JPH0617132A - Ultra-low iron loss grain oriented electrical steel sheet with extremely high magnetic flux density and method of manufacturing the same - Google Patents

Ultra-low iron loss grain oriented electrical steel sheet with extremely high magnetic flux density and method of manufacturing the same

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Publication number
JPH0617132A
JPH0617132A JP4175790A JP17579092A JPH0617132A JP H0617132 A JPH0617132 A JP H0617132A JP 4175790 A JP4175790 A JP 4175790A JP 17579092 A JP17579092 A JP 17579092A JP H0617132 A JPH0617132 A JP H0617132A
Authority
JP
Japan
Prior art keywords
steel sheet
annealing
magnetic flux
flux density
oriented electrical
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP4175790A
Other languages
Japanese (ja)
Other versions
JP2691828B2 (en
Inventor
Hodaka Honma
穂高 本間
Osamu Tanaka
収 田中
Katsuro Kuroki
克郎 黒木
Hiroaki Masui
浩昭 増井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Corp
Original Assignee
Nippon Steel Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Steel Corp filed Critical Nippon Steel Corp
Priority to JP4175790A priority Critical patent/JP2691828B2/en
Priority to DE69332394T priority patent/DE69332394T2/en
Priority to KR93012299A priority patent/KR960009170B1/en
Priority to EP93110517A priority patent/EP0577124B1/en
Publication of JPH0617132A publication Critical patent/JPH0617132A/en
Priority to US08/257,765 priority patent/US5507883A/en
Application granted granted Critical
Publication of JP2691828B2 publication Critical patent/JP2691828B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/14766Fe-Si based alloys
    • H01F1/14775Fe-Si based alloys in the form of sheets
    • H01F1/14783Fe-Si based alloys in the form of sheets with insulating coating

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)

Abstract

(57)【要約】 【目的】 本発明は、グラス被膜を有さず、かつ磁束密
度が極めて高い、加工性の良好な超低鉄損方向性電磁鋼
板及びその製造方法に関する。 【構成】 一次再結晶焼鈍後の鋼板を仕上焼鈍するにあ
たり、MgO100重量部に対してLi、K、Na、B
a、Ca、Mg、Zn、Fe、Zr、Sr、Sn、Al
等の塩化物、炭酸塩、硝酸塩、硫酸塩、硫化物の中から
選ばれる1種又は2種以上を2〜30重量部添加した焼
鈍分離剤を用い、仕上焼鈍時の昇温速度を10℃/hr
以下、雰囲気をN2 30%以上のN2 +H2 とし、次い
で、レーザー、歯形ロール、プレス、ケガキ、局部エッ
チング等により圧延方向に対し45〜90°の方向に線
状または点状キズを付与する。この時、一次再結晶焼鈍
後の鋼板の一次再結晶粒のうち、平均粒径の2倍を超え
る一次再結晶粒を10%未満とする。
(57) [Summary] [Object] The present invention relates to an ultra-low iron loss grain-oriented electrical steel sheet having no glass coating and having an extremely high magnetic flux density and good workability, and a method for producing the same. [Structure] When finish annealing a steel sheet after primary recrystallization annealing, Li, K, Na, B is added to 100 parts by weight of MgO.
a, Ca, Mg, Zn, Fe, Zr, Sr, Sn, Al
, Etc., using an annealing separator containing 2 to 30 parts by weight of one or more selected from chlorides, carbonates, nitrates, sulfates, sulfides, etc., and the temperature rising rate during finish annealing is 10 ° C. / Hr
Hereinafter, the atmosphere is set to N 2 + H 2 of 30% or more of N 2 , and then linear or dotted scratches are imparted in a direction of 45 to 90 ° with respect to the rolling direction by laser, tooth profile roll, press, scribing, local etching, etc. To do. At this time, of the primary recrystallized grains of the steel sheet after the primary recrystallization annealing, the primary recrystallized grains that exceed twice the average grain size are less than 10%.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、グラス被膜(フォルス
テライト被膜)を有しない方向性電磁鋼板、特に切断
性、打ち抜き性等の加工性に著しく優れた高磁束密度超
低鉄損方向性電磁鋼板とその製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a grain-oriented electrical steel sheet having no glass coating (forsterite coating), especially a high magnetic flux density ultra-low iron loss grain-oriented electromagnetic material which is remarkably excellent in workability such as cutting property and punching property. The present invention relates to a steel plate and a manufacturing method thereof.

【0002】[0002]

【従来の技術】方向性電磁鋼板は、一般に軟磁性材料と
して、主としてトランスその他の電気機器の鉄心として
使用されるもので、磁気特性として、励磁特性と鉄損特
性が良好であることが要求される。良好な磁気特性を得
るためには、磁化容易軸である<001>軸を圧延方向
に高度に揃えることが重要である。また、板厚、結晶粒
度、固有抵抗、被膜なども磁気特性に大きな影響を与え
るため重要である。
2. Description of the Related Art Grain-oriented electrical steel sheets are generally used as a soft magnetic material, mainly as an iron core of transformers and other electric equipment, and are required to have good magnetic excitation characteristics and iron loss characteristics. It In order to obtain good magnetic properties, it is important to highly align the <001> axis, which is the easy magnetization axis, with the rolling direction. Further, the plate thickness, the grain size, the specific resistance, the coating, etc. have a great influence on the magnetic properties, and are important.

【0003】結晶の方向性については、AlN、MnS
をインヒビターとして利用した高圧下最終冷延を特徴と
する方法により大幅に向上し、現在では磁束密度が理論
値に近いものまで製造されるようになってきた。一方、
方向性電磁鋼板の需要家における使用時に、磁気特性と
共に重要なのは被膜に起因する加工性である。通常、方
向性電磁鋼板は最終仕上焼鈍時に形成するグラス被膜と
絶縁被膜の二層被膜によって表面が処理されている。グ
ラス被膜は焼鈍分離剤のMgOと脱炭焼鈍時に形成する
SiO2 の反応生成物であるフォルステライト(Mg2
SiO4 )が主成分の被膜である。このセラミック被膜
は硬質で摩耗性が強く、電磁鋼板加工時のスリット、切
断、打ち抜きなどの工具類の耐久性に著しい悪影響を及
ぼす。例えば、グラス被膜を有する方向性電磁鋼板の打
ち抜き加工を行う場合には、金型の摩耗が生じ、数千回
程度の打ち抜きによって、打ち抜いたときにシートの返
りが大きくなり、使用時に問題が生じる程の返りが生じ
る。このため、金型の再研磨、新品との取り替えが必要
になる。これは、需要家における鉄心加工時の作業能率
を低下させ、またコスト上昇を招く結果になる。また、
電磁鋼板自体の磁気特性に対しては、たしかに被膜張力
による鉄損の改善効果があるが、形成状態によっては被
膜厚みの増加などによって、非磁性体による磁束密度の
低下の問題がある。このため、鋼板板厚の厚い材料のよ
うに被膜張力による鉄損改善効果が期待できないような
材料や、他の手段で磁区細分化を行い、鉄損が改善でき
るケース等では、むしろ前記問題からグラス被膜を有し
ない方向性電磁鋼板が望まれる。
Regarding the crystal orientation, AlN, MnS
It has been significantly improved by a method characterized by final cold rolling under high pressure using as an inhibitor, and now the magnetic flux density is close to the theoretical value. on the other hand,
When used in the consumer of grain-oriented electrical steel sheets, what is important along with magnetic properties is workability due to the coating. Usually, the grain-oriented electrical steel sheet is treated on its surface with a two-layer coating consisting of a glass coating and an insulating coating formed during final finishing annealing. The glass film is a reaction product of MgO which is an annealing separator and SiO 2 which is formed during decarburization annealing and is forsterite (Mg 2
SiO 4 ) is the main film. This ceramic coating is hard and has strong wear resistance, and has a significant adverse effect on the durability of tools such as slits, cutting and punching when processing electromagnetic steel sheets. For example, in the case of punching a grain-oriented electrical steel sheet having a glass coating, the die wears, and the punch returns a large number of times when punched, resulting in problems during use. A certain degree of return will occur. Therefore, it is necessary to re-polish the mold and replace it with a new one. This results in a reduction in the work efficiency of the customer when processing the iron core and an increase in cost. Also,
Although the magnetic properties of the electromagnetic steel sheet itself have an effect of improving iron loss due to the film tension, there is a problem that the magnetic flux density decreases due to the non-magnetic material due to an increase in the film thickness depending on the formation state. For this reason, in the case where the iron loss improvement effect due to the film tension cannot be expected, such as a thick steel plate material, or in the case where the magnetic loss can be improved by subdividing the magnetic domain by other means, etc. A grain-oriented electrical steel sheet without a glass coating is desired.

【0004】とりわけ、近年では磁区細分化技術とし
て、光学的、機械的、化学的な手段による技術が発達
し、グラス被膜の張力なしでも鉄損の改善が得られるよ
うになり、むしろグラス被膜を有しない方向性電磁鋼板
の方が磁化の際の時壁移動のピンニング現象を起こすグ
ラス被膜の内部酸化層等の悪影響がないため有利である
ことも解ってきた。このためグラス被膜を有しない高磁
束密度方向性電磁鋼板の開発は需要家での種々の使用条
件を考える際に重要で、ニーズが高まっている。
In particular, in recent years, as a magnetic domain subdivision technique, a technique developed by optical, mechanical and chemical means has been developed so that iron loss can be improved without the tension of the glass coating. It has also been found that the grain-oriented electrical steel sheet that does not have the advantage is advantageous because it does not have an adverse effect such as the internal oxide layer of the glass coating that causes the pinning phenomenon of wall movement during magnetization. Therefore, the development of a high magnetic flux density grain-oriented electrical steel sheet without a glass coating is important when considering various usage conditions in the consumer, and needs are increasing.

【0005】とりわけ、現在、方向性電磁鋼板に代わる
軟磁性材料として、非晶質合金がクローズアップされて
いるが、磁束密度が低い、占積率が低い、加工性が劣悪
等、実用化に際して様々な困難に直面している。従っ
て、鉄損特性において非晶質合金と対抗し得る方向性電
磁鋼板を開発するために、グラス被膜を有しない材料を
開発することが重要となってきている。
At present, amorphous alloys are currently being used as a soft magnetic material to replace grain-oriented electrical steel sheets. However, in practical applications, such as low magnetic flux density, low space factor, and poor workability. We are facing various difficulties. Therefore, in order to develop a grain-oriented electrical steel sheet that can counter an amorphous alloy in iron loss characteristics, it has become important to develop a material having no glass coating.

【0006】グラス被膜を有しない方向性電磁鋼板の製
造方法としては、例えば特開昭53−22113号公報
に開示のものがある。これは、脱炭焼鈍において酸化膜
の厚みを3μm以下とし、焼鈍分離剤として含水珪酸塩
鉱物粉末を5〜40%含有する微粒子のアルミナを用
い、これを鋼板に塗布し、仕上焼鈍することからなる。
この方法によると、酸化膜を薄くし、さらに含水珪酸塩
鉱物の配合によって、剥離し易いグラス被膜が形成さ
れ、金属光沢を有するものが得られるとされている。焼
鈍分離剤によりグラス被膜の形成を抑制する方法として
は、特開昭56−65983号公報に示されるように、
水酸化アルミニウム不純物除去用添加物20重量部、抑
制物質10重量部を配合した焼鈍分離剤を鋼板に塗布
し、0.5μm以下の薄いグラス被膜を形成する方法が
ある。また、特開昭59−96278号公報には、脱炭
焼鈍で形成した酸化層のSiO2 との反応が弱いAl2
3 と、1300℃以上の高温で焼成し、活性を低下さ
せたMgOとからなる焼鈍分離剤が提案されている。こ
の焼鈍分離剤によると、フォルステライトの形成が抑制
されるというものである。
[0006] As a method for producing a grain-oriented electrical steel sheet having no glass coating, for example, there is one disclosed in JP-A-53-22113. This is because the decarburization annealing has a thickness of an oxide film of 3 μm or less, and fine particles of alumina containing 5 to 40% of hydrous silicate mineral powder are used as an annealing separator, which is applied to a steel sheet and finish annealed. Become.
According to this method, it is said that an oxide film is thinned and a glass coating film that is easily peeled off is formed by adding a hydrous silicate mineral, and a glass film having a metallic luster is obtained. As a method for suppressing the formation of a glass film by using an annealing separator, as disclosed in JP-A-56-65983,
There is a method in which an annealing separator containing 20 parts by weight of an additive for removing impurities of aluminum hydroxide and 10 parts by weight of an inhibitor is applied to a steel sheet to form a thin glass film of 0.5 μm or less. Further, in Japanese Patent Laid-Open No. 59-96278, Al 2 which has a weak reaction with SiO 2 in an oxide layer formed by decarburization annealing.
An annealing separator composed of O 3 and MgO whose activity has been reduced by firing at a high temperature of 1300 ° C. or higher has been proposed. According to this annealing separator, the formation of forsterite is suppressed.

【0007】これらの先行技術は、いずれも通常のオリ
エントコアと呼ばれる磁束密度がB 8 値で1.88T以
下と低く、従って鉄損値も高い低級な方向性電磁鋼板を
ベースとする技術であり、本発明のように、超低鉄損を
実現するための条件を満たす方向性電磁鋼板を安定して
得る技術を開発するには至っていない。
All of these prior arts are conventional orientations.
The magnetic flux density called the ent core is B 8Value of 1.88T or less
A low-grade grain-oriented electrical steel sheet with a low bottom and therefore a high iron loss value
It is a technology based on the ultra low iron loss as in the present invention.
Stable grain oriented electrical steel sheets that meet the requirements for realization
The technology to gain is not yet developed.

【0008】[0008]

【発明が解決しようとする課題】本発明は、打ち抜き
性、スリット性、切断性等が極めて優れた、ほぼ均一に
グラス被膜のない高磁束密度超低鉄損方向性電磁鋼板及
び該鋼板を工業的に安価に製造する方法を提供すること
を目的とする。
DISCLOSURE OF THE INVENTION The present invention provides a high magnetic flux density ultra-low iron loss grain-oriented electrical steel sheet which is excellent in punching property, slitting property, cutting property, etc. and has a substantially uniform glass coating, and an industrial steel sheet. It is an object of the present invention to provide a method of economically manufacturing.

【0009】[0009]

【課題を解決するための手段】本発明の要旨とするとこ
ろは下記のとおりである。 (1) 重量で、Si:1.0〜7.0%を含み、鋼板
の金属表面から15μm内に分布する内部酸化層の量
が、当該厚み領域内の酸素含有量で1%以下であり、B
8 ≧1.93Tである磁束密度の極めて高い超低鉄損方
向性電磁鋼板。
The subject matter of the present invention is as follows. (1) By weight, the amount of the internal oxide layer containing Si: 1.0 to 7.0% and distributed within 15 μm from the metal surface of the steel sheet is 1% or less in terms of the oxygen content in the thickness region. , B
Ultra low iron loss grain-oriented electrical steel sheet with extremely high magnetic flux density of 8 ≧ 1.93T.

【0010】(2) 表面に線状または点状キズが圧延
方向から45〜90度の方向に、2〜15mmの間隔で
付与されている請求項1記載の磁束密度の極めて高い超
低鉄損方向性電磁鋼板。 (3) 重量で、Si:1.0〜7.0%、酸可溶性A
l:0.010〜0.070%を含有し、残部がFe及
び不可避的不純物からなる鋼塊あるいはスラブを、熱延
し、冷延し、一次再結晶焼鈍し、焼鈍分離剤を塗布した
後、高温仕上焼鈍を行い、ヒートフラットニングを行う
ことによって方向性電磁鋼板を製造する方法において、
前記一次再結晶焼鈍後の鋼板の一次再結晶粒のうち粒径
が平均粒径の2倍を超えるものが10%未満であるよう
に調整し、同鋼板に焼鈍分離剤として、MgO100重
量部に対してLi、K、Na、Ba、Ca、Mg、Z
n、Fe、Zr、Sn、Sr、Alの塩化物、炭酸塩、
硝酸塩、硫酸塩、硫化物の中から選ばれる1種又は2種
以上を2〜30重量部添加したものを塗布し、高温仕上
焼鈍時の昇温速度を、950〜1150℃の間で、10
℃/hr以下とし、かつ焼鈍雰囲気を少なくともN2
0%以上のN2 +H2 とすることを特徴とする磁束密度
の極めて高い超低鉄損方向性電磁鋼板の製造方法。
(2) An ultra-low iron loss having an extremely high magnetic flux density according to claim 1, wherein linear or dot-like scratches are provided on the surface in the direction of 45 to 90 degrees from the rolling direction at intervals of 2 to 15 mm. Grain-oriented electrical steel sheet. (3) Si: 1.0 to 7.0% by weight, acid-soluble A
After the hot rolling, cold rolling, primary recrystallization annealing, and application of the annealing separator, a steel ingot or slab containing 1: 0. 10 to 0.070% and the balance Fe and unavoidable impurities , In a method of producing a grain-oriented electrical steel sheet by performing high temperature finish annealing and heat flattening,
Of the primary recrystallized grains of the steel sheet after the primary recrystallization annealing, those having a grain size of more than twice the average grain size were adjusted to be less than 10%, and the same steel sheet was treated with 100 parts by weight of MgO as an annealing separator. In contrast, Li, K, Na, Ba, Ca, Mg, Z
n, Fe, Zr, Sn, Sr, Al chlorides, carbonates,
2 to 30 parts by weight of one or more selected from nitrates, sulfates and sulfides is applied, and the temperature rising rate at the time of high temperature finish annealing is 10 to 90 ° C. at 950 to 1150 ° C.
C./hr or less and the annealing atmosphere is at least N 2 3
A method for producing an ultra-low iron loss grain-oriented electrical steel sheet having an extremely high magnetic flux density, which is characterized in that N 2 + H 2 is 0% or more.

【0011】(4) 重量で、Si:1.0〜7.0
%、酸可溶性Al:0.010〜0.070%、C:
0.021〜0.075%、N:0.003〜0.01
30%、S≦0.030%、Mn:0.05〜0.45
%を含有し、残部がFe及び不可避的不純物からなるス
ラブの熱延前の加熱を、1280℃未満の温度で行い、
一次再結晶完了後、高温仕上焼鈍の二次再結晶開始前の
間で窒化することを特徴とする前項3記載の磁束密度の
極めて高い超低鉄損方向性電磁鋼板の製造方法。
(4) Si: 1.0 to 7.0 by weight
%, Acid-soluble Al: 0.010 to 0.070%, C:
0.021 to 0.075%, N: 0.003 to 0.01
30%, S ≦ 0.030%, Mn: 0.05 to 0.45
%, With the balance being Fe and unavoidable impurities, the slab being heated before hot rolling at a temperature below 1280 ° C.,
The method for producing an ultra-low iron loss grain-oriented electrical steel sheet with extremely high magnetic flux density according to the above item 3, wherein nitriding is performed after the completion of primary recrystallization and before the start of secondary recrystallization of high temperature finish annealing.

【0012】(5) ヒートフラットニングの前又は後
に、レーザー、歯形ロール、プレス、ケガキ、局部エッ
チング等の局部加工により鋼板表面に線状または点状キ
ズを付与することを特徴とする前項3又は4記載の磁束
密度の極めて高い超低鉄損方向性電磁鋼板の製造方法。 以下、本発明を詳細に説明する。
(5) Before or after the heat flattening, a linear or dot-like flaw is imparted to the surface of the steel sheet by local processing such as laser, tooth profile roll, press, scribe, local etching, or the like. 4. The method for manufacturing an ultra-low iron loss grain-oriented electrical steel sheet according to 4, which has an extremely high magnetic flux density. Hereinafter, the present invention will be described in detail.

【0013】本発明の高磁束密度超低鉄損方向性電磁鋼
板の製造工程では、スラブ加熱段階ではインヒビター元
素、例えばAl、N、Mn、S等の鋼中への溶解を完全
に行わず、脱炭焼鈍後、材料を強還元雰囲気中で窒化処
理をすることによって(Al、Si)Nを主成分とする
インヒビターを形成させ、仕上焼鈍過程で良好な二次再
結晶を発達させた後、磁区細分化することを基本工程と
する。
In the process for producing the high magnetic flux density ultra-low iron loss grain oriented electrical steel sheet of the present invention, the inhibitor elements such as Al, N, Mn and S are not completely dissolved in the steel during the slab heating step, After decarburization annealing, the material is subjected to a nitriding treatment in a strong reducing atmosphere to form an inhibitor containing (Al, Si) N as a main component, and good secondary recrystallization is developed in the finish annealing process. The basic process is to subdivide the magnetic domains.

【0014】前記した成分組成の出発材と工程による本
発明のグラス被膜を有しない高磁束密度方向性電磁鋼板
を得る方法においては、脱炭焼鈍〜仕上焼鈍過程での処
理方法に特徴がある。最終板厚に冷間圧延された素材
は、連続ラインにおいて脱炭焼鈍される。この脱炭焼鈍
により鋼中のCの除去と一次再結晶が行われ、同時に鋼
板表面にSiO 2 を主成分とする酸化膜の形成が行われ
る。脱炭焼鈍は、800〜875℃の温度で、雰囲気は
2 +H2 中で露点をコントロールして行われる。次い
で脱炭焼鈍の後半あるいは終了後、若しくはこれらの両
段階において、同一ライン又は別に設けたラインで窒化
処理が行われる。この際に生じた窒化物は、インヒビタ
ーとして最終仕上焼鈍時に二次再結晶を発現させる。
Books based on the starting materials and processes of the above-mentioned composition
High magnetic flux density grain-oriented electrical steel sheet without glass coating of the invention
In the method of obtaining the
There is a characteristic in the method of processing. Material cold rolled to final plate thickness
Is decarburized and annealed in a continuous line. This decarburization annealing
Removes C in the steel and performs primary recrystallization.
SiO on the plate surface 2The oxide film mainly composed of
It The decarburization annealing is performed at a temperature of 800 to 875 ° C., and the atmosphere is
N2+ H2It is performed by controlling the dew point inside. Next
In the latter half or after the decarburization annealing, or both
Nitriding on the same line or on a separate line at the stage
Processing is performed. The nitride generated at this time is
As a result, secondary recrystallization is developed during final finish annealing.

【0015】この後、焼鈍分離剤を塗布し、乾燥して巻
き取り、最終仕上焼鈍される。この際の焼鈍分離剤の組
成は、グラス被膜の形成制御や分解反応に重要な役割を
持つ。本発明に用いる焼鈍分離剤としては、MgOを主
成分として、添加剤として、Li、K、Na、Ba、C
a、Mg、Zn、Fe、Zr、Sn、Sr、Al等の塩
化物、炭酸塩、硝酸塩、硫酸塩、硫化物の1種又は2種
以上を2〜30重量部用いる。
After that, an annealing separator is applied, dried, wound, and finally finish annealed. The composition of the annealing separator at this time plays an important role in controlling the formation of the glass film and in the decomposition reaction. The annealing separator used in the present invention contains MgO as a main component, and Li, K, Na, Ba, C as additives.
2 to 30 parts by weight of one or more of chlorides, carbonates, nitrates, sulfates, sulfides such as a, Mg, Zn, Fe, Zr, Sn, Sr, and Al are used.

【0016】本発明において焼鈍分離剤と共に重要なの
は第三の要素技術である最終仕上焼鈍の条件である。本
発明者らは、本発明のようにインヒビターとして(A
l、Si)Nを用い、焼鈍分離剤と最終仕上焼鈍条件に
よってグラス被膜の形成制御、分解反応を起こさせる工
程を採る場合においては、焼鈍雰囲気条件が二次再結晶
の安定化と高磁束密度化に重要な要素となることを膨大
な実験と研究の結果つきとめた。
What is important in the present invention together with the annealing separator is the condition of the final finish annealing which is the third elemental technique. The present inventors have found that as an inhibitor (A
In the case of adopting the steps of controlling the formation of the glass film and causing the decomposition reaction by using the annealing separator and the final finishing annealing condition, the annealing atmosphere condition is the stabilization of the secondary recrystallization and the high magnetic flux density. As a result of enormous experiments and research, we have determined that it will be an important factor for the realization.

【0017】即ち、本発明のように、(Al、Si)N
系のインヒビターを利用する工程においては、二次再結
晶開始温度領域までグラス被膜形成の制御、分解反応を
行いながらインヒビターの強度を一定レベルに保つ必要
がある。これは、焼鈍分離剤によって、一旦グラス被膜
の形成が始まり、次いで分解反応を誘起する工程では、
グラス被膜の分解反応が開始する時期から鋼中のインヒ
ビターの分解が急速に進行するからである。このため、
本発明のように、特定条件下で仕上焼鈍を行わないと、
良好な二次再結晶と高磁束密度が得られない。仕上焼鈍
条件としては、グラス被膜の分解反応が開始する昇温
時、二次再結晶が開始・進行するときの雰囲気を、N2
30%以上として行われる。これにより、二次再結晶進
行時の(Al、Si)Nの分解速度が抑えられ、Gos
s粒成長速度が適正化される。
That is, as in the present invention, (Al, Si) N
In the process of utilizing the system inhibitor, it is necessary to control the glass film formation and carry out the decomposition reaction up to the temperature range of the secondary recrystallization initiation temperature to maintain the inhibitor strength at a constant level. This is because the process of initiating the decomposition of the glass film by the annealing separator once initiating the decomposition reaction,
This is because the decomposition of the inhibitor in the steel rapidly progresses from the time when the decomposition reaction of the glass film starts. For this reason,
As in the present invention, unless finish annealing is performed under specific conditions,
Good secondary recrystallization and high magnetic flux density cannot be obtained. As the finish annealing condition, the atmosphere when the secondary recrystallization starts / progresses at the time of temperature rise at which the decomposition reaction of the glass coating starts, and N 2
It is performed as 30% or more. This suppresses the decomposition rate of (Al, Si) N during the progress of secondary recrystallization,
The grain growth rate is optimized.

【0018】この効果は、昇温速度が遅いとき更に顕著
に現れ、30%以上のN2 分圧と徐加熱が組み合わされ
るときは、極めて高いB8 値が得られるが、N2 分圧が
低いと逆に二次再結晶不良を生じる。仕上焼鈍された鋼
板は形状矯正、歪取焼鈍をかねて連続焼鈍ラインで80
0〜900℃で絶縁被膜剤の焼き付けとヒートフラット
ニングされる。このヒートフラットニングの前又は後
に、レーザー、歯形ロール、プレス、ケガキ、局部エッ
チング等により、深さ5〜50μm、間隔2〜15mm
で圧延方向に対して45〜90度の方向に線条キズまた
は点条キズが導入される。この後、需要家における使用
目的に応じて種々の絶縁被膜剤が塗布され、焼き付け処
理される。
This effect is more remarkable when the temperature rising rate is slow, and when the N 2 partial pressure of 30% or more and the gradual heating are combined, an extremely high B 8 value is obtained, but the N 2 partial pressure is increased. On the contrary, if it is low, secondary recrystallization failure occurs. The finish annealed steel sheet is 80 in a continuous annealing line for shape correction and strain relief annealing.
The insulating coating agent is baked and heat flattened at 0 to 900 ° C. Before or after this heat flattening, the depth is 5 to 50 μm and the distance is 2 to 15 mm by laser, tooth profile roll, press, scribing, local etching, etc.
Thus, linear scratches or dot scratches are introduced in the direction of 45 to 90 degrees with respect to the rolling direction. After that, various insulating coating agents are applied and baked according to the purpose of use in the consumer.

【0019】超低鉄損を実現するための張力被膜を形成
しようとするときは、絶縁被膜剤として、例えば特公昭
53−28375号公報に示されるような、燐酸塩〜コ
ロイダルシリカ系の被膜剤が塗布され、焼き付け処理さ
れる。また、後の需要家での使用工程で良加工性を必要
とする場合には、ヒートフラットニング後の鋼板上に有
機被膜剤又は半有機被膜剤を塗布・焼き付け処理して使
用しても良いし、無機被膜剤を塗布・焼き付け処理した
後、有機系被膜剤を塗布・焼き付け処理して二層被膜を
形成しても良い。有機系被膜剤としては、(1)アクリ
ル、ポリビニル、酢酸ビニル、エポキシ、スチレン等の
樹脂及び/又はこれらの重合体、架橋体の1種又は2種
以上の全有機被膜剤か(2)前記(1)における樹脂と
クロム酸塩、燐酸、燐酸塩、ホウ酸、ホウ酸塩等の1種
又は2種以上の混合物からなる半有機系被膜剤を150
〜450℃の温度で塗布・焼き付け処理して使用する。
In order to form a tension coating film for achieving ultra-low iron loss, a phosphate-colloidal silica coating agent as disclosed in, for example, Japanese Patent Publication No. 53-28375 is used as an insulating coating agent. Is applied and baked. Further, when good workability is required in the subsequent consumer use process, an organic coating agent or a semi-organic coating agent may be applied and baked on the steel plate after heat flattening and used. Then, the inorganic coating agent may be applied and baked, and then the organic coating agent may be applied and baked to form a two-layer coating. The organic coating agent is (1) one or two or more kinds of all organic coating agents of resins such as acrylic, polyvinyl, vinyl acetate, epoxy, styrene and / or polymers and cross-linked products thereof. (2) The above A semi-organic coating agent comprising the resin in (1) and one or a mixture of two or more of chromate, phosphoric acid, phosphate, boric acid, borate and the like is used.
Use by applying and baking at a temperature of ~ 450 ° C.

【0020】これらの有機系被膜剤の塗布・焼き付け処
理により、打ち抜き性、スリット性、切断性等が著しく
改善される。本発明によれば、従来のグラス被膜を有す
る製品の打ち抜き性が、スチールダイスを使用する場合
には5千回程度であるのに対し、グラス被膜を有しない
製品では、無機絶縁被膜剤を塗布・焼き付けした場合、
約10万回、更にこの上に半有機系被膜剤を塗布・焼き
付けした場合には、200万回程度まで打ち抜き性が向
上する。
By applying and baking these organic coating agents, the punching property, slitting property and cutting property are remarkably improved. According to the present invention, the punchability of a conventional product having a glass coating is about 5,000 times when a steel die is used, whereas the product having no glass coating is coated with an inorganic insulating coating agent.・ When baked
When the semi-organic coating agent is applied and baked about 100,000 times, the punchability is improved up to about 2 million times.

【0021】次に、本発明における構成要件の限定理由
に就いて述べる。まず、出発材として使用する電磁鋼ス
ラブの成分組成の限定理由は次の通りである。Cはその
含有量が0.021%未満では、二次再結晶が不安定に
なり、二次再結晶した場合にも製品の磁束密度がB8
1.80T程度と低いものになる。一方、0.075%
超になると、脱炭焼鈍工程に長時間を費やすため、生産
性を阻害する。
Next, the reasons for limiting the constituents of the present invention will be described. First, the reasons for limiting the component composition of the electromagnetic steel slab used as a starting material are as follows. When the content of C is less than 0.021%, the secondary recrystallization becomes unstable, and the magnetic flux density of the product becomes as low as about 1.80 T at B 8 even when the secondary recrystallization is performed. On the other hand, 0.075%
If it exceeds this value, it takes a long time for the decarburization annealing process, which hinders the productivity.

【0022】Siは、その含有量によって固有抵抗が変
化し、多いほど鉄損特性が良好である。1.0%未満の
時、脱炭焼鈍時にSiO2 の酸化層が鋼板表面に形成さ
れにくく、本発明による二次再結晶時の表面シール効果
が得られにくい。Si含有量が7.0%を超えると、最
終製品の靱性が極端に劣化し、実用に耐えない。なお、
超低鉄損の実現のしやすさと言う点では、Si含有量を
2.5%以上として製品の固有抵抗を確保することが望
ましく、生産性の面からは、Si4.5%以下として、
冷間圧延時の割れ、破断防止を低減することが望まし
い。
The specific resistance of Si changes depending on its content, and the larger the content, the better the iron loss characteristics. When it is less than 1.0%, an oxide layer of SiO 2 is difficult to be formed on the surface of the steel sheet during decarburization annealing, and the surface sealing effect at the time of secondary recrystallization according to the present invention is difficult to be obtained. When the Si content exceeds 7.0%, the toughness of the final product is extremely deteriorated and it cannot be put to practical use. In addition,
From the viewpoint of easy realization of ultra-low iron loss, it is desirable to secure the specific resistance of the product by setting the Si content to 2.5% or more, and from the viewpoint of productivity, Si4.5% or less,
It is desirable to reduce cracking and breakage prevention during cold rolling.

【0023】Sは、多すぎると、二次再結晶時のインヒ
ビター強度のバランスが崩れて高B 8 が得られない。
本発明のように、グラスレス二次再結晶を行う場合、ス
ラブ加熱温度が1280℃未満であれば0.030%ま
で添加しても十分高B8 が得られる。Mnは、少なす
ぎるとS偏析による熱延割れを誘起し、多すぎると二次
再結晶時のインヒビターのバランスを崩すと共に、脱炭
焼鈍時の〔O〕付着量を増加させてグラスレス化に悪影
響を及ぼす。斯かる観点から、Mn含有量を0.05〜
0.45%に限定する。
If S is too much, the amount of S during the secondary recrystallization is decreased.
Bitter strength out of balance and high B 8value Can't get
As in the present invention, when performing glassless secondary recrystallization,
If the lab heating temperature is less than 1280 ° C, 0.030% or less
High enough even if added in B8value Is obtained. Mn is small
If it is too large, hot-rolling cracks due to S segregation will be induced, and if too much, secondary
Debalance the inhibitor during recrystallization and decarburize
Poor glasslessness by increasing the [O] adhesion amount during annealing
Make a sound. From this viewpoint, the Mn content is 0.05 to
It is limited to 0.45%.

【0024】本発明では二次再結晶に必要な析出物とし
て(Al、Si)Nを用いる。従って、必要最小限のA
lNを確保するためには、酸可溶Alは0.010%以
上、Nは0.0030%以上必要である。しかしなが
ら、酸可溶Alが0.070%を超えると、純化工程で
Alを含む酸化物が鋼板表面に多量に生成し、鉄損特性
を損なうので0.07%以下とした。一方、Nの含有量
は、0.0130%を超えるとブリスターと呼ばれる鋼
板表面の割れが発生し、また一次再結晶の粒径が調整で
きないため、0.0030〜0.0130%に限定す
る。
In the present invention, (Al, Si) N is used as a precipitate necessary for secondary recrystallization. Therefore, the minimum required A
To secure 1N, 0.010% or more of acid-soluble Al and 0.0030% or more of N are required. However, when the acid-soluble Al exceeds 0.070%, a large amount of oxide containing Al is generated on the surface of the steel sheet in the purification step, and the iron loss characteristics are impaired, so the content was made 0.07% or less. On the other hand, if the content of N exceeds 0.0130%, cracks on the surface of the steel sheet called blister occur, and the grain size of primary recrystallization cannot be adjusted, so it is limited to 0.0030 to 0.0130%.

【0025】最終仕上焼鈍の条件は、本発明のように最
終焼鈍過程でグラス被膜の適正な形成と分解を行う工程
においては非常に重要である。通常、方向性電磁鋼板の
最終仕上焼鈍においては、雰囲気ガスはN2 、H2 或い
はこれらの混合ガスが用いられるが、表面の酸化制御と
コストの問題からN2+H2 が有利である。本発明の場
合、グラスレス化反応の過程の中でインヒビターの強度
を制御するため、昇温中の雰囲気ガスとして少なくとも
2 30%以上のN2 、H2 及び他の不活性ガスから成
る雰囲気が用いられる。N2 分圧が30%未満では、グ
ラスレス化の反応過程で生じる(Al、Si)Nの弱体
化の抑制効果がなく、高磁束密度材が安定して得られな
い。逆にN2 100%のような場合には、MgOの物性
値によっては、鋼板間の酸化度の上昇によって、酸化が
生じて、鋼板表面にむらが生じる傾向があるので、好ま
しくはN2 30〜90%の範囲とする。
The conditions for the final finish annealing are very important in the step of properly forming and decomposing the glass film in the final annealing process as in the present invention. Usually, N 2 or H 2 or a mixed gas of these is used as the atmosphere gas in the final finish annealing of the grain-oriented electrical steel sheet, but N 2 + H 2 is advantageous from the viewpoints of surface oxidation control and cost. For the present invention, for controlling the strength of the inhibitor in the course of a glass-free reaction, consisting of at least N 2 30% or more N 2, H 2 and other inert gas as the atmosphere gas in NoboriAtsushichu atmosphere Is used. When the N 2 partial pressure is less than 30%, there is no effect of suppressing weakening of (Al, Si) N generated in the glassless reaction process, and a high magnetic flux density material cannot be obtained stably. If such a N 2 100% on the contrary, depending on the physical properties of MgO, by increasing the degree of oxidation of between steel plates, to cause oxidation, tend to irregularities on the surface of the steel sheet occurs, preferably N 2 30 ˜90% range.

【0026】仕上焼鈍時の昇温速度は遅いほど高磁束密
度が得られ易く、特に10℃/hr以下の速度で効果が
現れる。一次再結晶粒は、BAF昇温中で二次再結晶を
開始するまでに徐々に成長していく。従って、昇温速度
が遅いときは成長量も大きくなるので、一次再結晶粒径
を小さめに制御しておく必要がある。このとき、仕上焼
鈍中に長時間かけて成長した結晶粒は、粒径分布、集合
組織が二次再結晶に対して適正化されるので、平均結晶
粒径が同じであっても高い磁束密度を得ることができ
る。
The slower the temperature rising rate during finish annealing, the higher the magnetic flux density is likely to be obtained, and the effect is particularly exhibited at a rate of 10 ° C./hr or less. The primary recrystallized grains gradually grow until the secondary recrystallization is started while the BAF temperature is rising. Therefore, when the temperature rising rate is slow, the amount of growth also becomes large, and it is necessary to control the primary recrystallized grain size to be small. At this time, the grain size distribution and texture of the crystal grains grown for a long time during finish annealing are optimized for secondary recrystallization, so even if the average grain size is the same, high magnetic flux density Can be obtained.

【0027】即ち、二次再結晶に際して、最も高いB8
値が得られる最適の平均粒径がある。この平均粒径は、
大きすぎると二次再結晶不良、即ち細粒発生の原因とな
り、小さすぎると方位集積度が不十分で良好な磁気特性
が得られない。ところが、脱炭焼鈍温度を高めて上記最
適な平均粒径を狙うと、粒径分布がなだらかになり、粗
粒が多く発生する。この粗粒は、安定な二次再結晶を阻
害する。これに対して脱炭焼鈍後の結晶粒径を若干低め
にしておき、仕上焼鈍を徐加熱することによって一次再
結晶直後の平均結晶粒径を最適化すると、粒径分布が鋭
くなり、粗粒の発生が抑えられる。その結果高B8値お
よび安定した二次再結晶が得られるのである。実際に本
発明者らが試みた実験によると、実施例の項でも示す
が、平均粒径の二倍以上の大きさを持つ結晶粒の面積率
が10%を超えた場合、平均粒径が最適であっても、二
次再結晶不良を生じた(図2参照)。実際に本発明者ら
が0.15mm厚の材料で試みた実験結果を図1に示
す。昇温速度が早いときには脱炭焼鈍温度が比較的高く
ても(840℃)二次再結晶するが、得られる磁束密度
は低い。一方、徐加熱した場合は、後述のように昇温時
の窒素分圧を適正化(N 2 50%)すれば脱炭焼鈍温度
が低くとも高いB8 が得られている。
That is, in the secondary recrystallization, the highest B8
There is an optimum average particle size for which a value is obtained. This average particle size is
If it is too large, it may cause secondary recrystallization failure, that is, the generation of fine grains.
If it is too small, the orientation integration is insufficient and good magnetic properties are obtained.
Can't get However, by increasing the decarburization annealing temperature,
Aiming at an appropriate average particle size will result in a gradual particle size distribution.
Many grains are generated. This coarse grain prevents stable secondary recrystallization.
Hurt. On the other hand, the grain size after decarburization annealing was slightly reduced.
The primary annealing by gradually heating the finish annealing.
Optimizing the average crystal grain size immediately after crystallization results in a sharp grain size distribution.
And the generation of coarse particles is suppressed. As a result, high B8Value
And stable secondary recrystallization is obtained. Actually books
Experiments conducted by the inventors show that the examples are also shown.
Is the area ratio of crystal grains with a size more than twice the average grain size.
If the average particle size is more than 10%,
Secondary recrystallization failure occurred (see FIG. 2). In fact, the inventors
Fig. 1 shows the experimental results of trials using 0.15mm thick material.
You When the heating rate is fast, the decarburization annealing temperature is relatively high.
Even at (840 ℃) secondary recrystallization occurs, but the obtained magnetic flux density
Is low. On the other hand, when heating slowly,
Nitrogen partial pressure of (N 250%) decarburization annealing temperature
B is low but high8value Has been obtained.

【0028】ところで、本発明のように二次再結晶と被
膜消失が平行するプロセスでは、BAF中窒素分圧が低
いと(Al、Si)Nの分解が急速に進行するので、昇
温速度が遅い時は、一次再結晶粒が成長しすぎてしまっ
て二次再結晶が不安定になる。そこでN2 分圧を高めて
インヒビターの分解を抑えると、一次再結晶粒の成長が
適正化され、極めて高い磁束密度が得られる。特に板厚
が0.17mm以下と薄いときは、N2 分圧を50%以
上とすることが望ましい。また、これらの仕上焼鈍条件
は、少なくとも二次再結晶の開始直前である950℃か
ら、完了する1150℃までの間で満たしていることが
必要である。またさらには、(Al、Si)Nの安定化
に効果のある700℃以上で行うことが望ましい。
By the way, in the process in which the secondary recrystallization and the film disappearance are parallel to each other as in the present invention, if the nitrogen partial pressure in BAF is low, the decomposition of (Al, Si) N proceeds rapidly, so that the temperature rising rate is increased. When it is late, the primary recrystallized grains grow too much and the secondary recrystallization becomes unstable. Therefore, if the N 2 partial pressure is increased to suppress the decomposition of the inhibitor, the growth of the primary recrystallized grains is optimized, and an extremely high magnetic flux density is obtained. Particularly when the plate thickness is as thin as 0.17 mm or less, it is desirable that the N 2 partial pressure be 50% or more. Further, these finish annealing conditions need to be satisfied at least from 950 ° C., which is just before the start of secondary recrystallization, to 1150 ° C., which is complete. Furthermore, it is desirable to carry out at 700 ° C. or higher, which is effective in stabilizing (Al, Si) N.

【0029】以上より、本発明によれば、仕上焼鈍の昇
温速度を遅くすると共にN2 分圧を高め、かつ一次再結
晶直後の粒径を小さくすることによって、高い磁束密度
を得ることができることがわかった。
As described above, according to the present invention, a high magnetic flux density can be obtained by decreasing the temperature rising rate of finish annealing, increasing the N 2 partial pressure, and decreasing the grain size immediately after primary recrystallization. I knew I could do it.

【0030】[0030]

【実施例】Si:3.50%、C:0.054%、M
n:0.14%、S:0.008%、Al:0.029
5%、N:0.073%を含み、残部Feおよび不可避
的不純物からなる鋼を、連続鋳造によってスラブに鋳込
み、1200℃でスラブ加熱を行って熱延した後、焼鈍
し、酸洗後、板厚0.22mmまで冷延し、脱炭焼鈍を
110秒行った。この時、脱炭焼鈍の温度は、830
℃、840℃の2水準を行った。この時の一次再結晶粒
の平均粒径及び平均粒径の2倍を超える粒の割合を図2
に示す。この脱炭焼鈍板に窒化処理を行って〔N〕=2
26ppmとした後、塩化物、炭酸塩、硝酸塩、硫酸塩
などを含む焼鈍分離剤を塗布して仕上焼鈍を行った。高
温仕上焼鈍のサイクルは、図3に示した3条件を行っ
た。こうして得られた二次再結晶板を、連続ラインにお
いて、2.5%硫酸液で80℃×10秒の軽酸洗処理を
行い、50%Al(H2 PO4 3 50kg+30%コ
ロイダルシリカ70kg+CrO3 5kgからなる絶縁
被膜剤を塗布し、850℃×30秒の焼き付けとヒート
フラットニング処理を行った。その後レーザーを用いて
鋼板の圧延方向と直角方向に、間隔5mm、照射幅0.
15mm、照射痕の深さ2.0μmの条件で歪付与処理
を行って最終製品とした。
EXAMPLES Si: 3.50%, C: 0.054%, M
n: 0.14%, S: 0.008%, Al: 0.029
Steel containing 5% and N: 0.073% and the balance Fe and unavoidable impurities was cast into a slab by continuous casting, hot-rolled by heating the slab at 1200 ° C., annealing, pickling, The sheet was cold rolled to a thickness of 0.22 mm and decarburized and annealed for 110 seconds. At this time, the temperature of decarburization annealing is 830
C. and 840.degree. C. were applied at two levels. At this time, the average grain size of the primary recrystallized grains and the ratio of grains exceeding twice the average grain size are shown in FIG.
Shown in. This decarburized annealed sheet was subjected to nitriding treatment [N] = 2.
After adjusting to 26 ppm, an annealing separator containing chloride, carbonate, nitrate, sulfate, etc. was applied to finish annealing. The high temperature finish annealing cycle was performed under the three conditions shown in FIG. The secondary recrystallized plate thus obtained was subjected to a light pickling treatment with a 2.5% sulfuric acid solution at 80 ° C. for 10 seconds in a continuous line to obtain 50% Al (H 2 PO 4 ) 3 50 kg + 30% colloidal silica 70 kg + CrO. An insulation coating agent consisting of 35 kg was applied, followed by baking at 850 ° C. for 30 seconds and heat flattening treatment. Then, using a laser, the interval was 5 mm and the irradiation width was 0.
Straining was performed under the conditions of 15 mm and the depth of the irradiation mark was 2.0 μm to obtain a final product.

【0031】表1に、焼鈍分離剤への添加物の条件の一
覧を、表2に得られた結果を示す。
Table 1 shows a list of conditions for additives to the annealing separator, and Table 2 shows the obtained results.

【0032】[0032]

【表1】 [Table 1]

【0033】[0033]

【表2】 [Table 2]

【0034】本発明例によるものは、いずれも鋼板表面
に酸化物被膜を有さず、グラスレス化が良好であった。
また、仕上焼鈍中の昇温速度を遅くした場合は、N2
圧を高めて脱炭焼鈍温度を低めにすると、極めて高いB
8 値が得られた。
All of the examples according to the present invention did not have an oxide film on the surface of the steel sheet and were excellent in glasslessness.
Also, when the temperature rising rate during finish annealing is slowed, if the N 2 partial pressure is increased and the decarburization annealing temperature is lowered, the B
Eight values were obtained.

【0035】[0035]

【発明の効果】本発明によれば、グラス被膜を有さな
い、磁束密度の極めて高い超低鉄損方向性電磁鋼板、特
に切断性、打ち抜き性等の加工性に著しく優れた高磁束
密度低鉄損方向性電磁鋼板を安価に製造できる。
EFFECTS OF THE INVENTION According to the present invention, an ultra-low iron loss grain oriented electrical steel sheet having no glass coating and having an extremely high magnetic flux density, especially a high magnetic flux density low which is remarkably excellent in workability such as cutting property and punching property. Iron loss direction electrical steel sheet can be manufactured at low cost.

【図面の簡単な説明】[Brief description of drawings]

【図1】板厚0.15mm材で、脱炭焼鈍温度及び仕上
焼鈍サイクルを変えたときの磁束密度変化を示す図であ
る。焼鈍分離剤は、MgO100gに対してCaCl2
5g添加している。
FIG. 1 is a diagram showing a change in magnetic flux density when a decarburization annealing temperature and a finishing annealing cycle are changed for a plate having a thickness of 0.15 mm. The annealing separator is CaCl 2 for 100 g of MgO.
5g is added.

【図2】一次再結晶粒径と脱炭焼鈍温度の関係を示す図
である。
FIG. 2 is a diagram showing a relationship between a primary recrystallized grain size and a decarburization annealing temperature.

【図3】仕上焼鈍条件を示す図である。FIG. 3 is a diagram showing finish annealing conditions.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 増井 浩昭 福岡県北九州市戸畑区飛幡町1番1号 新 日本製鐵株式会社八幡製鐵所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hiroaki Masui 1-1 No. 1 Tobita-cho, Tobata-ku, Kitakyushu, Fukuoka Prefecture New Nippon Steel Corporation Yawata Works

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】 重量で、Si:1.0〜7.0%を含
み、鋼板の金属表面から15μm内に分布する内部酸化
層の量が、当該厚み領域内の酸素含有量で1%以下であ
り、B8 ≧1.93Tである磁束密度の極めて高い超低
鉄損方向性電磁鋼板。
1. The amount of the internal oxide layer containing Si: 1.0 to 7.0% by weight and distributed within 15 μm from the metal surface of the steel sheet is 1% or less in terms of oxygen content in the thickness region. And an ultra-low iron loss grain-oriented electrical steel sheet with an extremely high magnetic flux density, in which B 8 ≧ 1.93T.
【請求項2】 表面に線状または点状キズが圧延方向か
ら45〜90度の方向に、2〜15mmの間隔で付与さ
れている請求項1記載の磁束密度の極めて高い超低鉄損
方向性電磁鋼板。
2. The ultra-low iron loss direction with extremely high magnetic flux density according to claim 1, wherein linear or dot-like scratches are provided on the surface in the direction of 45 to 90 degrees from the rolling direction at intervals of 2 to 15 mm. Magnetic electrical steel sheet.
【請求項3】 重量で、Si:1.0〜7.0%、酸可
溶性Al:0.010〜0.070%を含有し、残部が
Fe及び不可避的不純物からなる鋼塊あるいはスラブ
を、熱延し、冷延し、一次再結晶焼鈍し、焼鈍分離剤を
塗布した後、高温仕上焼鈍を行い、ヒートフラットニン
グを行うことによって方向性電磁鋼板を製造する方法に
おいて、前記一次再結晶焼鈍後の鋼板の一次再結晶粒の
うち粒径が平均粒径の2倍を超えるものが10%未満で
あるように調整し、同鋼板に焼鈍分離剤として、MgO
100重量部に対してLi、K、Na、Ba、Ca、M
g、Zn、Fe、Zr、Sn、Sr、Alの塩化物、炭
酸塩、硝酸塩、硫酸塩、硫化物の中から選ばれる1種又
は2種以上を2〜30重量部添加したものを塗布し、高
温仕上焼鈍時の昇温速度を、950〜1150℃の間
で、10℃/hr以下とし、かつ焼鈍雰囲気を少なくと
もN2 30%以上のN2 +H2 とすることを特徴とする
磁束密度の極めて高い超低鉄損方向性電磁鋼板の製造方
法。
3. A steel ingot or slab containing Si: 1.0 to 7.0% by weight, acid-soluble Al: 0.010 to 0.070% by weight, and the balance being Fe and inevitable impurities, Hot rolling, cold rolling, primary recrystallization annealing, after applying an annealing separator, high temperature finish annealing, in the method of producing a grain-oriented electrical steel sheet by performing heat flattening, the primary recrystallization annealing Of the primary recrystallized grains of the subsequent steel sheet, those having a grain size exceeding twice the average grain size were adjusted to less than 10%, and MgO was used as an annealing separator on the same steel sheet.
Li, K, Na, Ba, Ca, M for 100 parts by weight
2 to 30 parts by weight of one or more selected from chlorides, carbonates, nitrates, sulfates, and sulfides of g, Zn, Fe, Zr, Sn, Sr, and Al is added, and applied. The magnetic flux density is characterized in that the temperature rising rate during high-temperature finish annealing is 10 ° C./hr or less between 950 and 1150 ° C., and the annealing atmosphere is N 2 + H 2 of at least N 2 30% or more. Of extremely low iron loss grain oriented electrical steel sheet with extremely high
【請求項4】 重量で、Si:1.0〜7.0%、酸可
溶性Al:0.010〜0.070%、C:0.021
〜0.075%、N:0.003〜0.0130%、S
≦0.030%、Mn:0.05〜0.45%を含有
し、残部がFe及び不可避的不純物からなるスラブの熱
延前の加熱を、1280℃未満の温度で行い、一次再結
晶完了後、高温仕上焼鈍の二次再結晶開始前の間で窒化
することを特徴とする請求項3記載の磁束密度の極めて
高い超低鉄損方向性電磁鋼板の製造方法。
4. By weight, Si: 1.0 to 7.0%, acid-soluble Al: 0.010 to 0.070%, C: 0.021.
~ 0.075%, N: 0.003-0.0130%, S
≦ 0.030%, Mn: 0.05 to 0.45% is contained, and the rest is heated before hot rolling of a slab consisting of Fe and unavoidable impurities at a temperature of less than 1280 ° C. to complete primary recrystallization. The method for producing an ultra-low core loss grain-oriented electrical steel sheet having an extremely high magnetic flux density according to claim 3, wherein the nitriding is performed after that and before the start of secondary recrystallization in high temperature finish annealing.
【請求項5】 ヒートフラットニングの前又は後に、レ
ーザー、歯形ロール、プレス、ケガキ、局部エッチング
等の局部加工により鋼板表面に線状または点状キズを付
与することを特徴とする請求項3又は4記載の磁束密度
の極めて高い超低鉄損方向性電磁鋼板の製造方法。
5. A linear or point-like scratch is imparted to the surface of the steel sheet by local processing such as laser, tooth roll, press, scribe, local etching, etc., before or after heat flattening. 4. The method for manufacturing an ultra-low iron loss grain-oriented electrical steel sheet according to 4, which has an extremely high magnetic flux density.
JP4175790A 1992-06-26 1992-07-02 Ultra low iron loss grain oriented electrical steel sheet with extremely high magnetic flux density. Expired - Lifetime JP2691828B2 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP4175790A JP2691828B2 (en) 1992-07-02 1992-07-02 Ultra low iron loss grain oriented electrical steel sheet with extremely high magnetic flux density.
DE69332394T DE69332394T2 (en) 1992-07-02 1993-07-01 Grain-oriented electrical sheet with high flux density and low iron losses and manufacturing processes
KR93012299A KR960009170B1 (en) 1992-07-02 1993-07-01 Grain oriented electrical steel sheet having high magnetic flux density and ultra iron loss and process for producing the same
EP93110517A EP0577124B1 (en) 1992-07-02 1993-07-01 Grain oriented electrical steel sheet having high magnetic flux density and ultra low iron loss and process for producing the same
US08/257,765 US5507883A (en) 1992-06-26 1994-06-09 Grain oriented electrical steel sheet having high magnetic flux density and ultra low iron loss and process for production the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4175790A JP2691828B2 (en) 1992-07-02 1992-07-02 Ultra low iron loss grain oriented electrical steel sheet with extremely high magnetic flux density.

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Publication Number Publication Date
JPH0617132A true JPH0617132A (en) 1994-01-25
JP2691828B2 JP2691828B2 (en) 1997-12-17

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07316831A (en) * 1994-05-23 1995-12-05 Kaisui Kagaku Kenkyusho:Kk Ceramic film forming agent and method for producing the same
EP0753588A1 (en) * 1995-07-14 1997-01-15 Nippon Steel Corporation Method for producing a grain-oriented electrical steel sheet having a mirror surface and improved core loss
CN1054885C (en) * 1995-07-26 2000-07-26 新日本制铁株式会社 Method for producing grain-oriented electrical steel sheet having mirror surface and improved iron loss

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8920581B2 (en) 2008-12-16 2014-12-30 Nippon Steel & Sumitomo Metal Corporation Grain-oriented electrical steel sheet and manufacturing method thereof
WO2017201418A1 (en) 2016-05-20 2017-11-23 Arcanum Alloys, Inc. Methods and systems for coating a steel substrate
WO2021155280A1 (en) * 2020-01-31 2021-08-05 Arcanum Alloys, Inc. Modified steel compositions and methods related thereto

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0480322A (en) * 1990-07-20 1992-03-13 Nippon Steel Corp Production of grain-oriented silicon steel sheet reduced in iron loss

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0480322A (en) * 1990-07-20 1992-03-13 Nippon Steel Corp Production of grain-oriented silicon steel sheet reduced in iron loss

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07316831A (en) * 1994-05-23 1995-12-05 Kaisui Kagaku Kenkyusho:Kk Ceramic film forming agent and method for producing the same
EP0753588A1 (en) * 1995-07-14 1997-01-15 Nippon Steel Corporation Method for producing a grain-oriented electrical steel sheet having a mirror surface and improved core loss
CN1054885C (en) * 1995-07-26 2000-07-26 新日本制铁株式会社 Method for producing grain-oriented electrical steel sheet having mirror surface and improved iron loss

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