が両面で８g/m2未満の場合、被膜形成量が不足し、一方20g/m2より多い場合、被膜形成量が過剰となる。いずれの場合も被膜の外観や密着性を損なうため、焼鈍分離剤の塗布量は、鋼板の両面に目付量で８〜20g/m2の範囲に限定する。 After hot-rolled sheet annealing, it is cold-rolled at least once with intermediate or intermediate annealing, followed by recrystallization annealing, and an annealing separator mainly composed of MgO is applied to both sides of the steel sheet at 8 to 20 g / It applied in weight per unit area of m 2. When the basis weight is less than 8 g / m 2 on both sides, the film formation amount is insufficient. On the other hand, when the basis weight is more than 20 g / m 2 , the film formation amount is excessive. In any case, the coating amount of the annealing separator is limited to a range of 8 to 20 g / m 2 in terms of the basis weight on both surfaces of the steel sheet in order to impair the appearance and adhesion of the coating.
また、本発明に従う焼鈍分離剤は、その焼鈍分離剤中のMgO：100質量部に対してTiO2：１〜30質量部を含有し、かつ焼鈍分離剤中Ｂと鋼中Ｂの合計量が鋼質量に対して0.0002〜0.002mass％となるように調整するのは、前述したとおりである。
TiO2がMgO：100質量部に対して１質量部未満だと被膜中Ti量が不足し、一方30質量部より多いと焼鈍分離剤中のMgOが不足するため、いずれも被膜の外観や密着性を損なうこととなる。また、Ｂの合計量（焼鈍分離剤中Ｂ＋鋼中Ｂ）が鋼質量に対して0.0002mass％未満だと、所期したような被膜の耐熱衝撃性が得られない。一方0.002mass％超だと、被膜の外観や密着性が損なわれるのみならず、過剰なＢが鋼中に残留し、鋼板の純化不良を引き起こしてしまう。従って、TiO2とＢの量はそれぞれ上記の範囲に限定する。さらに好ましくは、TiO2が５〜15質量部であり、Ｂ比率は0.001〜0.002mass％である。
Moreover, the annealing separator according to the present invention contains TiO 2 : 1 to 30 parts by mass with respect to MgO: 100 parts by mass in the annealing separator, and the total amount of B in the annealing separator and B in the steel is The adjustment to be 0.0002 to 0.002 mass% with respect to the steel mass is as described above.
If TiO 2 is less than 1 part by mass with respect to 100 parts by mass of MgO, the amount of Ti in the film will be insufficient, while if it exceeds 30 parts by mass, MgO in the annealing separator will be insufficient. It will damage the sex. Further, if the total amount of B (B in annealing separator + B in steel) is less than 0.0002 mass% with respect to the steel mass, the thermal shock resistance of the coating film as expected cannot be obtained. On the other hand, if it exceeds 0.002 mass%, not only the appearance and adhesion of the coating film are impaired, but also excess B remains in the steel, resulting in poor purification of the steel sheet. Accordingly, the amounts of TiO 2 and B are limited to the above ranges, respectively. More preferably, a TiO 2 5 to 15 parts by weight, B ratio is 0.001~0.002mass%.
なお、前述したように、焼鈍分離剤中にＢ化合物を添加してＢ量を調整してもよい。例えば、ホウ酸やホウ酸塩などのＢ化合物を、焼鈍分離剤中のMgO：100質量部に対してＢ換算で0.1〜５質量部程度含有させることが好適である。さらに、被膜性状改善や磁気特性改善の観点から、他の公知の化合物を焼鈍分離剤に添加してもよい。例えば、アルカリ土類金属の水酸化物、硫酸塩などは被膜の外観や密着性の改善に効果的である。 As described above, the amount of B may be adjusted by adding a B compound in the annealing separator. For example, it is preferable to contain about 0.1 to 5 parts by mass of B compound such as boric acid or borate in terms of B with respect to 100 parts by mass of MgO in the annealing separator. Furthermore, other known compounds may be added to the annealing separator from the viewpoint of improving film properties and magnetic properties. For example, alkaline earth metal hydroxides and sulfates are effective in improving the appearance and adhesion of the coating.
本発明において、最終仕上げ焼鈍中、1050℃以上の高い温度範囲で少なくとも２時間、窒素濃度が15vol％以上の非酸化性雰囲気とし、その後1150〜1250℃の温度範囲で少なくとも２時間、窒素濃度が２vol%以下の水素雰囲気とする必要がある。 In the present invention, during the final finish annealing, a non-oxidizing atmosphere having a nitrogen concentration of 15 vol% or more is maintained for at least 2 hours in a high temperature range of 1050 ° C. or higher, and then the nitrogen concentration is at least 2 hours in a temperature range of 1150 to 1250 ° C. The hydrogen atmosphere must be 2 vol% or less.
窒素濃度が15vol％以上の非酸化性雰囲気中での処理は、TiやＢをフォルステライト被膜中に窒化物として固定するのに必要なプロセスである。ここで、この処理の上記した温度、時間および雰囲気のうちいずれか一つでも、その条件を満たさない場合は、所期したような窒化物固定の効果が得られない。なお、1250℃より高いと焼鈍炉の耐火物が損傷し、コストが高くなるので、窒素濃度が15vol％以上とする温度域は1250℃以下程度とすることが好ましい。
また、引続く窒素濃度が２vol%以下の水素雰囲気中での処理は、被膜形成および鋼中Ｎを含む不純物の純化に必要な工程である。
The treatment in a non-oxidizing atmosphere having a nitrogen concentration of 15 vol% or more is a process necessary for fixing Ti and B as nitrides in the forsterite film. Here, if any one of the above-described temperature, time, and atmosphere of this treatment does not satisfy the conditions, the desired effect of fixing the nitride cannot be obtained. If the temperature is higher than 1250 ° C., the refractory of the annealing furnace is damaged and the cost is increased. Therefore, the temperature range in which the nitrogen concentration is 15 vol% or higher is preferably about 1250 ° C. or lower.
Further, the subsequent treatment in a hydrogen atmosphere having a nitrogen concentration of 2 vol% or less is a process necessary for film formation and purification of impurities including N in the steel.
上記した以外の製造条件については、従来公知の方法を用いることができる。例えば、昇温過程の低温領域において、還元性雰囲気を導入することは被膜形成上不利であるため、水素濃度が２vol%以下の窒素雰囲気、アルゴン雰囲気、または両者の混合雰囲気を導入することが好ましい。一方高温領域においては、還元性雰囲気を導入することが被膜形成上有利であるため、水素濃度：２vol%以上の還元性雰囲気を導入することが好ましい。 Conventionally known methods can be used for manufacturing conditions other than those described above. For example, introduction of a reducing atmosphere in the low temperature region of the temperature raising process is disadvantageous in terms of film formation. Therefore, it is preferable to introduce a nitrogen atmosphere, an argon atmosphere, or a mixed atmosphere of which the hydrogen concentration is 2 vol% or less. . On the other hand, in the high temperature region, since it is advantageous for forming a film to introduce a reducing atmosphere, it is preferable to introduce a reducing atmosphere having a hydrogen concentration of 2 vol% or more.
ここに、両者の切り替え温度は700〜950℃とすることが好適である。好適範囲を外れた場合、被膜の外観や密着性が損なわれるおそれが生じる。また、700〜900℃の温度領域で数十時間保定を行うことは、磁気特性向上の観点から有利である。さらに、仕上焼鈍を２回に分けて、２次再結晶と被膜形成を別々に実施することは、被膜性状改善の観点から有利である。 Here, the switching temperature between the two is preferably 700 to 950 ° C. When it deviates from a suitable range, there exists a possibility that the external appearance and adhesiveness of a film may be impaired. In addition, it is advantageous to maintain for several tens of hours in the temperature range of 700 to 900 ° C. from the viewpoint of improving magnetic properties. Furthermore, it is advantageous from the viewpoint of improving the properties of the film that the final annealing is divided into two times and the secondary recrystallization and the film formation are performed separately.
本発明では、最終仕上げ焼鈍後、平坦化焼鈍を行って鋼板の形状を矯正することが有効であり、鋼板を積層して使用する場合には、鉄損を改善する目的で、平坦化焼鈍前または後に、鋼板表面に絶縁コーティングを施すことが有効である。この絶縁コーティングは、鉄損低減のために、鋼板に張力を付与できるコーティングとすることが望ましい。張力を付与できるコーティングとしては、シリカを含有する無機系コーティングや物理蒸着法、化学蒸着法等によるセラミックコーティング等が挙げられる。 In the present invention, it is effective to correct the shape of the steel sheet by performing flattening annealing after the final finish annealing. Alternatively, it is effective to apply an insulating coating to the steel sheet surface later. This insulating coating is desirably a coating capable of imparting tension to the steel sheet in order to reduce iron loss. Examples of the coating capable of imparting tension include inorganic coating containing silica, ceramic coating by physical vapor deposition, chemical vapor deposition, and the like.
本発明では、最終仕上げ焼鈍後、さらには絶縁コーティング付与後において、鋼板表面にレーザーを照射することにより、鋼板の磁区を細分化する。
本発明で照射するレーザーの光源としては、連続波レーザー、パルスレーザーのいずれでもよく、YAGレーザーやCO2レーザー等の種類を選ばない。また、照射痕は線状でも点状でも構わないが、これら照射痕の方向は、鋼板の圧延方向に対して、90°から45°をなす方向であることが好ましい。
なお、最近使用されるようになってきたグリーンレーザーマーカーは、照射精度の面で特に好適である。
In the present invention, the magnetic domains of the steel sheet are subdivided by irradiating the surface of the steel sheet with laser after the final finish annealing and further after the application of the insulating coating.
The laser light source used in the present invention may be either a continuous wave laser or a pulsed laser, and any type such as a YAG laser or a CO 2 laser may be used. The irradiation marks may be linear or point-like, but the direction of these irradiation marks is preferably a direction that forms 90 ° to 45 ° with respect to the rolling direction of the steel sheet.
The green laser marker that has recently been used is particularly suitable in terms of irradiation accuracy.
本発明で用いるグリーンレーザーマーカーにおけるレーザーの出力は、単位長さ当たりの熱量として、５〜100J/m程度の範囲が好ましい。また、レーザービームのスポット径は0.1〜0.5mm程度の範囲とし、圧延方向の繰返し間隔は１〜20mm程度の範囲とすることが好ましい。
なお、鋼板に付与される線状歪の幅は50〜500μｍ程度とするのが好適である。ここに、線状とは、実線だけでなく、点線や破線なども含むものとする。
The laser output of the green laser marker used in the present invention is preferably in the range of about 5 to 100 J / m as the amount of heat per unit length. The spot diameter of the laser beam is preferably in the range of about 0.1 to 0.5 mm, and the repetition interval in the rolling direction is preferably in the range of about 1 to 20 mm.
In addition, it is suitable that the width | variety of the linear distortion provided to a steel plate shall be about 50-500 micrometers. Here, the line shape includes not only a solid line but also a dotted line and a broken line.
本発明において、上述した工程や製造条件以外については、従来公知の方向性電磁鋼板の製造方法を適用すればよい。 In the present invention, conventionally known methods for producing grain-oriented electrical steel sheets may be applied except for the above-described steps and production conditions.
〔実施例１〕
mass％で、Ｃ：0.062％、Si：3.32％、Mn：0.07％、Se：0.016％、Ｓ：0.002％、sol.Al：0.025％、Ｎ：0.0090％、Sb：0.02％およびＢ：0.00005％を含有し、残部Fe及び不可避不純物からなる成分組成の鋼スラブを連続鋳造にて製造し、1410℃、30分間の加熱後、熱間圧延により板厚：2.1mmの熱延板としたのち、1000℃で熱延板焼鈍を施し、酸洗した。ついで、１回目の冷間圧延を行った後、1100℃の温度で中間焼鈍を施し、２回目の冷間圧延を220℃の温度での温間圧延として板厚：0.23mmに仕上げた。
[Example 1]
In mass%, C: 0.062%, Si: 3.32%, Mn: 0.07%, Se: 0.016%, S: 0.002%, sol.Al: 0.025%, N: 0.0090%, Sb: 0.02% and B: 0.00005 % The steel slab of the component composition comprising the balance Fe and inevitable impurities is produced by continuous casting, and after heating for 30 minutes at 1410 ° C., the hot rolled sheet is formed into a hot rolled sheet having a thickness of 2.1 mm, Hot rolled sheet annealing was performed at 1000 ° C. and pickled. Next, after the first cold rolling, intermediate annealing was performed at a temperature of 1100 ° C., and the second cold rolling was finished as a warm rolling at a temperature of 220 ° C. to a sheet thickness of 0.23 mm.
ついで、この冷延板に湿水素雰囲気中、830℃の脱炭焼鈍を施したのち、表１に記載の条件で、焼鈍分離剤を塗布して仕上げ焼鈍を実施した。ここで、仕上げ焼鈍の昇温過程において、850℃で30時間の保定処理を行い、保定終了までは窒素雰囲気を導入した。続く850〜1180℃の温度領域においては、雰囲気を表１に記載のとおりとし、昇温速度：10℃/ｈで昇温し、1180℃に到達した時点で100％Ｈ2雰囲気に切り替えを行い、５時間の保定を行った。
仕上げ焼鈍後、平坦化焼鈍を行い、同時にコロイダルシリカとリン酸マグネシウムからなる絶縁コーティングを塗布した。最後に、磁区細分化処理としてビーム径：0.3mm、出力：100WのYAGレーザーを圧延方向と直角に、100μｍ幅、５mm間隔、スキャン速度：10m/sで照射し、製品板とした。かくして得られた製品板で1200kVAの３相３脚トランスを作製し、トランス鉄損と騒音を測定した。
上記製品板のフォルステライト被膜中のTi、Ｂ、Ｎ量並びにフォルステライト被膜の剥離率、鉄損および騒音量の測定結果を表２に示す。なお、剥離率は線分法により、鋼板1000ｍにつき、レーザ照射部の中心線に沿って、任意の位置の10ｃｍ長さのレーザ照射部をサンプリングし、評価することで求めた。
Next, the cold-rolled sheet was decarburized and annealed at 830 ° C. in a wet hydrogen atmosphere, and then annealed by applying an annealing separator under the conditions shown in Table 1. Here, in the temperature raising process of finish annealing, a holding treatment was performed at 850 ° C. for 30 hours, and a nitrogen atmosphere was introduced until the holding was completed. In the following temperature range of 850 to 1180 ° C, the atmosphere is as shown in Table 1. The temperature is increased at a rate of 10 ° C / h, and when it reaches 1180 ° C, the atmosphere is switched to 100% H 2 atmosphere. It was held for 5 hours.
After finish annealing, flattening annealing was performed, and at the same time, an insulating coating composed of colloidal silica and magnesium phosphate was applied. Finally, as a magnetic domain fragmentation treatment, a YAG laser beam having a beam diameter of 0.3 mm and an output of 100 W was irradiated perpendicularly to the rolling direction at a width of 100 μm, an interval of 5 mm, and a scanning speed of 10 m / s to obtain a product plate. A 1200 kVA three-phase three-leg transformer was produced from the product plate thus obtained, and transformer iron loss and noise were measured.
Table 2 shows the results of measurement of the amount of Ti, B, and N in the forsterite film of the product plate, the peeling rate of the forsterite film, the iron loss, and the amount of noise. The peeling rate was obtained by sampling and evaluating a 10 cm long laser irradiated portion at an arbitrary position along the center line of the laser irradiated portion per 1000 m of steel plate by a line segment method.
表２に示したとおり、レーザーによる磁区細分化処理を施し、本発明の範囲のTi、Ｂ量および、これらの被膜中Ｎに対する物質量比（Ti＋Ｂ）/Ｎを満足するフォルステライト被膜を有している方向性電磁鋼板を用いると、実機トランスの騒音は低く、極めて良好な鉄損特性が得られている。しかしながら、本発明の範囲を逸脱した方向性電磁鋼板を用いた実機トランスは、低騒音および低鉄損のいずれかまたは両立が得られていない。 As shown in Table 2, subjected to magnetic domain refining treatment by laser, Ti in the range of the present invention, B content and has these things weight ratio in N film (Ti + B) / N forsterite film which satisfies When the grain-oriented electrical steel sheet is used, the noise of the actual transformer is low and extremely good iron loss characteristics are obtained. However, the actual transformer using the grain-oriented electrical steel sheet that deviates from the scope of the present invention does not achieve either low noise and low iron loss or both.
〔実施例２〕
表３に示す成分組成を有し、残部Fe及び不可避不純物から成る鋼スラブを連続鋳造にて製造し、1380℃、１時間の加熱後、熱間圧延により板厚：1.8mmの熱延板としたのち、1000℃の温度で熱延板焼鈍を施し、酸洗して、１回目の冷間圧延を行った後、1150℃の温度で中間焼鈍を施し、２回目の冷間圧延を200℃の温度での温間圧延として板厚：0.23mmに仕上げた。
[Example 2]
A steel slab having the composition shown in Table 3 and comprising the remainder Fe and inevitable impurities is manufactured by continuous casting, heated at 1380 ° C. for 1 hour, and then hot rolled to obtain a hot rolled sheet having a thickness of 1.8 mm. After that, hot-rolled sheet annealing was performed at a temperature of 1000 ° C., pickled, and after the first cold rolling, intermediate annealing was performed at a temperature of 1150 ° C., and the second cold rolling was performed at 200 ° C. Finished to a thickness of 0.23 mm as warm rolling at a temperature of.
ついで、湿水素雰囲気中、830℃の脱炭焼鈍を施したのち、0.1mass％のＢを含むMgO：100質量部に対してTiO2：８質量部を混合した焼鈍分離剤を、目付量（両面）：13g/m2で塗布し、仕上げ焼鈍を実施した。ここで、仕上げ焼鈍の昇温中、850℃以下の温度領域においては雰囲気をＮ2：Ar=50：50のＮ2,Ar混合ガスとし、850〜1200℃の温度領域においては、雰囲気をＮ2：Ｈ2=30：70のＮ2,Ｈ2混合ガスとして昇温速度：14℃/ｈで昇温し、1200℃に到達した時点で100％Ｈ2雰囲気に切り替えを行い、３時間の保定を行った。仕上げ焼鈍後、平坦化焼鈍を行い、同時にコロイダルシリカとリン酸マグネシウムからなる絶縁コートを塗布した。最後に、磁区細分化処理としてビーム径：0.3mm、出力：100WのYAGレーザーを圧延方向と直角に、100μｍ幅、５mm間隔、スキャン速度：10m/sで照射し、製品板とした。かくして得られた製品板で1200kVAの３相３脚トランスを作製し、トランス鉄損と騒音を調査した。
上記製品板のフォルステライト被膜中のTi、Ｂ、Ｎ量並びにフォルステライト被膜の剥離率、鉄損および騒音量の測定結果を表４に示す。なお、剥離率は、実施例１と同じく、線分法を用い、10ｃｍの範囲について評価して求めた。
Next, after performing decarburization annealing at 830 ° C. in a wet hydrogen atmosphere, an annealing separator obtained by mixing 8 parts by mass of TiO 2 with 100 parts by mass of MgO containing 0.1 mass% B ( Both sides): Coating was performed at 13 g / m 2 and finish annealing was performed. Here, during the temperature increase of the finish annealing, the atmosphere is N 2 : Ar = 50: 50 N 2 and Ar mixed gas in the temperature range of 850 ° C. or lower, and the atmosphere is N in the temperature range of 850 to 1200 ° C. 2 : H 2 = 30: 70 as N 2 , H 2 mixed gas, heating rate is 14 ° C / h, and when it reaches 1200 ° C, it is switched to 100% H 2 atmosphere for 3 hours. Baoding was performed. After finish annealing, flattening annealing was performed, and at the same time, an insulating coat made of colloidal silica and magnesium phosphate was applied. Finally, as a magnetic domain fragmentation treatment, a YAG laser beam having a beam diameter of 0.3 mm and an output of 100 W was irradiated perpendicularly to the rolling direction at a width of 100 μm, an interval of 5 mm, and a scanning speed of 10 m / s to obtain a product plate. A 1200 kVA three-phase, three-leg transformer was fabricated from the product plate thus obtained, and the transformer iron loss and noise were investigated.
Table 4 shows the measurement results of the amount of Ti, B, and N in the forsterite film of the product plate, the peel rate of the forsterite film, the iron loss, and the amount of noise. The peel rate was obtained by evaluating the range of 10 cm using the line segment method as in Example 1.
表４に示したとおり、レーザーによる磁区細分化処理を施し、本発明の範囲のTi、Ｂ量および、これらの被膜中Ｎに対する物質量比（Ti＋Ｂ）/Ｎを満足するフォルステライト被膜を有している方向性電磁鋼板を用いると、実機トランスの騒音は低く、極めて良好な鉄損特性が得られている。しかしながら、本発明の範囲を逸脱した方向性電磁鋼板を用いた実機トランスは、特に低騒音が得られていない。
As shown in Table 4, subjected to magnetic domain refining treatment by laser, Ti in the range of the present invention, B content and has these things weight ratio in N film (Ti + B) / N forsterite film which satisfies When the grain-oriented electrical steel sheet is used, the noise of the actual transformer is low and extremely good iron loss characteristics are obtained. However, the actual transformer using the grain-oriented electrical steel sheet that departs from the scope of the present invention does not have particularly low noise.
Claims (2)
(1) 上記焼鈍分離剤中に、該焼鈍分離剤中のMgO：100質量部に対してTiO2：１〜30質量部を含有させる、
(2) 上記焼鈍分離剤の鋼板表面に対する塗布量を、目付量（両面）で８〜20g/m2とする、
(3) 上記焼鈍分離剤中のＢと鋼中のＢの合計量が鋼質量に対して0.0002〜0.002mass％の範囲とする、
(4) 上記最終仕上げ焼鈍を、窒素濃度が15vol％以上の非酸化性雰囲気中にて、1050℃以上、２時間以上の条件で行う、
(5) ついで、窒素濃度が２vol%以下の水素雰囲気中にて、1150〜1250℃の温度範囲に少なくとも２時間保持する
ことを特徴とする方向性電磁鋼板の製造方法。 The slab for grain-oriented electrical steel sheet is hot-rolled and then subjected to hot-rolled sheet annealing as necessary, and then cold-rolled at least once with one or more intermediate annealings to the final thickness. Then, after decarburization annealing, and then applying an annealing separator mainly composed of MgO to the steel sheet surface, after final finishing annealing, the direction of the magnetic domain is subdivided by laser irradiation. When manufacturing electrical steel sheets,
(1) In the annealing separator, TiO 2 : 1 to 30 parts by mass with respect to 100 parts by mass of MgO in the annealing separator,
(2) The amount of the annealing separator applied to the steel sheet surface is 8 to 20 g / m 2 in basis weight (both sides).
(3) The total amount of B in the annealing separator and B in the steel is in the range of 0.0002 to 0.002 mass% with respect to the steel mass.
(4) The final finish annealing is performed in a non-oxidizing atmosphere with a nitrogen concentration of 15 vol% or more under conditions of 1050 ° C. or more and 2 hours or more.
(5) Next, a method for producing a grain-oriented electrical steel sheet, wherein the steel sheet is kept in a temperature range of 1150 to 1250 ° C. for at least 2 hours in a hydrogen atmosphere having a nitrogen concentration of 2 vol% or less.
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