JPH07118743A - Production of high magnetic flux density grain-oriented silicon steel sheet free from forsterite film - Google Patents

Production of high magnetic flux density grain-oriented silicon steel sheet free from forsterite film

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Publication number
JPH07118743A
JPH07118743A JP7739092A JP7739092A JPH07118743A JP H07118743 A JPH07118743 A JP H07118743A JP 7739092 A JP7739092 A JP 7739092A JP 7739092 A JP7739092 A JP 7739092A JP H07118743 A JPH07118743 A JP H07118743A
Authority
JP
Japan
Prior art keywords
annealing
steel sheet
magnetic flux
flux density
high magnetic
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.)
Pending
Application number
JP7739092A
Other languages
Japanese (ja)
Inventor
Takeo Nagashima
武雄 長島
Yoshiyuki Ushigami
義行 牛神
Shuichi Yamazaki
修一 山崎
Hiroyasu Fujii
浩康 藤井
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 JP7739092A priority Critical patent/JPH07118743A/en
Publication of JPH07118743A publication Critical patent/JPH07118743A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To obtain a high magnetic flux density grain-oriented silicon steel sheet by finish annealing in a short time. CONSTITUTION:This steel sheet has a compsn. contg. 2 to 4.8% Si, 0.08 to 0.020% acid soluble A1, <=0.010% N, and the balance Fe with inevitable impurities, and the amt. of acid soluble Al obtd. by subtracting Al equivalent to N from acid soluble Al in the hot rolled steel strip is regulated to <=0.01%. After cold rolling, it is subjected to primary recrystallization annealing and is coated with a separation agent for annealing essentially consisting of alumina and its temp. is raised to 920 to 1150 deg.C in a neutral or reducing atmosphere so as to regulate the temp. rising rate in finish annealing to >=50 deg.C/Hr, and it is held to the same temp. for >=5hr. Moreover, it is preferabe for obtaining a high magnetic flux density material to execute nitriding by ammonia before the start of the finish annealing and to straighten the inhibitor. Thus, the high magnetic flux density grain-oriented silicon steel sheet can be obtd. in a short time, and domain fractionating treatment and tension coating are executed to obtain an ultralow core loss material.

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、磁束密度が高く鉄損が
極めて低い方向性珪素鋼板(以下方向性電磁鋼板と云
う)に関するものである。特に、二次再結晶工程(仕上
げ焼鈍工程)で、その鋼板表面にフォルステライト(以
下、グラスと云う)被膜を形成させず、同時に、サーマ
ルエッチングにより鋼板表面を平滑(鏡面)化した状態
で同工程を完了させ、その後、磁区細分化、張力コーテ
ィング等の処理を行い、鉄損特性の改善を図ろうとする
ものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a grain-oriented silicon steel sheet having high magnetic flux density and extremely low iron loss (hereinafter referred to as grain-oriented electrical steel sheet). Especially, in the secondary recrystallization step (finish annealing step), the forsterite (hereinafter referred to as glass) film is not formed on the surface of the steel sheet, and at the same time, the steel sheet surface is smoothed (mirror surface) by thermal etching. After the process is completed, magnetic domain subdivision, tension coating, and other treatments are performed to improve the iron loss characteristics.

【0002】[0002]

【従来の技術】方向性電磁鋼板は、電気機器の磁気鉄心
として多用され、エネルギーロスを少なくすべく、改善
が繰り返されてきた。方向性電磁鋼板の鉄損を低減する
手段として、仕上げ焼鈍後の材料表面にレーザービーム
を照射し、局部歪を与え、それによって磁区を細分化し
て鉄損を低下させる方法が、例えば特開昭58−264
05号公報に開示されている。
2. Description of the Related Art Grain-oriented electrical steel sheets are frequently used as magnetic iron cores for electric equipment, and have been repeatedly improved to reduce energy loss. As a means for reducing the iron loss of grain-oriented electrical steel sheets, a method of irradiating a laser beam on the surface of the material after finish annealing to give local strain to thereby subdivide the magnetic domains to reduce the iron loss is disclosed in, for example, Japanese Patent Application Laid-Open No. 58-264
No. 05 publication.

【0003】また局部歪は、通常行われる加工後の応力
除去焼鈍(歪取り焼鈍)によって除去されるので、磁区
細分化効果が消失する。この改善策、すなわち応力除去
焼鈍しても磁区細分化効果が消失しない手段が、例えば
特開昭62−8617号公報に開示されている。
Further, since the local strain is removed by the stress relief annealing (strain relief annealing) after the usual working, the magnetic domain refining effect disappears. For example, Japanese Patent Laid-Open No. 62-8617 discloses a remedy for this problem, that is, a means in which the magnetic domain refinement effect does not disappear even when stress relief annealing is performed.

【0004】さらに鉄損値の低減を図るためには、鋼板
表面近傍の磁区の動きを阻害する地鉄表面の凹凸を取り
除くこと(平滑化)が重要である。平滑化の最も高いレ
ベルが鏡面である。仕上げ焼鈍後の材料表面を平滑化
(鏡面化)する方法としては、特開昭64−83620
号公報に開示されている化学研磨、電解研磨等がある。
In order to further reduce the iron loss value, it is important to remove (smooth) the irregularities on the surface of the base metal which hinder the movement of magnetic domains near the surface of the steel sheet. The highest level of smoothing is specular. As a method for smoothing (mirror-finishing) the material surface after finish annealing, there is disclosed in JP-A-64-83620.
There are chemical polishing, electrolytic polishing, and the like disclosed in the publication.

【0005】[0005]

【発明が解決しようとする課題】従来、鋼板表面を鏡面
化(平滑化)する方法としては、前記化学研磨、電解研
磨の他にブラシ研磨、サンドペーパー研磨、研削等の化
学的或いは物理的方法がある。しかしながら、これらの
方法は、小試片、少量の試料を作るには適するが、工業
的に多量生産される金属ストリップ等の表面鏡面化(平
滑化)のためには、諸々の困難を伴う。
Conventionally, as a method of mirror-finishing (smoothing) the surface of a steel sheet, chemical or physical methods such as brush polishing, sandpaper polishing and grinding other than the above chemical polishing and electrolytic polishing are used. There is. However, these methods are suitable for producing small test pieces and small samples, but are accompanied by various difficulties for the surface mirror-finishing (smoothing) of industrially mass-produced metal strips and the like.

【0006】最も平滑化できるとされる化学的方法、即
ち、化学研磨においては、薬剤濃度管理、排水処理等の
環境問題、また物理的方法においては、工業的に大きな
面積を持つ表面を同一基準で平滑化(鏡面化)すること
は、極めて困難である。本発明は、これらの問題を排し
て、工業的生産規模で方向性電磁鋼板の表面を鏡面化
(平滑化)する方法を提供することを目的とする。
In the chemical method that is said to be the most smooth, that is, in chemical polishing, environmental problems such as chemical concentration control and wastewater treatment, and in the physical method, a surface having an industrially large area is used as the same standard. It is extremely difficult to smooth (mirror-finish) with. An object of the present invention is to eliminate these problems and to provide a method for mirror-finishing (smoothing) the surface of a grain-oriented electrical steel sheet on an industrial production scale.

【0007】[0007]

【課題を解決するための手段】当然ながら鏡面化(平滑
化)のために、磁気特性が失われてはならない。本発明
においては、仕上げ焼鈍工程で同時に目的を達成しよう
とするものである。すなわち、二次再結晶の方位を制御
し、極度に高い磁束密度を得、かつ鏡面(平滑表面)を
得ようとするものである。
As a matter of course, the magnetic characteristics must not be lost due to mirroring (smoothing). In the present invention, it is intended to simultaneously achieve the object in the finish annealing step. That is, the orientation of secondary recrystallization is controlled to obtain an extremely high magnetic flux density and to obtain a mirror surface (smooth surface).

【0008】本発明の特徴とするところは、仕上げ焼鈍
時に鏡面(平滑表面)を得るところにある。すなわち、
通常行われているMgOを主体とする焼鈍分離剤を用い
ずに、Al2 3 等のSiO2 と反応しない或いは、反
応しにくい物質を焼鈍分離剤として用いて、高い磁束密
度の方向性電磁鋼板を得ると同時に鋼板の表面にグラス
(フォルステライト)被膜を形成させずに、金属表面を
露出させた状態で二次再結晶させ、同時に、サーマルエ
ッチングにより金属表面を鏡面(平滑化)することを特
徴とする。
A feature of the present invention is to obtain a mirror surface (smooth surface) during finish annealing. That is,
Without using a commonly used annealing separator mainly composed of MgO, a substance which does not react with SiO 2 such as Al 2 O 3 or which hardly reacts is used as the annealing separator, and a directional electromagnetic field having a high magnetic flux density is obtained. At the same time as obtaining the steel plate, without forming a glass (forsterite) film on the surface of the steel plate, secondary recrystallization is performed with the metal surface exposed, and at the same time, the metal surface is mirror-finished (smoothed) by thermal etching. Is characterized by.

【0009】本発明はSi:2.0〜4.8重量%、酸
可溶性Al:0.008〜0.020重量%、N≦0.
010重量%、残部Fe及び不可避的不純物からなる珪
素熱延鋼帯を必要に応じて焼鈍した後、1回または中間
焼鈍をはさむ2回以上の冷間圧延を行い、所定の板厚と
し、次いで一次再結晶焼鈍を行った後焼鈍分離剤を塗布
し、仕上げ焼鈍を施す方向性珪素鋼板の製造において、
熱延鋼帯での酸可溶性AlからN当量のAlを引いた酸
可溶性Alの量を0.010重量%以下とし、一次再結
晶焼鈍後、Al2 3 (アルミナ)を主体とする焼鈍分
離剤を塗布し、中性或いは、還元性雰囲気で仕上げ焼鈍
の昇温速度を50℃/Hr以上で920〜1150℃まで
昇温し、該温度に到達時、該温度で5時間以上保持する
ことである。
In the present invention, Si: 2.0 to 4.8% by weight, acid-soluble Al: 0.008 to 0.020% by weight, N ≦ 0.
A silicon hot-rolled steel strip consisting of 010 wt%, balance Fe and unavoidable impurities is annealed if necessary, and then cold rolled once or twice or more with intermediate annealing, to a predetermined plate thickness, and then In the production of a grain-oriented silicon steel sheet, which is subjected to a primary recrystallization annealing, is applied with an annealing separator, and is then subjected to finish annealing,
The amount of acid-soluble Al obtained by subtracting N equivalent of Al from acid-soluble Al in the hot-rolled steel strip is set to 0.010% by weight or less, and after primary recrystallization annealing, annealing separation mainly composed of Al 2 O 3 (alumina) Apply the agent, raise the heating rate of finish annealing in a neutral or reducing atmosphere at 920 to 1150 ° C at 50 ° C / Hr or more, and when the temperature is reached, hold at that temperature for 5 hours or more. Is.

【0010】ここで、一次再結晶焼鈍から仕上げ焼鈍工
程に入る前にアンモニアによる窒化処理を行うこと及び
昇温時の雰囲気中のN2 を5%以上とすることは、イン
ヒビター強化の面から有効である。焼鈍分離剤の塗布を
静電塗布とすることもグラス被膜を生成しないこと及び
インヒビター劣化防止の面から有効である。焼鈍分離剤
としてMgO以外のアルカリ土金属の酸化物を用いるこ
とができる。
Here, it is effective from the viewpoint of inhibitor strengthening to perform a nitriding treatment with ammonia before starting from the primary recrystallization annealing to the finishing annealing step, and to make N 2 in the atmosphere at the time of temperature rising 5% or more. Is. It is also effective to apply the annealing separator as an electrostatic coating from the viewpoint of not forming a glass coating and preventing the deterioration of the inhibitor. An oxide of an alkaline earth metal other than MgO can be used as the annealing separator.

【0011】以下、本発明について詳細に説明する。本
発明者等は、仕上げ焼鈍中のインヒビター(析出物)の
挙動を詳しく調べたところ、鋼中N量の多い場合は、析
出物としてAlNの他に窒化珪素が生成し、鋼中N量の
少ない場合は、析出物としては、AlNのみであること
が分かった。しかしながら窒化珪素は熱力学から分かる
ように高温で不安定で通常900℃以上では、分解して
安定に存在しない。
The present invention will be described in detail below. The present inventors have investigated the behavior of the inhibitor (precipitate) during finish annealing in detail, and when the amount of N in the steel is large, silicon nitride is generated as a precipitate in addition to AlN, and the amount of N in the steel is When the amount was small, it was found that the precipitate was only AlN. However, as can be seen from thermodynamics, silicon nitride is unstable at high temperatures and usually decomposes and does not exist stably at 900 ° C. or higher.

【0012】従って900℃以上で二次再結晶させるた
めのインヒビターとしては、窒化珪素は不適であり、A
lNが有効である。しかしながら、AlNは、鋼板表面
(界面)におけるAlの酸化により劣化することが本発
明者等の実験で分かっている。
Therefore, silicon nitride is not suitable as an inhibitor for secondary recrystallization at 900 ° C. or higher.
1N is effective. However, it is known from experiments by the present inventors that AlN deteriorates due to oxidation of Al on the surface (interface) of the steel sheet.

【0013】前記するように酸可溶性Alは一次再結晶
焼鈍時生ずる鋼板表面の酸化層中の酸素や、焼鈍雰囲気
中の微量の酸素(水分)を捕えてAl2 3 となる。二
次再結晶に必要な温度まで短時間で昇温し酸可溶性Al
と焼鈍雰囲気中の酸素との反応時間を短くし、インヒビ
ター劣化を抑えることが有効である。本発明者等の実験
では50℃/H以上の急速加熱が有効で、これ未満で
は、インヒビター劣化が大きく、十分な磁束密度の方向
性電磁鋼板が得られなかった。なおインヒビター強度と
して鋼中酸可溶性Al濃度を示すが、Alは、AlN,
(Al,Si)N等の化合物(析出物)を形成して、イ
ンヒビターとなっているので、酸可溶性Al量がインヒ
ビター強度を示す指標と考えて良い。
As described above, the acid-soluble Al becomes Al 2 O 3 by capturing oxygen in the oxide layer on the surface of the steel sheet generated during the primary recrystallization annealing and a small amount of oxygen (water) in the annealing atmosphere. Acid-soluble Al is heated in a short time to the temperature required for secondary recrystallization.
It is effective to shorten the reaction time with oxygen in the annealing atmosphere and suppress inhibitor deterioration. In the experiments conducted by the present inventors, rapid heating of 50 ° C./H or more is effective, and if the heating temperature is less than 50 ° C., the inhibitor deterioration is large and a grain-oriented electrical steel sheet having a sufficient magnetic flux density cannot be obtained. The inhibitor strength indicates the concentration of acid-soluble Al in steel. Al is AlN,
Since a compound (precipitate) such as (Al, Si) N is formed and acts as an inhibitor, the amount of acid-soluble Al can be considered as an index showing the inhibitor strength.

【0014】さらに、本発明者らは、インヒビター劣化
の律速過程を詳しく調査したところ、前記の鋼板界面に
おけるAlの酸化以外に鋼中窒素及び焼鈍雰囲気中の窒
素量にも影響されることが分かった。なお、焼鈍雰囲気
中の窒素量は鋼板界面を通して鋼中の窒素量を増加させ
ているものであり、その効果は、当初から鋼中に入って
いる窒素と同じである。鋼中窒素及び焼鈍雰囲気中の窒
素は、AlN等の析出物を増加させてAlを固定し、A
lの鋼板界面への移動を少なくするために、Alの酸化
が抑制されるのである。
Further, the inventors of the present invention have conducted a detailed investigation on the rate-determining process of inhibitor deterioration, and found that the amount of nitrogen in the steel and the amount of nitrogen in the annealing atmosphere are also influenced in addition to the oxidation of Al at the steel sheet interface. It was The amount of nitrogen in the annealing atmosphere increases the amount of nitrogen in the steel through the steel sheet interface, and the effect is the same as nitrogen contained in the steel from the beginning. Nitrogen in steel and nitrogen in the annealing atmosphere increase precipitates such as AlN to fix Al,
Oxidation of Al is suppressed in order to reduce the migration of 1 to the steel plate interface.

【0015】従って、仕上げ焼鈍中の鋼中酸可溶性Al
量は、窒素分圧の高い方が、劣化は少なく、高温までイ
ンヒビターは強い。本発明の主旨とするところの一つで
ある高い磁束密度を得るためには、インヒビターは、強
い方が良いのであるが、強く一定に維持されることが望
ましい。但し、強すぎていつまでも二次再結晶しないよ
うではいけない。
Therefore, acid-soluble Al in steel during finish annealing
The higher the nitrogen partial pressure, the less the amount of deterioration, and the stronger the inhibitor is at high temperatures. In order to obtain a high magnetic flux density, which is one of the gist of the present invention, it is preferable that the inhibitor is strong, but it is preferable that the inhibitor is strongly and constantly maintained. However, it should not be so strong that secondary recrystallization does not occur.

【0016】二次再結晶する強度で強く保持されること
が高い磁束密度を得るための条件である。ここで本発明
者らが熱延鋼帯での酸可溶性AlからN当量のAlを引
いた酸可溶性Alの量を0.010重量%以下とした理
由について述べる。
It is a condition for obtaining a high magnetic flux density that it is strongly retained with the strength of secondary recrystallization. Here, the reason why the present inventors set the amount of acid-soluble Al obtained by subtracting N equivalent of Al from acid-soluble Al in the hot-rolled steel strip to 0.010% by weight or less will be described.

【0017】図1は、一次再結晶焼鈍後アンモニアによ
る窒化処理をした後の鋼板内部の析出物を抽出して、電
子顕微鏡で5000倍に拡大した写真である。大きな析
出物は熱延鋼帯時に既に存在するNとAlが結合してA
lNとなって成長した析出物である。小さい析出物はア
ンモニア窒化によって新しく生成したAlNである。熱
延鋼帯に存在するAlNは、鋼成分を決める製鋼から長
い時間高温に晒されてきているので、いわゆるオストワ
ルド成長をして大きなAlN粒子に成長したのである。
一次再結晶焼鈍後窒化によって形成されたAlNは、ま
だオストワルド成長が十分でなく、小さいままで存在す
る。
FIG. 1 is a photograph in which precipitates inside the steel sheet after the primary recrystallization annealing and nitriding treatment with ammonia were extracted and magnified 5000 times with an electron microscope. Large precipitates are formed by the combination of N and Al that are already present in the hot-rolled steel strip.
It is a precipitate that has grown to 1N. The small precipitate is AlN newly formed by ammonia nitriding. The AlN existing in the hot-rolled steel strip has been exposed to high temperature for a long time from the steel making which determines the steel composition, so that the so-called Ostwald growth was performed to grow into large AlN particles.
The AlN formed by the nitridation after the primary recrystallization annealing does not have sufficient Ostwald growth, and remains small.

【0018】周知のようにインヒビター効果は析出物の
量に比例し、その大きさに反比例する。従って、熱延鋼
帯に存在するAlNのインヒビター効果は、一次再結晶
後に窒化によって生成するAlNのインヒビター効果よ
りはるかに小さい。
As is well known, the inhibitor effect is proportional to the amount of precipitate and inversely proportional to its size. Therefore, the inhibitor effect of AlN existing in the hot-rolled steel strip is much smaller than that of AlN produced by nitriding after primary recrystallization.

【0019】本発明者らは、一次再結晶後に生ずるAl
Nの量を適正化するために、熱延鋼帯に存在するAlN
以外の酸可溶性Alを規定したものである。このことに
よりインヒビターとして主体となる一次再結晶後に生ず
るAlNをある適正な値に定めることができた。これ
は、製造上極めて重要なことであり、すなわち、常にイ
ンヒビターを必要十分な量確保できるということであ
る。
The present inventors have found that Al generated after primary recrystallization
AlN present in hot-rolled steel strip to optimize the amount of N
Other acid-soluble Al is defined. As a result, it was possible to set AlN generated after primary recrystallization, which is the main inhibitor, to an appropriate value. This is extremely important in manufacturing, that is, the inhibitor can always be secured in a necessary and sufficient amount.

【0020】一次再結晶後の窒化量がある一定量以上で
あれば窒化量に関わらず、必要十分なインヒビター量を
確保できることになる。一次再結晶後アンモニア窒化或
いは、仕上げ焼鈍中の窒素分圧をコントロールして、イ
ンヒビターを確保する時にこのコントロールが極めて容
易になる。
If the nitriding amount after the primary recrystallization is a certain amount or more, a necessary and sufficient inhibitor amount can be secured regardless of the nitriding amount. This control becomes extremely easy when controlling the nitrogen partial pressure during ammonia nitridation or finish annealing after primary recrystallization to secure the inhibitor.

【0021】前述したように仕上げ焼鈍中の窒素分圧を
上げると鋼中窒素が増し、Alの溶解が少なくなるので
酸可溶性Alの減少が抑えられるのであるが、必要以上
に化合物AlNを形成していないAlが存在すると、イ
ンヒビターとしての新たに生成するAlNは過剰にな
り、二次再結晶が完了するまでに長い時間を要すると
か、二次再結晶が不安定になったりする不都合が生ず
る。このような不都合が熱延鋼帯のAlNを形成してい
ない酸可溶性Alを制限することで可能となる。
As described above, if the nitrogen partial pressure during finish annealing is increased, nitrogen in the steel is increased and the dissolution of Al is decreased, so that the decrease of acid-soluble Al is suppressed, but the compound AlN is formed more than necessary. If unreacted Al is present, newly generated AlN as an inhibitor becomes excessive, and it takes a long time to complete the secondary recrystallization, or the secondary recrystallization becomes unstable. Such inconvenience becomes possible by limiting the acid-soluble Al that does not form AlN in the hot-rolled steel strip.

【0022】インヒビター強度を強く一定に保つのは、
二次再結晶開始から終了まで方位の良い結晶(GOSS
粒)のみを成長させるためであり、二次再結晶開始から
終了までにインヒビターが弱体化すると方位の悪い粒ま
で成長し、製品鋼板の磁束密度が下がる。この方策とし
て焼鈍雰囲気の窒素の分圧を上げて鋼板中の窒素量を増
やし析出物としてのAlNを一定に維持することが望ま
しい。しかしながら、本発明の主旨とするところの一つ
である鏡面を得るには、窒素分圧があまり高くなり過ぎ
てはいけない。
To keep the inhibitor strength strong and constant,
Crystals with good orientation from the start to the end of secondary recrystallization (GOSS
This is to grow only grains), and if the inhibitor weakens from the start to the end of secondary recrystallization, grains with bad orientation grow and the magnetic flux density of the product steel sheet decreases. As a measure for this, it is desirable to increase the partial pressure of nitrogen in the annealing atmosphere to increase the amount of nitrogen in the steel sheet and keep AlN as a precipitate constant. However, the nitrogen partial pressure must not be too high in order to obtain a mirror surface, which is one of the gist of the present invention.

【0023】インヒビターを一定の強さで二次再結晶さ
せるという点でAlNの溶解度が変化しない、すなわち
インヒビター強度が変わらない一定温度での二次再結晶
は極めて有効である。
The secondary recrystallization at a constant temperature at which the solubility of AlN does not change, that is, the inhibitor strength does not change, is extremely effective in that the inhibitor is secondarily recrystallized at a constant strength.

【0024】前記するように、AlNの溶解度は、一定
温度に保持すれば変わらないが、酸可溶性Alは雰囲気
中の酸素或いは、鋼板表面のAlより酸素親和性の小さ
い元素の酸化物より酸素をとり、Al2 3 となって減
少してゆき、インヒビターは劣化する。従って、この場
合も、窒素分圧を上げてAlNの溶解を抑え、酸可溶性
Alの減少を抑制しなければならない。
As described above, the solubility of AlN does not change if it is maintained at a constant temperature, but the acid-soluble Al has more oxygen than oxygen in the atmosphere or an oxide of an element having a lower oxygen affinity than Al on the surface of the steel sheet. Then, it becomes Al 2 O 3 and decreases, and the inhibitor deteriorates. Therefore, also in this case, it is necessary to raise the nitrogen partial pressure to suppress the dissolution of AlN and suppress the decrease of the acid-soluble Al.

【0025】以下、実施条件について述べる。一次再結
晶焼鈍後から仕上げ焼鈍前にアンモニアにより窒化処理
を行い、インヒビターを強化することは有効である。こ
れは、一次再結晶完了時のインヒビター強度では、二次
再結晶のためには不十分で、また仕上げ焼鈍中の窒素分
圧を上げてインヒビターを強化或いは、劣化防止しても
二次再結晶時に十二分なインヒビターを確保できない。
このため一般にアンモニア処理によるインヒビター強度
が、磁気特性を向上させる。
The implementation conditions will be described below. It is effective to strengthen the inhibitor by nitriding with ammonia after the primary recrystallization annealing and before the finish annealing. This is because the inhibitor strength at the time of completion of primary recrystallization is not sufficient for secondary recrystallization, and even if the inhibitor is strengthened or deterioration is prevented by increasing the partial pressure of nitrogen during finish annealing. Sometimes we can't get enough inhibitors.
Therefore, the inhibitor strength obtained by the ammonia treatment generally improves the magnetic properties.

【0026】二次再結晶進行時に必要なインヒビターを
確保するために、焼鈍雰囲気中に窒素ガスを5%以上9
5%以下入れるのが望ましいが、水素ガス100%でも
良い。なお、窒素ガス5%未満では、インヒビターの強
化或いは、劣化防止には、効果が薄い。
In order to secure an inhibitor necessary for the progress of secondary recrystallization, 5% or more of nitrogen gas is used in the annealing atmosphere.
It is desirable to add 5% or less, but 100% hydrogen gas may be used. If the nitrogen gas content is less than 5%, the effect of strengthening the inhibitor or preventing deterioration is small.

【0027】なお、中性或いは還元性雰囲気とは、窒
素、酸素、水分、水素、アルゴン等の不活性ガスの内か
ら1種或いは2種以上のガスの混合物で、珪素の酸化還
元に対して中性或いは還元性であるガス組成をいう。一
般に電磁鋼板の仕上げ焼鈍では、窒素及び水素ガスが用
いられるので、この両ガスの0%から100%までの組
み合わせである。
The neutral or reducing atmosphere is one or a mixture of two or more gases selected from inert gases such as nitrogen, oxygen, water, hydrogen, argon, etc., for oxidation-reduction of silicon. A gas composition that is neutral or reducing. Generally, nitrogen and hydrogen gas are used in the finish annealing of the electromagnetic steel sheet, and therefore the combination of these gases is 0% to 100%.

【0028】窒素分圧を調整するために、この両ガスの
組み合わせにアルゴン、ヘリウム等の不活性ガスを混合
しても何等支障はない。中性或いは還元性雰囲気とする
のは、鋼中Alの減少防止及び、鋼中の珪素を酸化させ
て表面にSiO2 を増加させないためである。
There is no problem even if an inert gas such as argon or helium is mixed with the combination of both gases in order to adjust the nitrogen partial pressure. The neutral or reducing atmosphere is used to prevent reduction of Al in the steel and to oxidize silicon in the steel so as not to increase SiO 2 on the surface.

【0029】仕上げ焼鈍前の鋼板表面の酸化層中のSi
2 及び焼鈍炉中の僅かな酸素或いは、水分によって仕
上げ焼鈍中に生成するSiO2 は、ここにMgOが存在
するとフォルステライト被膜(グラス被膜)を形成する
ので焼鈍分離剤としては、SiO2 と反応しないか或い
は、反応しにくい物質が必要である。この目的に合致す
るものとしては、Al2 3 (アルミナ)が最も良い。
なお、アルミナに下記物質等を含んでも何等差し障りな
い。
Si in the oxide layer on the surface of the steel sheet before finish annealing
Since SiO 2 generated during finish annealing due to O 2 and a slight amount of oxygen or water in the annealing furnace forms a forsterite film (glass film) when MgO is present therein, SiO 2 is used as an annealing separator. A substance that does not react or is difficult to react is required. Al 2 O 3 (alumina) is the best one that meets this purpose.
In addition, even if the following substances are included in alumina, there is no problem.

【0030】さらに本発明の主旨とするところの鏡面
(平滑面)を得ると言う観点からは、BaO,CaO,
SrO等のアルカリ土金属の酸化物粉末が有効であっ
た。また、鋼板表面に被膜を作らないためには、反応性
の小さい物質状態、例えば粉末の粒度を大きくするとか
水和物を作ることなく、鋼板表面に塗布する方法が有効
であった。水和物を作ることなく鋼板表面に焼鈍分離剤
を塗布する方法として静電塗布は、極めて有効であっ
た。
Further, from the viewpoint of obtaining a mirror surface (smooth surface), which is the gist of the present invention, BaO, CaO,
An oxide powder of an alkaline earth metal such as SrO was effective. Further, in order to prevent the formation of a coating film on the surface of the steel sheet, a method of applying it to the surface of the steel sheet without reducing the reactivity of the substance, for example, increasing the particle size of the powder or forming a hydrate was effective. Electrostatic coating was extremely effective as a method of coating the annealing separator on the surface of the steel sheet without forming a hydrate.

【0031】仕上げ焼鈍における二次再結晶可能な温度
までの昇温速度は、高速であればあるほどインヒビター
の劣化が少なく好都合であった。昇温速度15℃/Hr未
満では、インヒビターの劣化が著しく二次再結晶時に必
要なインヒビターが確保されず、十分な二次再結晶が得
られず、鋼板の磁束密度(B8 )は低かった。本発明の
主旨の一つである高い磁束密度を得るという点では、5
0℃/Hr以上の昇温速度が必要であった。
The higher the rate of temperature rise up to the temperature at which secondary recrystallization is possible in finish annealing, the more favorable the inhibitor is because it is less likely to deteriorate. If the heating rate is less than 15 ° C./Hr, the inhibitor is remarkably deteriorated and the inhibitor required for secondary recrystallization is not secured, sufficient secondary recrystallization is not obtained, and the magnetic flux density (B 8 ) of the steel sheet is low. . In terms of obtaining a high magnetic flux density, which is one of the main points of the present invention, it is 5
A heating rate of 0 ° C./hr or more was required.

【0032】二次再結晶させるために一定の温度で保持
することは、高い磁束密度を得るためには特に有効であ
る。これは、インヒビターの劣化を防止して適度なイン
ヒビター強度で二次再結晶させるものである。この温度
は、920℃未満では、二次再結晶完了までの時間が長
くなり過ぎて実用的でなくなる。また、1150℃超で
は、インヒビターの劣化が著しくなり過ぎて二次再結晶
完了まで必要なインヒビターを確保できない。
Holding at a constant temperature for secondary recrystallization is particularly effective for obtaining a high magnetic flux density. This is to prevent deterioration of the inhibitor and carry out secondary recrystallization with an appropriate inhibitor strength. If this temperature is lower than 920 ° C., the time until the completion of secondary recrystallization becomes too long and it becomes impractical. On the other hand, if the temperature exceeds 1150 ° C., the inhibitor is so much deteriorated that the necessary inhibitor cannot be secured until the secondary recrystallization is completed.

【0033】二次再結晶させるための保持時間は5時間
以上必要で、これより短い時間では保持時間内に完了し
ない。該保持温度に到達したとき、前記するようにイン
ヒビターの劣化を抑え、インヒビター強度を一定にする
ために窒素分圧を昇温時より高くする。
The holding time for secondary recrystallization is required to be 5 hours or more, and shorter time does not complete within the holding time. When the holding temperature is reached, the nitrogen partial pressure is made higher than that at the time of temperature increase in order to suppress the deterioration of the inhibitor and keep the inhibitor strength constant as described above.

【0034】ただし、窒素分圧は高くすれば高いほど良
いというものではない。あまり高くするとインヒビター
が強くなり過ぎて二次再結晶完了までに時間がかかり過
ぎることや、二次再結晶しない等の不都合を生ずる。な
お、二次再結晶完了後、純化及び鋼板表面の鏡面化(平
滑化)を完全にするために水素濃度を上げ、1200℃
付近で数時間保持することは、極めて有効である。
However, the higher the nitrogen partial pressure, the better. If it is too high, the inhibitor becomes too strong, and it takes too long to complete the secondary recrystallization, and the secondary recrystallization does not occur. After the completion of secondary recrystallization, the hydrogen concentration was increased to 1200 ° C. in order to completely purify and mirror-finish (smooth) the steel plate surface.
Holding for several hours in the vicinity is extremely effective.

【0035】本発明における鋼成分は、Si:2.0〜
4.8重量%、酸可溶性Al:0.008〜0.020
重量%、N≦0.010重量%、残部Fe及び不可避的
不純物からなり、それ以外の元素は、特に限定しない。
Siは電気抵抗を高め鉄損を下げるうえで重要である
が、4.8%超では、冷間圧延時に割れ易くなる。一
方、2.0%未満では、電気抵抗が低く鉄損を下げるう
えで問題がある。
The steel composition in the present invention is Si: 2.0-
4.8% by weight, acid-soluble Al: 0.008 to 0.020
%, N ≦ 0.010% by weight, balance Fe and unavoidable impurities, and other elements are not particularly limited.
Si is important for increasing the electric resistance and reducing the iron loss, but if it exceeds 4.8%, it tends to crack during cold rolling. On the other hand, if it is less than 2.0%, there is a problem in that the electric resistance is low and the iron loss is lowered.

【0036】酸可溶性Alは、インヒビター構成元素で
重要であり、窒素、珪素等と化合して、AlN,(A
l,Si)N等の析出物を作り、インヒビターの役割を
果たす。インヒビター強度の面、すなわち、磁束密度が
高くなる範囲として、0.008〜0.020重量%で
ある。
Acid-soluble Al is important as an inhibitor constituent element, and is combined with nitrogen, silicon, etc. to form AlN, (A
l, Si) N, etc. are formed to function as an inhibitor. In terms of the inhibitor strength, that is, the range in which the magnetic flux density is high, it is 0.008 to 0.020% by weight.

【0037】窒素は、0.010重量%超では、ブリス
ターと呼ばれる空孔を鋼板中に生ずるのでこの範囲が最
適である。また、インヒビター構成元素として、Mn,
S,Se,Sn,B,Bi,Nb,Ti,P等を添加す
ることができる。
If the content of nitrogen exceeds 0.010% by weight, holes called blisters are formed in the steel sheet, so this range is optimal. In addition, Mn,
S, Se, Sn, B, Bi, Nb, Ti, P and the like can be added.

【0038】以下、本発明の実施態様を述べる。Si:
2.0〜4.8重量%、酸可溶性Al:0.008〜
0.020重量%、N≦0.010重量%、残部Fe及
び不可避的不純物からなる溶鋼を、通常の工程で、もし
くは、連続鋳造して熱延鋼板或いは、熱延鋼帯とする。
この熱延鋼板或いは、熱延鋼帯は、750℃〜1200
℃の温度域で、30秒〜30分間磁束密度向上のための
焼鈍が行われる。
The embodiments of the present invention will be described below. Si:
2.0-4.8% by weight, acid-soluble Al: 0.008-
Molten steel consisting of 0.020% by weight, N ≦ 0.010% by weight, balance Fe and unavoidable impurities is cast into a hot-rolled steel sheet or a hot-rolled steel strip in a usual process or continuously cast.
This hot rolled steel sheet or hot rolled steel strip has a temperature of 750 ° C. to 1200 ° C.
Annealing for improving the magnetic flux density is performed in the temperature range of ° C for 30 seconds to 30 minutes.

【0039】続いて、これらの熱延鋼板或いは、熱延鋼
帯は、冷間圧延される。冷間圧延は、特公昭40−15
644号公報に開示されているように最終冷間圧延率8
0%以上とする。冷間圧延後の材料は、通常鋼中の炭素
を除去するために湿水雰囲気中で、750℃〜900℃
の温度域で一次再結晶焼鈍される。この時、脱炭、一次
再結晶と共に、鋼板表面には、酸化層が形成される。
Subsequently, these hot-rolled steel sheets or hot-rolled steel strips are cold-rolled. Cold rolling is conducted in Japanese Patent Publication No. 40-15
As disclosed in Japanese Patent No. 644, the final cold rolling rate 8
0% or more. The material after cold rolling is usually 750 ° C. to 900 ° C. in a wet water atmosphere to remove carbon in steel.
Primary recrystallization annealing is performed in the temperature range of. At this time, an oxide layer is formed on the surface of the steel sheet together with decarburization and primary recrystallization.

【0040】この酸化層は、湿水雰囲気すなわち水分の
入った雰囲気の水分量の程度(通常、露点で表す)によ
るが、いわゆる内部酸化層を形成し鋼板表面から0.1
〜6.0μmの厚さになり、ここには、酸化物として、
主にSiO2 が存在する。なお一次再結晶焼鈍時形成さ
れる酸化物の酸素量の80〜90%以上は、SiO2
形態をとっている。インヒビター強化のためアンモニア
による窒化処理を行うことは磁束密度向上に極めて有効
である。
This oxide layer forms a so-called internal oxide layer depending on the degree of water content (usually expressed as a dew point) in a wet water atmosphere, that is, an atmosphere containing water.
The thickness is about 6.0 μm, and here, as an oxide,
SiO 2 is mainly present. Note that 80 to 90% or more of the oxygen content of the oxide formed during the primary recrystallization annealing is in the form of SiO 2 . Nitriding treatment with ammonia to strengthen the inhibitor is extremely effective in improving the magnetic flux density.

【0041】一次再結晶板は、焼鈍分離剤が塗布されて
仕上げ焼鈍炉に入る。仕上げ焼鈍の昇温速度は、インヒ
ビター劣化を防止するために、なるべく大きく望ましく
は、50℃/Hr以上である。仕上げ焼鈍の雰囲気は、中
性或いは還元性とし、920℃〜1150℃に到達後、
該温度で5時間以上保持する。なお、窒素分圧調整のた
めアルゴン、ヘリウム等の不活性ガスを混合することは
何等差障りない。
The primary recrystallized plate is coated with an annealing separator and enters the finish annealing furnace. The temperature rising rate of finish annealing is as large as possible and preferably 50 ° C./Hr or more in order to prevent inhibitor deterioration. The atmosphere of finish annealing is neutral or reducing, and after reaching 920 ° C to 1150 ° C,
Hold at that temperature for 5 hours or more. It should be noted that mixing an inert gas such as argon or helium for adjusting the nitrogen partial pressure does not cause any problem.

【0042】二次再結晶完了後、純化のため100%水
素で高温(約1200℃)保持される。なお、通常用い
られる焼鈍分離剤(MgOを主体とする)と異なって、
焼鈍分離剤に水分或いは、水和水分を持ち込まないよう
にできるので、仕上げ焼鈍中、除去のための工程が要ら
ず、その分仕上げ焼鈍は、短くすることができる。仕上
げ焼鈍終了後、レーザービーム照射等の磁区細分化処理
を行い、さらに張力コーティングを行う。
After the secondary recrystallization is completed, the product is kept at a high temperature (about 1200 ° C.) with 100% hydrogen for purification. Note that, unlike the commonly used annealing separator (mainly MgO),
Since it is possible to prevent moisture or hydrated water from being brought into the annealing separator, a step for removal is not required during the final annealing, and the final annealing can be shortened accordingly. After finishing annealing, magnetic domain subdivision processing such as laser beam irradiation is performed, and tension coating is further performed.

【0043】[0043]

【実施例】【Example】

実施例1 Si:3.3重量%、酸可溶性Al:0.020重量
%、N:0.008重量%、Mn:0.13重量%、
S:0.007重量%、C:0.05重量%、残部Fe
及び不可避的不純物からなる珪素熱延鋼帯、及びS
i:3.3重量%、酸可溶性Al:0.031重量%、
N:0.008重量%、Mn:0.13重量%、S:
0.007重量%、C:0.05重量%、残部Fe及び
不可避的不純物からなる珪素熱延鋼帯の両鋼帯を110
0℃で2分間焼鈍した後、冷間圧延し、0.23mm厚と
した。
Example 1 Si: 3.3 wt%, acid-soluble Al: 0.020 wt%, N: 0.008 wt%, Mn: 0.13 wt%,
S: 0.007 wt%, C: 0.05 wt%, balance Fe
And hot-rolled silicon steel strip consisting of unavoidable impurities, and S
i: 3.3% by weight, acid-soluble Al: 0.031% by weight,
N: 0.008% by weight, Mn: 0.13% by weight, S:
Both steel strips of the hot-rolled silicon steel strip made of 0.007% by weight, C: 0.05% by weight, the balance Fe and inevitable impurities are 110
After annealing at 0 ° C. for 2 minutes, it was cold rolled to a thickness of 0.23 mm.

【0044】これらの冷延板を脱炭を兼ねるために湿水
雰囲気とした焼鈍炉で820℃で2分間焼鈍し、一次再
結晶させた。次に二次再結晶を安定化させるために、ア
ンモニア雰囲気中で窒化処理を行い、全窒素量を両鋼板
とも175ppm とし、インヒビターを強化した。
These cold-rolled sheets were annealed at 820 ° C. for 2 minutes in an annealing furnace in a wet water atmosphere in order to also serve as decarburization, and primary recrystallization was performed. Next, in order to stabilize the secondary recrystallization, nitriding treatment was performed in an ammonia atmosphere so that the total nitrogen content was 175 ppm in both steel sheets, and the inhibitor was strengthened.

【0045】その後、Al2 3 :100%からなる焼
鈍分離剤を静電塗布し、仕上げ焼鈍の雰囲気を10%N
2 −90%H2 とし150℃/Hrの昇温速度を保ちなが
ら1050℃まで昇温した。1050℃到達後、該温度
で10時間保持した。その後、さらに焼鈍雰囲気を10
0%水素に切り換え、さらに1200℃まで昇温し、該
温度でさらに10時間保持した。仕上げ焼鈍終了後、レ
ーザービームを照射し、リン酸−クロム酸系の張力コー
ティング処理を行った。得られた製品の特性は、表1の
通りである。
After that, an annealing separating agent consisting of Al 2 O 3 : 100% is electrostatically applied, and the atmosphere of finish annealing is set to 10% N.
The temperature was set to 2-90% H 2, and the temperature was raised to 1050 ° C. while maintaining the temperature rising rate of 150 ° C./Hr. After reaching 1050 ° C., the temperature was maintained for 10 hours. After that, the annealing atmosphere is further increased to 10
After switching to 0% hydrogen, the temperature was further raised to 1200 ° C., and the temperature was maintained for 10 hours. After finishing annealing, a laser beam was irradiated to perform a phosphoric acid-chromic acid tension coating process. The characteristics of the obtained product are as shown in Table 1.

【0046】[0046]

【表1】 [Table 1]

【0047】実施例2 Si:3.3重量%、酸可溶性Al:0.020重量
%、N:0.009重量%、Mn:0.13重量%、
S:0.007重量%、C:0.05重量%、残部Fe
及び不可避的不純物からなる珪素熱延鋼帯、及びS
i:3.3重量%、酸可溶性Al:0.031重量%、
N:0.009重量%、Mn:0.13重量%、S:
0.007重量%、C:0.05重量%、残部Fe及び
不可避的不純物からなる珪素熱延鋼帯の両鋼帯を110
0℃で2分間焼鈍した後、冷間圧延し、0.23mm厚と
した。
Example 2 Si: 3.3% by weight, acid-soluble Al: 0.020% by weight, N: 0.009% by weight, Mn: 0.13% by weight,
S: 0.007 wt%, C: 0.05 wt%, balance Fe
And hot-rolled silicon steel strip consisting of unavoidable impurities, and S
i: 3.3% by weight, acid-soluble Al: 0.031% by weight,
N: 0.009% by weight, Mn: 0.13% by weight, S:
Both steel strips of the hot-rolled silicon steel strip made of 0.007% by weight, C: 0.05% by weight, the balance Fe and inevitable impurities are 110
After annealing at 0 ° C. for 2 minutes, it was cold rolled to a thickness of 0.23 mm.

【0048】これらの冷延板を脱炭を兼ねるために湿水
雰囲気とした焼鈍炉で830℃で2分間焼鈍し、一次再
結晶させた。次に二次再結晶を安定化させるために、ア
ンモニア雰囲気中で窒化処理を行い、全窒素量を両鋼板
とも150ppm とし、インヒビターを強化した。
These cold-rolled sheets were annealed at 830 ° C. for 2 minutes in an annealing furnace in a wet water atmosphere in order to also serve as decarburization, and primary recrystallization was performed. Next, in order to stabilize the secondary recrystallization, nitriding treatment was performed in an ammonia atmosphere so that the total nitrogen content was 150 ppm in both steel sheets, and the inhibitor was strengthened.

【0049】その後、Al2 3 :100%からなる焼
鈍分離剤を静電塗布し、仕上げ焼鈍の雰囲気を25%N
2 −75%H2 とし150℃/Hrの昇温速度を保ちなが
ら1050℃まで昇温した。1050℃到達後、該温度
で10時間保持した。
After that, an annealing separator composed of Al 2 O 3 : 100% is electrostatically applied, and the atmosphere of finish annealing is set to 25% N.
The temperature was set to 2-75% H 2, and the temperature was raised to 1050 ° C. while maintaining the rate of temperature increase of 150 ° C./Hr. After reaching 1050 ° C., the temperature was maintained for 10 hours.

【0050】その後、さらに焼鈍雰囲気を100%水素
に切り換え、さらに1200℃まで昇温し、該温度でさ
らに10時間保持した。仕上げ焼鈍終了後、レーザービ
ームを照射し、リン酸−クロム酸系の張力コーティング
処理を行った。得られた製品の特性は、表2の通りであ
る。
Thereafter, the annealing atmosphere was further switched to 100% hydrogen, the temperature was further raised to 1200 ° C., and the temperature was maintained for 10 hours. After finishing annealing, a laser beam was irradiated to perform a phosphoric acid-chromic acid tension coating process. The characteristics of the obtained product are as shown in Table 2.

【0051】[0051]

【表2】 [Table 2]

【0052】[0052]

【発明の効果】本発明により、磁束密度が高く、磁気特
性を阻害する要因である鋼板表面の凹凸の小さい(鏡面
である)方向性電磁鋼板が容易に得られ、レーザービー
ム照射処理等の磁区細分化、張力コーティング処理によ
り極めて低鉄損の磁気材料が提供された。この方向性電
磁鋼板の製造に当たっては鋼板の鏡面化処理が通常の仕
上げ焼鈍炉中で行われるため、極めて容易であり、工業
上の価値は絶大である。
According to the present invention, a grain-oriented electrical steel sheet having a high magnetic flux density and small irregularities on the surface of the steel sheet (which is a mirror surface) which is a factor that obstructs magnetic properties can be easily obtained, and magnetic domains for laser beam irradiation treatment or the like can be obtained. The subdivided, tension-coated treatment provided a magnetic material with extremely low iron loss. In the production of this grain-oriented electrical steel sheet, mirror finishing of the steel sheet is carried out in a normal finish annealing furnace, so that it is extremely easy and its industrial value is enormous.

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

【図1】一次再結晶焼鈍後、アンモニア窒化した鋼板か
ら抽出した析出物の5000倍電子顕微鏡写真である。
FIG. 1 is a 5000 × electron micrograph of precipitates extracted from a steel sheet subjected to ammonia nitridation after primary recrystallization annealing.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 藤井 浩康 富津市新富20−1 新日本製鐵株式会社技 術開発本部内 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Hiroyasu Fujii 20-1 Shintomi, Futtsu City Nippon Steel Corporation Technical Development Division

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】 Si:2.0〜4.8重量%、酸可溶性
Al:0.008〜0.020重量%、N≦0.010
重量%、残部Fe及び不可避的不純物からなる珪素熱延
鋼帯を必要に応じて焼鈍した後、1回または中間焼鈍を
はさむ2回以上の冷間圧延を行い、所定の板厚とし、次
いで一次再結晶焼鈍を行った後焼鈍分離剤を塗布し、仕
上げ焼鈍を施す方向性珪素鋼板の製造において、熱延鋼
帯での酸可溶性AlからN当量のAlを引いた酸可溶性
Alの量を0.010重量%以下とし、一次再結晶焼鈍
後、Al2 3 (アルミナ)を主体とする焼鈍分離剤を
塗布し、中性或いは、還元性雰囲気で仕上げ焼鈍の昇温
速度を50℃/Hr以上で920〜1150℃まで昇温
し、該温度で5時間以上保持することを特徴とするフォ
ルステライト被膜のない高磁束密度方向性珪素鋼板の製
造方法。
1. Si: 2.0 to 4.8% by weight, acid-soluble Al: 0.008 to 0.020% by weight, N ≦ 0.010.
A silicon hot-rolled steel strip consisting of weight%, balance Fe and unavoidable impurities is annealed as required, and then cold rolled once or twice or more with intermediate annealing to obtain a predetermined plate thickness, and then primary In the production of a grain-oriented silicon steel sheet in which a recrystallization annealing is performed and then an annealing separator is applied and finish annealing is performed, the amount of acid-soluble Al obtained by subtracting N equivalent of Al from acid-soluble Al in a hot-rolled steel strip is 0. After the primary recrystallization annealing, the annealing separator containing Al 2 O 3 (alumina) as the main component is applied to the content of 0.010% by weight or less, and the temperature increase rate of the final annealing is 50 ° C./Hr in a neutral or reducing atmosphere. A method for producing a high magnetic flux density grain-oriented silicon steel sheet having no forsterite coating, which comprises heating to 920 to 1150 ° C. and holding the temperature for 5 hours or more.
【請求項2】 熱延鋼帯での酸可溶性AlからN当量の
Alを引いた酸可溶性Alの量を0.010重量%以下
とし、一次再結晶焼鈍後、アンモニアによる窒化処理を
行い、その後、Al2 3 (アルミナ)を主体とする焼
鈍分離剤を塗布し、中性或いは、還元性雰囲気で仕上げ
焼鈍の昇温速度を50℃/Hr以上で920〜1150℃
まで昇温し、該温度で5時間以上保持することを特徴と
する請求項1記載のフォルステライト被膜のない高磁束
密度方向性珪素鋼板の製造方法。
2. The amount of acid-soluble Al obtained by subtracting N equivalent of Al from acid-soluble Al in a hot-rolled steel strip is set to 0.010 wt% or less, and after primary recrystallization annealing, nitriding treatment with ammonia is performed, and thereafter, , An annealing separator mainly composed of Al 2 O 3 (alumina) is applied, and the temperature rising rate of finish annealing in a neutral or reducing atmosphere is 50 ° C./hr or more at 920 to 1150 ° C.
The method for producing a high magnetic flux density grain-oriented silicon steel sheet having no forsterite coating according to claim 1, wherein the temperature is raised to and maintained for 5 hours or more.
【請求項3】 仕上げ焼鈍時の雰囲気中N2 ガスを5%
以上とすることを特徴とする請求項1又は請求項2記載
のフォルステライト被膜のない高磁束密度方向性珪素鋼
板の製造方法。
3. N 2 gas of 5% in the atmosphere during finish annealing.
The method for producing a high magnetic flux density grain-oriented silicon steel sheet having no forsterite coating according to claim 1 or 2, characterized by the above.
【請求項4】 焼鈍分離剤の塗布を静電塗布とすること
を特徴とする請求項1又は請求項2記載のフォルステラ
イト被膜のない高磁束密度方向性珪素鋼板の製造方法。
4. The method for producing a high magnetic flux density grain-oriented silicon steel sheet having no forsterite coating according to claim 1 or 2, wherein the annealing separator is applied electrostatically.
【請求項5】 焼鈍分離剤としてMgO以外のアルカリ
土金属の酸化物を用いることを特徴とする請求項1又は
請求項2記載のフォルステライト被膜のない高磁束密度
方向性珪素鋼板の製造方法。
5. The method for producing a high magnetic flux density grain-oriented silicon steel sheet without a forsterite coating according to claim 1, wherein an oxide of an alkaline earth metal other than MgO is used as the annealing separator.
JP7739092A 1992-03-31 1992-03-31 Production of high magnetic flux density grain-oriented silicon steel sheet free from forsterite film Pending JPH07118743A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7739092A JPH07118743A (en) 1992-03-31 1992-03-31 Production of high magnetic flux density grain-oriented silicon steel sheet free from forsterite film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7739092A JPH07118743A (en) 1992-03-31 1992-03-31 Production of high magnetic flux density grain-oriented silicon steel sheet free from forsterite film

Publications (1)

Publication Number Publication Date
JPH07118743A true JPH07118743A (en) 1995-05-09

Family

ID=13632568

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7739092A Pending JPH07118743A (en) 1992-03-31 1992-03-31 Production of high magnetic flux density grain-oriented silicon steel sheet free from forsterite film

Country Status (1)

Country Link
JP (1) JPH07118743A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100435456B1 (en) * 1999-11-30 2004-06-10 주식회사 포스코 A method for manufacturing low temperature reheated grain-oriented electrical steel sheet having no glass film
EP2377961A4 (en) * 2008-12-16 2017-05-17 Nippon Steel & Sumitomo Metal Corporation Oriented electrical steel sheet, and method for producing same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100435456B1 (en) * 1999-11-30 2004-06-10 주식회사 포스코 A method for manufacturing low temperature reheated grain-oriented electrical steel sheet having no glass film
EP2377961A4 (en) * 2008-12-16 2017-05-17 Nippon Steel & Sumitomo Metal Corporation Oriented electrical steel sheet, and method for producing same

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