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JPH0668133B2 - Method for producing unidirectional silicon steel sheet with excellent magnetic properties - Google Patents
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JPH0668133B2 - Method for producing unidirectional silicon steel sheet with excellent magnetic properties - Google Patents

Method for producing unidirectional silicon steel sheet with excellent magnetic properties

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Publication number
JPH0668133B2
JPH0668133B2 JP62112408A JP11240887A JPH0668133B2 JP H0668133 B2 JPH0668133 B2 JP H0668133B2 JP 62112408 A JP62112408 A JP 62112408A JP 11240887 A JP11240887 A JP 11240887A JP H0668133 B2 JPH0668133 B2 JP H0668133B2
Authority
JP
Japan
Prior art keywords
annealing
steel sheet
temperature
gradient
secondary recrystallization
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.)
Expired - Lifetime
Application number
JP62112408A
Other languages
Japanese (ja)
Other versions
JPS63277716A (en
Inventor
勝生 岩本
雅之 坂口
嘉明 飯田
光正 黒沢
義紀 小林
Original Assignee
川崎製鉄株式会社
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 川崎製鉄株式会社 filed Critical 川崎製鉄株式会社
Priority to JP62112408A priority Critical patent/JPH0668133B2/en
Priority to US07/190,280 priority patent/US4975127A/en
Priority to EP88304050A priority patent/EP0292150B1/en
Priority to DE3888725T priority patent/DE3888725T2/en
Priority to CA000566363A priority patent/CA1332344C/en
Priority to KR1019880005531A priority patent/KR960003173B1/en
Publication of JPS63277716A publication Critical patent/JPS63277716A/en
Publication of JPH0668133B2 publication Critical patent/JPH0668133B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Soft Magnetic Materials (AREA)

Description

【発明の詳細な説明】 (産業上の利用分野) この発明は、磁気特性に優れた一方向性けい素鋼板の製
造方法に関し、磁気特性中でも磁束密度の有利な改善を
図ろうとするものである。
TECHNICAL FIELD The present invention relates to a method for producing a unidirectional silicon steel sheet having excellent magnetic properties, and is intended to advantageously improve the magnetic flux density even in the magnetic properties. .

(従来の技術) 主として変圧器や電動機などの鉄心材料として用いられ
る一方向性けい素鋼板に要求される特性は、一定の磁化
力において得られる磁束密度が高いこと、および一定の
磁束密度を与えた場合にその鉄損が低いことである。通
常これらの代表値としては、磁化力800A/mにおける
磁束密度B8(T:テスラ)および磁束密度1.70T、周
波数50Hzにおける鉄損W17/50(W/Kg)が採用されている。
(Prior art) The characteristics required of unidirectional silicon steel sheets mainly used as iron core materials for transformers and electric motors are that the magnetic flux density obtained at a constant magnetizing force is high and that a constant magnetic flux density is given. That is, the iron loss is low. Usually, magnetic flux density B 8 (T: Tesla) and magnetic flux density 1.70 T at a magnetizing force of 800 A / m and iron loss W 17/50 (W / Kg) at a frequency of 50 Hz are adopted as typical values .

これらの両特性を含む磁気特性を向上させるためには、
現在まで多くの研究がなされ、特に素材の成分、熱間お
よび冷間圧延法、熱処理方法等の改善によってそれぞれ
少なからざる成果が得られている。
In order to improve the magnetic characteristics including both of these characteristics,
Much research has been conducted to date, and in particular, significant improvements have been achieved in each of the components of the material, hot and cold rolling methods, heat treatment methods, and the like.

従来の一方向性けい素鋼板は、通常Si:2.5〜4.5wt%
(以下単に%で示す)を含む低炭素鋼に微量のMn,S,Se,
Sb,Al,Sn,NおよびB等のインヒビター形成元素を添加し
た素材を熱間圧延した後、1回もしくは中間焼鈍を挟む
2回以上の冷間圧延を経て、該冷延鋼板に脱炭を兼ねた
1次再結晶焼鈍を施し、しかるのち最終仕上げ焼鈍工程
において2次再結晶処理を施すことによって2次再結晶
粒を{110}〈001〉方位に高度に集積させると共に、引き
続く鈍化焼鈍によって鋼板中の不純物を除去することに
より良好な磁気特性を得ている。
Conventional unidirectional silicon steel sheet is usually Si: 2.5-4.5wt%
Low carbon steels containing (hereinafter simply expressed as%) contain trace amounts of Mn, S, Se,
After hot-rolling a material to which an inhibitor-forming element such as Sb, Al, Sn, N and B is added, the cold-rolled steel sheet is decarburized through one or two or more cold rollings with intermediate annealing. The secondary recrystallized grains are highly integrated in the {110} <001> orientation by performing the primary recrystallization annealing that also serves as the secondary recrystallization treatment in the final finish annealing step, and by the subsequent annealing annealing. Good magnetic properties are obtained by removing impurities in the steel sheet.

この際、2次再結晶粒の方位が{110}〈001〉へ集積する
ほど鋼板の磁束密度は高くなるが、一方で巨大な2次粒
と成り易く、粒内の磁区幅が増し、渦流損の増加により
鉄損特性が劣化する傾向にあった。そこで2次粒を微細
化することを目的とした努力が種々施され、例えば特開
昭60-89521号公報では、再結晶促進域と地帯域を交互に
設け2次粒の核発生を増しかつ成長を阻止することで2
次粒の微細化を図り鉄損を向上させる方法が提案されて
いる。しかしながら、近年物理的な局所歪の導入による
磁区細分化技術(例えば特開昭58-26410号公報)の確立
により、とくに2次粒を微細化せずとも低鉄損が得られ
るようになったため、技術開発の方向は、磁束密度の向
上に傾いている。
At this time, as the orientation of secondary recrystallized grains accumulates in {110} <001>, the magnetic flux density of the steel sheet becomes higher, but on the other hand, it becomes easy to become huge secondary grains, the magnetic domain width in the grains increases, and the vortex flow increases. The iron loss characteristics tended to deteriorate due to the increase in loss. Therefore, various efforts have been made to reduce the size of the secondary grains. For example, in Japanese Patent Laid-Open No. Sho 60-89521, recrystallization promoting regions and ground zones are alternately provided to increase the nucleation of the secondary grains. 2 by stopping growth
A method has been proposed in which the secondary grain is made finer to improve the iron loss. However, in recent years, with the establishment of a magnetic domain subdivision technique (for example, Japanese Patent Laid-Open No. 58-26410) by introducing a physical local strain, it has become possible to obtain a low iron loss without particularly refining secondary grains. , The direction of technological development is tilted toward the improvement of magnetic flux density.

この点、特公昭58-50295号公報では、2次再結晶時に一
方向の温度勾配を与え、{110}〈001〉方位の2次粒を選
択成長させることで高い磁束密度を得る方法が開示され
ている。この方法は、相対的に高温では2次粒の核発生
速度が大きく、一方低温では粒成長速度が大きいとい
う、2次再結晶に特有の現象を利用したものであり、発
生した2次粒を温度勾配を与えながら加熱することによ
って巨大に粒成長させて、鋼板全体の方向性を向上させ
ようとするものである。
In this regard, Japanese Patent Publication No. 58-50295 discloses a method of obtaining a high magnetic flux density by applying a temperature gradient in one direction during secondary recrystallization and selectively growing secondary grains in the {110} <001> orientation. Has been done. This method utilizes a phenomenon peculiar to secondary recrystallization in which the secondary grain nucleation rate is high at a relatively high temperature, while the grain growth rate is high at a low temperature. By heating while giving a temperature gradient, huge grains are grown to improve the directionality of the entire steel sheet.

(発明が解決しようとする問題点) しかしながら上記の方法は、最初に発生する2時粒につ
いては何ら工夫が施されていないために、最初に核発生
した2次粒の方位によって板全体の特性が大きく影響さ
れるという、言わば偶然性に負うところが大きく、従っ
て必ずしも常に高いB10値が得られるわけではないとこ
ろに問題を残していた。
(Problems to be Solved by the Invention) However, since the above method has not been devised for the 2 o'clock grain that occurs first, the characteristics of the entire plate depend on the orientation of the secondary grain that initially occurs. That is, it was largely influenced by chance, that is, it was a problem that a high B 10 value was not always obtained.

この発明は上記の問題を有利に解決するもので、最初に
高い確率の下で{110}〈001〉すなわちゴス方位粒を核発
生させ、ついでこの方位の2次粒を優先的に成長させる
ことによって、2次粒の方位がゴス方位に高度に揃った
ひいては高磁束密度の一方向性けい素鋼板を安定して製
造することができる有利な方法を提案することを目的と
する。
The present invention advantageously solves the above problem by first nucleating {110} <001>, that is, Goss-oriented grains with high probability, and then preferentially growing secondary grains of this orientation. Accordingly, it is an object of the present invention to propose an advantageous method capable of stably producing secondary grain orientations highly aligned with the Goss orientation and thus stably producing a high magnetic flux density unidirectional silicon steel sheet.

(問題点を解決するための手段) さて発明者らは、以上のような観点から、核発生と粒成
長に関する研究を系統的に進めた。
(Means for Solving Problems) From the above viewpoints, the inventors systematically proceeded with research on nucleation and grain growth.

その結果、鋼板の板面内での集合組織またはインヒビタ
ーによる抑制力を変化させ、より抑制力の強い領域から
温度勾配を与えながら粒成長をさせてやれば、{110}〈0
01〉配向性に優れた2次粒が発生、成長することが判明
した。またこのような抑制力の強い領域では、2次再結
晶が開始する温度TSRは低くなっていることも併せて突
止めた。
As a result, if the inhibitory force due to the texture or the inhibitor in the plate surface of the steel sheet is changed and grain growth is performed while giving a temperature gradient from the region with stronger inhibitory force, {110} 〈0
01> It was found that secondary grains with excellent orientation are generated and grow. Further, it was also found that the temperature T SR at which the secondary recrystallization starts is low in such a region where the suppression force is strong.

この発明は、上記の知見に立脚するものである。The present invention is based on the above findings.

すなわちこの発明は、含けい素鋼スラブを、熱間圧延
し、ついで1回または中間焼鈍を挟む2回以上の冷間圧
延を施して最終板厚としたのち、脱炭・1次再結晶焼鈍
を施し、その後鋼板表面に焼鈍分離剤を塗布してから、
2次再結晶焼鈍ついで純化焼鈍を施す一連の工程によっ
て一方向性けい素鋼板を製造するに当り、 上記の焼鈍分離剤塗布工程において、焼鈍分離剤中にS
およびSeならびにそれらの化合物のうちから選んだ少な
くとも一種を含有させるものとし、鋼板の一端から他端
にかけて、連続的に該分離剤中のSおよび/またはSe濃
度が変化する領域を設けその領域の始めと終わりの濃度
差を0.01%以上とするか、あるいは段階的に該分離剤中
のSおよび/またはSe濃度が0.01%以上なる領域を形成
させるか、いずれか一方または両方の手段により、板幅
方向ないし長手方向にわたって2次再結晶開始温度に勾
配または手段を与え、 しかるのち上記2次再結晶開始温度の勾配よりも大きい
温度勾配の下に、2次再結晶開始温度が低い鋼板端部か
ら2次再結晶を開始させる傾斜焼鈍を施すことを特徴と
する、磁気特性に優れた一方向性けい素鋼板の製造方法
である。
That is, according to the present invention, a silicon steel-containing slab is hot-rolled and then cold-rolled once or twice or more with intermediate annealing to obtain a final plate thickness, followed by decarburization / primary recrystallization annealing. After applying the annealing separator on the steel plate surface,
In producing a unidirectional silicon steel sheet by a series of steps of performing secondary recrystallization annealing and then purifying annealing, in the annealing separating agent applying step, S is added to the annealing separating agent.
And Se and at least one selected from those compounds are contained, and a region where the S and / or Se concentration in the separating agent continuously changes is provided from one end to the other end of the steel sheet. The difference in the concentration between the beginning and the end is set to 0.01% or more, or a region where the concentration of S and / or Se in the separating agent is set to 0.01% or more is formed stepwise, or by one or both means. A gradient or means is given to the secondary recrystallization starting temperature across the width direction or the longitudinal direction, and then, under the temperature gradient larger than the gradient of the secondary recrystallization starting temperature, the steel sheet end portion having a low secondary recrystallization starting temperature Is a method for producing a unidirectional silicon steel sheet having excellent magnetic properties, which is characterized by performing a gradient annealing for starting secondary recrystallization.

以下この発明を具体的に説明する。The present invention will be specifically described below.

まずこの発明の出発素材については、従来公知の一方向
性けい素鋼板の成分たとえば、C:0.005〜0.15%、S
i:0.1〜7.0%およびMn:0.002〜0.15%を含有する他、
インヒビター形成成分としてS:0.005〜0.05%、Se:
0.005〜0.05%、Te:0.003〜0.03%、Sb:0.005〜0.05
%、Sn:0.03〜0.5%、Cu:0.02〜0.3%、Mo:0.005〜
0.05%、B:0.0003〜0.0040%、N:0.001〜0.01%、A
l:0.005〜0.05%およびNb:0.001〜0.05%のうちから
選んだ少なくとも一種を含有する素材いずれもが有利に
適合する。
First, regarding the starting material of the present invention, the components of conventionally known unidirectional silicon steel sheets, for example, C: 0.005 to 0.15%, S
i: 0.1 to 7.0% and Mn: 0.002 to 0.15%,
S: 0.005-0.05% as an inhibitor-forming component, Se:
0.005-0.05%, Te: 0.003-0.03%, Sb: 0.005-0.05
%, Sn: 0.03 to 0.5%, Cu: 0.02 to 0.3%, Mo: 0.005 to
0.05%, B: 0.0003 to 0.0040%, N: 0.001 to 0.01%, A
Any material containing at least one selected from l: 0.005 to 0.05% and Nb: 0.001 to 0.05% is advantageously suitable.

これらの素材は従来公知の製鋼法、たとえば転炉、電気
炉で製鋼され、さらに造塊−分塊法、連続鋳造法、また
はロール急冷法などによってスラブ、シートバーあるい
は直接薄鋼板としたのち、必要に応じて熱間圧延、温間
又は冷間圧延によって含けい素鋼板とする。ついで必要
に応じて均一化焼鈍、さらには中間焼鈍を挟む1回以上
の圧延により最終板厚に仕上げる。これら均一化焼鈍お
よび中間焼鈍は圧延後の結晶組織を均質化する再結晶処
理を目的としていて、通常は800〜1200℃で30秒〜10分
間保持して行う。また仕上げ厚は0.50mm以下とするが2
次再結晶が不安定となる0.23mm以下の薄仕上げ厚におい
てこの発明は特に有効である。
These materials are conventionally known steel-making methods, for example, steelmaking in a converter, an electric furnace, and further slab, sheet bar or directly thin steel sheet by an ingot-segmentation method, continuous casting method, roll quenching method, or the like, If necessary, it is made into a silicon steel sheet by hot rolling, warm rolling or cold rolling. Then, if necessary, homogenizing annealing is performed, and further, one or more rollings with intermediate annealing are performed to finish the final sheet thickness. The homogenizing annealing and the intermediate annealing are intended for the recrystallization treatment for homogenizing the crystal structure after rolling, and are usually carried out at 800 to 1200 ° C. for 30 seconds to 10 minutes. The finish thickness is 0.50mm or less, but 2
The present invention is particularly effective at a thin finish thickness of 0.23 mm or less at which secondary recrystallization becomes unstable.

次に湿水素中で700〜900℃、1〜15分間程度の焼鈍を施
して鋼中Cを除去するとともに、次の焼鈍時にゴス方位
の2次再結晶粒を達成させるのに有利な1次再結晶集合
組織を形成させる。なお出発素材が極低C材である場合
には脱炭焼鈍は不要である。
Next, it is annealed in wet hydrogen at 700 to 900 ° C. for 1 to 15 minutes to remove C in the steel, and at the time of the next annealing, a primary recrystallization grain having a Goss orientation is achieved. Recrystallized texture is formed. If the starting material is an extremely low C material, decarburization annealing is unnecessary.

ついで焼鈍分離剤を塗布するわけであるが、このとき焼
鈍分離剤中にSおよびSeならびにそれらの化合物のうち
から選んだ少なくとも一種を含有させ、この焼鈍分離剤
を塗布する際、鋼板の一端から他端にかけて、連続的に
該分離剤中のSおよび/またはSe濃度が変化する領域を
設けその領域の初めと終わりの濃度差を0.01%以上とす
るか、あるいは段階的に該分離剤中のSおよび/または
Se濃度が0.01%以上なる領域を形成させることにより、
換言すれば連続的および/または段階的に分離剤中のS
および/またはSeの濃度が0.01以上異なる領域(連続的
な場合はその領域の初めと終わりの濃度差を0.01%以上
とする意味である。以下同じ)を、鋼板の幅方向ないし
長手方向にわたって形成させることにより、2次再結晶
開始温度に勾配または段差を与えることが肝要である。
Then, an annealing separator is applied. At this time, at least one selected from S and Se and their compounds is contained in the annealing separator, and when this annealing separator is applied, from one end of the steel sheet. A region where the concentration of S and / or Se in the separating agent changes continuously is provided to the other end, and the concentration difference between the beginning and the end of the region is set to 0.01% or more, or the concentration difference in the separating agent is gradually increased. S and / or
By forming a region where the Se concentration is 0.01% or more,
In other words, S in the separating agent is continuously and / or stepwise.
And / or a region where the concentration of Se differs by 0.01 or more (in the case of continuous, it means that the concentration difference between the beginning and the end of the region is 0.01% or more. The same applies hereinafter) is formed in the width direction or the longitudinal direction of the steel sheet. Therefore, it is important to give a gradient or step to the secondary recrystallization starting temperature.

ここにその後の傾斜焼鈍いよって高度に集積した{110}
〈001〉集合組織を得るためには、2次再結晶開始温度T
SRが低い鋼板端部におけるTSRは他の領域よりも10℃以
上低くする必要があり、そのためには該鋼板端部におけ
るSおよび/またはSeの濃度を、他の領域よりも0.01%
以上濃くする必要がある。
Highly accumulated here due to subsequent tilt annealing {110}
To obtain the <001> texture, the secondary recrystallization start temperature T
The T SR at the steel plate edge where the SR is low needs to be lower than the other regions by 10 ° C. or more, and therefore the concentration of S and / or Se at the steel plate edge is 0.01% lower than that at the other regions.
It is necessary to make it darker.

なおSはSe濃度を調整するにはMgOを主成分とする焼鈍
分離剤を塗布し、乾燥する前にSおよびSeならびにそれ
らの化合物のうちから選んだ少なくとも一種を、板幅方
向ないしは長手方向に連続的および/または階段的に所
望濃度に応じて散布するなどの方法によって容易に達成
できる。
In order to adjust the Se concentration of S, an annealing separator containing MgO as a main component is applied, and before drying, at least one selected from S and Se and their compounds is applied in the width direction or the longitudinal direction. It can be easily achieved by a method such as continuous and / or stepwise spraying according to the desired concentration.

ついで2次再結晶焼鈍を施すが、この2次再結晶焼鈍
は、上記のようにして付与したTSRの勾配よりも大きい
温度勾配の下に、TSRが低い鋼板端部から2次再結晶を
開始させる傾斜焼鈍とする。ここにかような傾斜焼鈍に
おける温度勾配は、単位長さ1cm当り2℃以上とするこ
とが望ましい。
Then, a secondary recrystallization annealing is performed. This secondary recrystallization annealing is performed from the edge of the steel sheet having a low T SR under a temperature gradient larger than the gradient of T SR given as described above. Slanted annealing is started. The temperature gradient in such gradient annealing is preferably 2 ° C. or more per unit length of 1 cm.

しかるのち乾水素雰囲気中で1100〜1250℃、5〜25h
程度の鈍化焼鈍を施す。
Then, in dry hydrogen atmosphere, 1100-1250 ℃, 5-25h
Degree of annealing is applied.

なお上記したような仕上げ焼鈍は、コイル状の鋼帯を処
理するタイプが工業的に実施されているが、鋼板(切板
を含む)を一枚または積層した状態で連続的に焼鈍する
連続タイプも提案されていて、この発明ではどちらのタ
イプも使用できる。
Note that the finish annealing as described above is industrially carried out as a type that processes a coiled steel strip, but it is a continuous type in which one or more steel plates (including cut plates) are continuously annealed. Have been proposed, and either type can be used in the present invention.

また温度勾配の付与に当っては、炉内に温度勾配をもつ
ゾーンを設けることによって容易に達成でき、さらに温
度勾配の付与方向は、鋼板の板幅方向、長さ方向あるい
はその他任意の方向いずれであっても良い。
Further, in providing the temperature gradient, it is possible to easily achieve it by providing a zone having a temperature gradient in the furnace, and the direction of applying the temperature gradient can be the width direction of the steel sheet, the length direction or any other direction. May be

かかる一連の処理を施すことによって磁気特性の効果的
な向上を図ることができるが、この発明では、純化焼鈍
後、鋼板表面に張力付与型の極薄被膜を被成することに
よって磁気特性のより一層の向上を図ることもできる。
Although it is possible to effectively improve the magnetic properties by performing such a series of treatments, in the present invention, the magnetic properties can be more improved by forming a tension-imparting ultra-thin film on the surface of the steel sheet after purification annealing. Further improvement can be achieved.

かかる極薄被膜を被成するためには、まず鈍化焼鈍後の
鋼板表面の非金属物質を除去後、科学研磨あるいは電解
研磨を施して鋼板表面の平滑度を中心線平均粗さRaで0.
4μm以下とする。というのはこれ以上の粗さでは、次
に続く極薄被膜付与によっても鉄損の改善効果が望めな
いからである。
In order to form such an ultra-thin film, first, after removing the non-metallic substances on the steel sheet surface after the annealing annealing, the smoothness of the steel sheet surface is subjected to scientific polishing or electrolytic polishing with a center line average roughness Ra of 0.
4 μm or less. The reason is that if the roughness is higher than this, the effect of improving the iron loss cannot be expected even by the subsequent application of the ultrathin coating.

ついでCVD法やPVD法(イオンプレーティングやイオンイ
ンプランテイション)などの蒸着法によって、Ti,Nb,S
i,V,Cr,Al,Mn,B,Ni,Co,Mo,Zr,Ta,Hf,Wの窒化物および/
又は炭化物なにびにAl,Si,Mn,Mg,Zn,Tiの酸化物のうち
から選んだ少くとも一種より主として成る極薄被膜を鋼
板表面に強固に被成するのである。
Then, Ti, Nb, S are deposited by a vapor deposition method such as CVD method or PVD method (ion plating or ion implantation).
i, V, Cr, Al, Mn, B, Ni, Co, Mo, Zr, Ta, Hf, W nitride and /
Alternatively, the surface of the steel sheet is strongly coated with an ultrathin coating mainly composed of at least one selected from carbides, oxides of Al, Si, Mn, Mg, Zn and Ti.

なおかかる被膜の材質としては、上掲したもののほか、
熱膨脹係数が低く鋼板に強固に付着するものであれば何
であってもよい。
In addition to the above listed materials,
Any material having a low coefficient of thermal expansion and firmly adhering to the steel sheet may be used.

さらに必要により常法に従って好ましくは張力付与型低
熱膨脹の上塗り絶縁被膜を被成し、レーザー照射、プラ
ズマジェット照射、放電加工、けがき法およびボールペ
ン加工法等の磁区細分化技術を適用する。
Further, if necessary, a tension-imparting low thermal expansion top coat insulating film is preferably formed according to a conventional method, and a magnetic domain subdivision technique such as laser irradiation, plasma jet irradiation, electric discharge machining, scribing method and ballpoint pen processing method is applied.

(作用) TSRの低い領域からTSRの勾配より大きい温度勾配を付与
しながら鋼板を加熱すると、まず鋼板の端部がTSR以上
の温度に上昇し、配向性の良い粒が少量核発生して、2
次再結晶領域を形成する。かような2次再結晶領域とま
だTSRに達していない領域との間に、狭い範囲で1次再
結晶組織と2次再結晶組織が混在した領域が生じる。そ
して鋼板の温度が上昇するにつれてかかる領域は高温測
へと移動を続けることになり、それに伴って2次再結晶
領域が拡大して行き、粒成長が起こる。
(Operation) When heating the steel sheet while applying large temperature gradient than the slope of the T SR from low T SR regions, first end portion of the steel sheet increases to T SR a temperature above the orientation with good grain small amount nucleation Then 2
Next, a recrystallized region is formed. Between such a secondary recrystallization region and not yet reached the T SR region, a region where the primary recrystallized structure and a secondary recrystallized structure are mixed in a narrow range results. Then, as the temperature of the steel sheet rises, such a region will continue to move to pyrometry, and along with that, the secondary recrystallization region will expand and grain growth will occur.

前述したように、S、Se濃度が高く抑制力の強い領域か
らゴス方位粒が発生し易いので、上記のような温度勾配
の付与下に昇熱してやれば、通常の均一昇熱の場合に比
較して、より確実にゴス方位粒を発生させることがで
き、また最初の結晶方位粒がスムーズに高温側へ移項す
るので、大きな2次粒を得る上でも有利である。
As described above, since Goss-oriented grains are likely to be generated from the region where the S and Se concentrations are high and the suppressing force is strong, if the heat is raised under the temperature gradient as described above, it will be compared to the case of normal uniform heat raising. Then, the Goss-oriented grains can be generated more reliably, and the first crystal-oriented grains are smoothly transferred to the high temperature side, which is also advantageous in obtaining large secondary grains.

そしてこの成長を通じて、1次再結晶と2次再結晶の境
界領域の温度は比較的一定に保たれる。
Through this growth, the temperature in the boundary region between the primary recrystallization and the secondary recrystallization is kept relatively constant.

発明者らの実験によると2次再結晶粒の最初の核生成場
所と遅滞部でのTSRの温度差が10℃以上で、しかも温度
勾配が2℃/cm以上の場合にB10の改善により顕著な効
果が見られることが判明した。
According to the experiments conducted by the inventors, the improvement of B 10 is achieved when the temperature difference between T SR at the initial nucleation site of the secondary recrystallized grain and the delayed portion is 10 ° C or more and the temperature gradient is 2 ° C / cm or more. It was found that a remarkable effect was seen.

温度勾配を付与しながら2次再結晶を進行させた場合、
2次再結晶がおこる温度は鋼板の種類や昇熱条件によっ
て一定ではなく、その温度範囲を限定することは出来な
いが、例えばMnSeとSbをインヒビターとする方向性けい
素鋼板の場合850〜950℃の範囲にあり、この発明におい
てはこの境界領域に温度勾配を設ければ良いのであっ
て、その前後は従来採用している処理条件を採用しても
良く、もちろん温度勾配を設けてもよい。
When the secondary recrystallization is advanced while applying a temperature gradient,
The temperature at which secondary recrystallization occurs is not constant depending on the type of steel sheet and the heating conditions, and its temperature range cannot be limited. For example, in the case of grain-oriented silicon steel sheets with MnSe and Sb as inhibitors, 850-950 In the present invention, a temperature gradient may be provided in this boundary region. Before and after that, the treatment conditions conventionally employed may be adopted, and of course, the temperature gradient may be provided. .

かくして磁気特性とくに磁束密度に優れた一方向性けい
素鋼板を安定して得ることができるようになったのであ
る。
Thus, it has become possible to stably obtain a unidirectional silicon steel sheet having excellent magnetic properties, particularly magnetic flux density.

(実施例) 実施例1 C:0.045%、Si:3.30%、Mn:0.080%、S:0.003
%、Se:0.025%およびSb:0.025%を含有し、残部実質
的にFeの組成になる3.0mm厚の熱延板に、大気中で900
℃、2分の焼鈍を施したのち、酸洗して、0.75mm厚に冷
延し、続いて950℃、2分の中間焼鈍を施して0.30mmの
最終板厚に仕上げた。ついで脱脂後、湿水素中で835
℃、4分の脱炭焼鈍を施したのち、MgOを主成分とする
焼鈍分離剤を塗布、乾燥してからBox型仕上げ焼鈍炉に
おいてH2雰囲気中で840℃、30時間の2次再結晶焼鈍、
ついで1200℃で10時間の鈍化焼鈍を施した。
(Example) Example 1 C: 0.045%, Si: 3.30%, Mn: 0.080%, S: 0.003
%, Se: 0.025% and Sb: 0.025%, and the balance of the composition is essentially Fe.
After annealing at 2 ° C. for 2 minutes, it was pickled and cold rolled to a thickness of 0.75 mm, followed by intermediate annealing at 950 ° C. for 2 minutes to give a final sheet thickness of 0.30 mm. Then, after degreasing, 835 in wet hydrogen
After decarburization annealing at 4 ℃ for 4 minutes, apply an annealing separator containing MgO as the main component, dry it, and then perform secondary recrystallization in a Box-type finishing annealing furnace at 840 ℃ in a H 2 atmosphere for 30 hours. Annealing,
Then, annealing was performed at 1200 ° C. for 10 hours.

ここに上記の焼鈍分離剤塗布工程において、MgOを主成
分とする焼鈍分離剤を塗布した後、直ちに分離剤中のS
濃度が板幅方向の一端部は0%、他端部は5.0%と板幅
方向に連続して濃度が変化するように硫酸マグネシウム
を散布した。その後乾燥させてから20時間保定してコイ
ル幅方向の2次再結晶開始温度TSRを調べたところ、一
端部は895℃、中央部は875℃、他端部は860℃であった
ので、鋼板一端部から他端部にかけて温度勾配が1cmあ
たり3℃となるよう調整したBox型仕上げ焼鈍炉で、800
〜900℃間を3℃/hで徐熱昇温し、ついで1200℃、10
時間の最終仕上げ焼鈍を施した。
In the annealing separating agent applying step described above, immediately after the annealing separating agent containing MgO as a main component is applied, S in the separating agent is immediately applied.
Magnesium sulfate was sprayed so that the concentration was 0% at one end in the plate width direction and 5.0% at the other end so that the concentration continuously changed in the plate width direction. After drying, it was held for 20 hours and the secondary recrystallization start temperature T SR in the coil width direction was examined. One end was 895 ° C, the center was 875 ° C, and the other end was 860 ° C. A Box-type finishing annealing furnace, in which the temperature gradient from one end to the other end of the steel plate was adjusted to 3 ° C per cm, 800
The temperature is gradually heated up to 900 ℃ at 3 ℃ / h, then 1200 ℃, 10
A final finish anneal of time was applied.

かくして得られた製品板の磁気特性B10値について調べ
た結果を以下に示す。
The results of examining the magnetic property B 10 value of the product plate thus obtained are shown below.

なお比較のため硫酸マグネシウムを散布しない通常の工
程によって製造した製品板についての調査結果も併せて
示す。
For comparison, the results of the survey on the product sheet manufactured by the usual process without spraying magnesium sulfate are also shown.

10(T) 実施例 1.956 比較例 1.908 実施例2 C:0.054%、Si:3.28%、Mn:0.087%、S:0.028
%、sol Al:0.033%およびN:0.0080%を含有する組
成になる2.4mm厚の熱延板を、1000℃、2分間焼鈍後、
酸洗し、ついで0.27mm厚に仕上げ冷延した後、脱脂し、
その後湿水素中で脱炭焼鈍後、MgOを主成分とする焼鈍
分離剤を塗布してから、乾燥し、H2雰囲気中で20℃/hの
昇温速度で1200℃まで昇熱し、ついで10時間保持の仕上
げ焼鈍を施した。
B 10 (T) Example 1.956 Comparative Example 1.908 Example 2 C: 0.054%, Si: 3.28%, Mn: 0.087%, S: 0.028
%, Sol Al: 0.033% and N: 0.0080%, a 2.4 mm thick hot-rolled sheet having a composition of 1000 ° C. for 2 minutes was annealed.
After pickling, finishing cold rolling to 0.27 mm thickness, degreasing,
Then, after decarburization annealing in wet hydrogen, an annealing separating agent containing MgO as a main component is applied, followed by drying and heating to 1200 ° C in a H 2 atmosphere at a heating rate of 20 ° C / h, and then 10 A time-holding finish annealing was performed.

ここに上記の焼鈍分離剤塗布工程においてMgOを主成分
とする焼鈍分離剤を塗布したのち、直ちに分離剤中のS
濃度が板幅1000mmの板幅方向端部100mmは0%、残る板
幅900mmのひき続く1/2は1.50%、残る他端部の450mmは
3.5%と階段的に変化するように硫酸ストロンチウムを
散布したのち乾燥した。
After applying the annealing separating agent containing MgO as a main component in the above-mentioned annealing separating agent applying step, immediately after the S separating agent in the separating agent is applied.
The density is 0% when the width of the board is 1000 mm and the width of the edge is 100 mm. The remaining 1/2 of the width of 900 mm is 1.50% and the remaining edge is 450 mm.
Strontium sulfate was sprayed so as to change stepwise at 3.5% and then dried.

コイル幅方向のTSRを調べるために、20時間保定の焼鈍
を実施したところ、分離剤中にS量が0%の一端部は10
90℃、S量1.50%の中央部は1040℃、S量3.5%の残る
他端部は1005℃であったので、分離剤中のS量が3.5%
の端部を下部にして、炉床ヒーター設置式で1cmあたり
5℃の温度勾配をもつBox型仕上げ焼鈍炉で、H2雰囲気
中において20℃/hの昇温速度で1200℃まで昇熱し、つい
で10時間保持の仕上げ焼鈍を施した。
In order to examine T SR in the coil width direction, a 20-hour retention annealing was performed.
90 ° C, the central part with 1.50% S content was 1040 ° C and the other end with 3.5% S content was 1005 ° C, so the S content in the separating agent was 3.5%.
With the end of the as the lower part, with a hearth heater installed type, a Box-type finishing annealing furnace having a temperature gradient of 5 ° C. per 1 cm, heats up to 1200 ° C. in a H 2 atmosphere at a heating rate of 20 ° C./h, Then, finish annealing was performed for 10 hours.

かくして得られた製品板の磁気特性B10値について調べ
た結果を以下に示す。なお比較のため常法に従って得た
製品板についての調査結果も併せて示した。
The results of examining the magnetic property B 10 value of the product plate thus obtained are shown below. For comparison, the results of investigations on product plates obtained according to the usual method are also shown.

10(T) 実施例 1.988 比較例 1.933 実施例3 C:0.046%、Si:3.43%、Mn:0.082%、S:0.018
%、Se:0.026%、Sb:0.018%およびSn:0.035%を含
む組成になる2.0mm厚の熱延板を、935℃、2分間焼鈍
後、酸洗し、0.60mm厚に中間冷延したのち、950℃、2
分の中間焼鈍後、0.23mm厚の最終板厚に仕上げ冷延し
た。次に脱脂後、湿水素中で脱炭焼鈍後、MgOを主成分
とする焼鈍分離剤を塗布、乾燥したのち、H2雰囲気中で
800〜900℃間を5℃/hの速度で昇熱し、ついで1200℃に
10時間保定する仕上げ焼鈍を施した。
B 10 (T) Example 1.988 Comparative Example 1.933 Example 3 C: 0.046%, Si: 3.43%, Mn: 0.082%, S: 0.018
%, Se: 0.026%, Sb: 0.018% and Sn: 0.035%, a 2.0 mm thick hot-rolled sheet was annealed at 935 ° C. for 2 minutes, pickled, and cold-rolled to 0.60 mm in thickness. After that, 950 ℃, 2
After the intermediate annealing for a minute, the product was finished and cold rolled to a final plate thickness of 0.23 mm. Next, after degreasing, decarburization annealing in wet hydrogen, applying an annealing separator containing MgO as the main component, and drying, then in an H 2 atmosphere.
The temperature is raised from 800 to 900 ℃ at a rate of 5 ℃ / h, then to 1200 ℃.
Finish annealing was performed for 10 hours.

ここに上記の焼鈍分離剤塗布工程においてMgOを主成分
とする焼鈍分離剤を塗布後、直ちに硫化鉄と無水セレン
酸を、板幅方向端部はS+Se量が0%とし、板幅方向1/
3部にかけて連続的に濃度を増して散布し、1/3部におけ
るS+Se量は1%とし、板幅方向1/3〜2/3にかけてはS
+Seを1%とし、残る板幅2/3から他端部にかけては連
続的に濃度を増して他端部のS+Se量を3.5%とした
後、直ちに乾燥した。20時間保定したときの2次再結晶
開始温度について調べたところ、分離剤中のS+Se量が
0%の端部は900℃、中央部は878℃、S+Se量が3.5%
の他端部は865℃であったので、鋼板一端部から他端部
にかけて温度勾配が1cmあたり3.5℃になるような仕上
げ焼鈍炉中で800℃〜950℃間を、5℃/hの昇温速度で昇
熱し、ついで乾水素中で1200℃、10時間の仕上げ焼鈍を
施した。
Immediately after applying the annealing separating agent containing MgO as the main component in the above-mentioned annealing separating agent applying step, iron sulfide and selenium anhydride were immediately added, and S + Se amount was 0% at the end in the plate width direction, and 1 / in the plate width direction.
The concentration is continuously increased and sprayed over 3 parts, and the amount of S + Se in 1/3 part is 1%, and S over the plate width direction 1/3 to 2/3.
+ Se was set to 1%, the concentration was continuously increased from the remaining plate width 2/3 to the other end to make the amount of S + Se at the other end 3.5%, and then immediately dried. When the secondary recrystallization starting temperature after holding for 20 hours was investigated, the edge of S + Se in the separating agent was 0%, 900 ° C, the center was 878 ° C, and the amount of S + Se was 3.5%.
Since the other end of the steel plate was 865 ° C, the temperature gradient from the one end to the other end of the steel plate was 3.5 ° C per cm in the finishing annealing furnace. It was heated at a temperature rate and then subjected to finish annealing in dry hydrogen at 1200 ° C for 10 hours.

かくして得られた製品板の磁気特性B10について調べた
結果を、従来法により得られたものと比較して以下に示
す。
The results of examining the magnetic properties B 10 of the product plate thus obtained are shown below in comparison with those obtained by the conventional method.

10(T) 実施例 1.968 比較例 1.913 実施例4 C:0.054%、Si:3.28%、Mn:0.087%、S:0.028
%、Sn:0.038%、solAl:0.033%およびN:0.0080%
を含有する組成になる2.0mm厚の熱延板を、1025℃、1
分で焼鈍後、酸洗し、ついで0.19mm厚に冷延した後、脱
脂し、湿水素中で脱炭、1次再結晶焼鈍後、MgOを主成
分とする焼鈍分離剤を塗布したのち、950℃までは30℃/
h、950℃からは5℃/hの昇温速度で1100℃まで昇熱後、
水素雰囲気中で1200℃、10hの鈍化焼鈍を施した。
B 10 (T) Example 1.968 Comparative Example 1.913 Example 4 C: 0.054%, Si: 3.28%, Mn: 0.087%, S: 0.028
%, Sn: 0.038%, solAl: 0.033% and N: 0.0080%
The hot-rolled sheet with a thickness of 2.0 mm containing 10
After annealing in minutes, pickling, then cold rolling to a thickness of 0.19 mm, degreasing, decarburization in wet hydrogen, primary recrystallization annealing, and then applying an annealing separator containing MgO as a main component, 30 ° C / up to 950 ° C
h, after heating from 950 ℃ to 1100 ℃ at a heating rate of 5 ℃ / h,
Annealing annealing was performed at 1200 ° C for 10 hours in a hydrogen atmosphere.

上記の焼鈍分離剤塗布工程において、MgOを主成分とす
る分離剤を塗布したのち、直ちにセレンを板幅方向の端
部は2.0%、板幅方向の1/3のところのSe量は1.0%にな
るように連続的に濃度を減少し、板幅方向1/3〜2/3は1.
0%のまま、残る2/3からもう一方の板幅端部にかけては
Se量が0%になるように連続的に濃度を減じて散布し
た。さらに、硫酸マグネシウムを長手方向にS量が2.0
%から板幅の長さのところで0%になるように連続して
濃度が減少するように散布し、直ちに乾燥した。
In the above-mentioned annealing separating agent applying step, after applying the separating agent containing MgO as a main component, immediately selenium is applied at 2.0% in the plate width direction end portion, and the Se amount at 1/3 in the plate width direction is 1.0%. The concentration is continuously reduced so that 1/3 to 2/3 is 1.
0%, from the remaining 2/3 to the other plate width edge
The concentration was continuously reduced and sprayed so that the Se amount became 0%. Furthermore, magnesium sulfate has an S content of 2.0 in the longitudinal direction.
% To 0% at the length of the plate width, the concentration was continuously sprayed so as to decrease, and immediately dried.

20時間保定して2次再結晶開始温度を調べたところ、板
幅方向と長手方向でS+S量が合計で4%のところは98
7℃、3%のところは1004℃、2%のところは1023℃、
1%のところは1046℃、0%のところは1073℃であった
ので、鋼板端部から他端部にかけて温度勾配が3℃にな
るような仕上げ焼鈍炉で950℃から1100℃までを、5℃/
hの昇温速度で昇熱し、ついで水素雰囲気中で1200℃、1
0hの仕上焼鈍を施した。
When the secondary recrystallization start temperature was examined after holding for 20 hours, it was 98 when the total S + S amount in the width direction and the longitudinal direction was 4%.
7 ° C, 3% place is 1004 ° C, 2% place is 1023 ° C,
Since it was 1046 ° C at 1% and 1073 ° C at 0%, a finishing annealing furnace with a temperature gradient of 3 ° C from the edge of the steel plate to the other edge was operated at 950 ° C to 1100 ° C. ℃ /
The temperature is raised at a heating rate of h and then in a hydrogen atmosphere at 1200 ° C for 1
Finish annealing was performed for 0 h.

かくして得られた一方向性けい素鋼板の磁気特性B
8(T)について調べた結果を以下に示す。
Magnetic properties B of the thus obtained unidirectional silicon steel sheet B
The results of examining 8 (T) are shown below.

なお比較のためにSe,Sを散布しない通常の工程によっ
て製造した製品板についての調査結果も併せて示す。
For comparison, the results of investigations on product plates manufactured by a normal process in which Se and S are not dispersed are also shown.

8(T) 実施例 1.992 比較例 1.933 実施例5 C:0.040%、Si:3.35%、Mn:0.070%、Se:0.020%
およびSb:0.025%を含む組成になる2.2mm厚の熱延板
を、950℃、2分で焼鈍後、酸洗し、0.60mm厚に中間冷
延し、970℃、1.5分の中間焼鈍後、0.22mm厚に冷延した
のち、脱脂後、湿水素中で脱炭、1次再結晶焼鈍を施
し、ついでMgOを主成分とする焼鈍分離剤を塗布乾燥し
たのち、820〜925℃間を2.5℃/hの昇温速度で加熱した
のち、水素雰囲気中で1200℃、10hの鈍化焼鈍を施し
た。ついで酸洗により酸化被膜を除去してから3%HFと
H2O2液中で化学研摩を施して鏡面仕上げとした後、次に
CVD法によりTiCl4(70%)ガス雰囲気中で処理して鋼板表
面に0.8μm厚のTiNを被膜形成させた。
B 8 (T) Example 1.992 Comparative Example 1.933 Example 5 C: 0.040%, Si: 3.35%, Mn: 0.070%, Se: 0.020%
And 2.2 mm thick hot rolled sheet with a composition containing Sb: 0.025% are annealed at 950 ° C. for 2 minutes, pickled, intermediate cold rolled to a thickness of 0.60 mm, and annealed at 970 ° C. for 1.5 minutes. After cold rolling to 0.22 mm thickness, degreasing, decarburization in wet hydrogen, primary recrystallization annealing, then applying an annealing separator containing MgO as the main component and drying, and then between 820 and 925 ℃ After heating at a temperature rising rate of 2.5 ° C / h, annealing was performed at 1200 ° C for 10 hours in a hydrogen atmosphere. Then remove the oxide film by pickling and add 3% HF
After chemical polishing in H 2 O 2 solution to give a mirror finish,
A TiCl 4 (70%) gas atmosphere was used for CVD to form a 0.8 μm thick TiN film on the surface of the steel sheet.

上記の焼鈍分離剤塗布工程においてMgOを主成分とする
分離剤を塗布後、直ちに硫化鉄を板幅方向端部1/4は0
%に、板幅方向2/4は0.75%に、板幅方向3/4は1.5%
に、残る他端部は2.25%になるように段階的に散布した
のち、直ちに乾燥した。
Immediately after applying the separating agent containing MgO as the main component in the above-mentioned annealing separating agent applying step, iron sulfide was immediately applied to the edge portion 1/4 in the width direction of 0
% In the width direction 2/4 to 0.75% and in the width direction 3/4 1.5%
Then, the remaining other end was sprayed stepwise so as to be 2.25% and then immediately dried.

20時間保定後の2次再結晶開始温度を調べたところ、分
離剤中のS量0%の端部1/4は903℃、2/4部は888℃、3/
4部は873℃、残る他端部は858℃であったので、鋼板端
部から他端部にかけて温度勾配が1cmあたり2.5℃とな
るよう調整したBox型仕上げ焼鈍炉で、820〜925℃間を
2.5℃/hの昇温速度で昇熱し、ついで1200℃,10hの鈍化
焼鈍を水素雰囲気中で実施した。
When the secondary recrystallization start temperature after 20 hours retention was examined, the end 1/4 with S content of 0% in the separating agent was 903 ° C, 2/4 part was 888 ° C, 3 /
Since 4 parts were 873 ° C and the remaining other end was 858 ° C, it was a Box-type finishing annealing furnace adjusted to have a temperature gradient of 2.5 ° C per cm from the steel plate end to the other end, between 820 and 925 ° C. To
The temperature was raised at a heating rate of 2.5 ° C / h, and then annealing was performed at 1200 ° C for 10 hours in a hydrogen atmosphere.

かくして得られた一方向性けい素鋼板の磁気特性B
8(T)とw10/50(W/Kg)について調べた結果は、次のと
おりであった。
Magnetic properties B of the thus obtained unidirectional silicon steel sheet B
The results of examining 8 (T) and w 10/50 (W / Kg) were as follows.

なお比較のため硫化鉄を散布しない通常の工程によって
製造した製品板についての調査結果も併せて示す。
For comparison, the results of an investigation of a product plate manufactured by a normal process in which iron sulfide is not sprayed are also shown.

8(T) w10/50(W/Kg) 実施例 1.988 0.60 比較例 1.902 0.89 実施例6 C:0.054%、Si:3.28%、Mn:0.028%、solAl:0.033
%およびN:0.0080%を含有する組成になる2.4mm厚の
熱延板を、1000℃、2分で焼鈍後、酸洗し、次いで0.29
mm厚に冷延した後、脱脂し、湿水素中で脱端、1次再結
晶焼鈍後、MgOを主成分とする焼鈍分離剤を塗布したの
ち、945℃までは27℃/h、945℃からは5℃/hの昇温速度
で1100℃まで昇熱後、水素雰囲気中で1200℃、10hの鈍
化焼鈍を施し、さらに絶縁コーティング後、レーザー照
射により局部歪を導入した。
B 8 (T) w 10/50 (W / Kg) Example 1.988 0.60 Comparative Example 1.902 0.89 Example 6 C: 0.054%, Si: 3.28%, Mn: 0.028%, solAl: 0.033
% And N: 0.0080%, a 2.4 mm thick hot-rolled sheet is annealed at 1000 ° C. for 2 minutes, pickled, and then 0.29
After cold rolling to mm thickness, degreasing, de-edgeing in wet hydrogen, primary recrystallization annealing, and then applying an annealing separator containing MgO as the main component, 27 ℃ / h up to 945 ℃, 945 ℃ After heating up to 1100 ° C. at a temperature rising rate of 5 ° C./h, annealing annealing was performed at 1200 ° C. for 10 hours in a hydrogen atmosphere, and after insulating coating, local strain was introduced by laser irradiation.

上記の焼鈍分離剤塗布工程においてMgOを主成分とする
分離剤を塗布したのち、直ちに、硫酸マグネシウムと硫
酸ストロンチウムを、コイル一端部のS量が0%、他端
部が4.5%と連続して濃度が増すように散布した。その
後直ちに乾燥させ、20時間保定後の2次再結晶開始温度
を調べたところ、分離剤中のS量0%の板幅端部は1075
℃、他端部は975℃であったので、鋼板一端部から他端
部にかけて温度勾配が4℃となるように調整したBox型
仕上げ焼鈍炉で、945℃〜1100℃間を5℃/hの昇温速度
で徐熱昇温し、ついで水素雰囲気中で1200℃、10hの鈍
化焼鈍を施した。
After applying the separating agent containing MgO as the main component in the above-mentioned annealing separating agent applying step, magnesium sulfate and strontium sulfate were immediately added to the coil so that the S content at one end was 0% and the other end was 4.5%. Sprayed to increase the concentration. Immediately after that, it was dried, and the temperature at which secondary recrystallization started after 20 hours of retention was examined.
Since the temperature was ℃ and the other end was 975 ℃, it was a Box-type finishing annealing furnace adjusted to have a temperature gradient of 4 ℃ from one end to the other end of the steel plate. The temperature was gradually increased at a heating rate of 1, and then annealing was performed at 1200 ° C. for 10 hours in a hydrogen atmosphere.

かくして得られた一方向性けい素鋼板の磁気特性B
8(T)とw10/50(W/Kg)について調べた結果は以下のと
おりであった。
Magnetic properties B of the thus obtained unidirectional silicon steel sheet B
The results of examining 8 (T) and w 10/50 (W / Kg) were as follows.

なお、比較のため、硫化マグネシウムと硫酸ストロンチ
ウムを散布しない通常の工程によって製造した製品板に
ついての調査結果も併せて示す。
In addition, for comparison, the results of an examination of a product plate manufactured by a normal process in which magnesium sulfide and strontium sulfate are not sprayed are also shown.

8(T) w10/50(W/Kg) 実施例 2.034 0.76 比較例 1.941 0.99 (発明の効果) かくしてこの発明によれば、一方向性けい素鋼板の製造
において、2次再結晶焼鈍に先立って焼鈍分離剤を塗布
する際、SおよびSeならびにそれらの化合物のうちから
選んだ少なくとも一種を、鋼板の一端部から他の部分に
かけて連続的および/または階段的にSおよびSeの濃度
に0.01%以上の差異をもうけて、1次再結晶開始温度T
SRに10℃以上の勾配を与え、さらに、2次再結晶を進行
させる際、TSRよりも大きい温度勾配の下に鋼板の一端
部から鋼板に加える温度勾配が好ましくは1cm当り2℃
以上となる傾斜焼鈍を施すことによって、著しくB10
の高い一方向性けい素鋼板を安定して得ることができ
る。
B 8 (T) w 10/50 (W / Kg) Example 2.034 0.76 Comparative Example 1.941 0.99 (Effect of the Invention) Thus, according to the present invention, the secondary recrystallization annealing is performed in the production of the grain-oriented silicon steel sheet. When the annealing separator is applied in advance, at least one selected from S and Se and their compounds is added to the concentration of S and Se of 0.01 or more continuously and / or stepwise from one end of the steel sheet to the other. %, The primary recrystallization start temperature T
When a gradient of 10 ° C or more is applied to SR and the secondary recrystallization proceeds, the temperature gradient applied to the steel sheet from one end of the steel sheet is preferably 2 ° C / cm under a temperature gradient larger than T SR.
By performing the gradient annealing as described above, it is possible to stably obtain a unidirectional silicon steel sheet having a remarkably high B 10 value.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 黒沢 光正 千葉県千葉市川崎町1番地 川崎製鉄株式 会社技術研究本部内 (72)発明者 小林 義紀 千葉県千葉市川崎町1番地 川崎製鉄株式 会社技術研究本部内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Mitsumasa Kurosawa 1 Kawasaki-cho, Chiba-shi, Chiba Kawasaki Steel Co., Ltd. Technical Research Division (72) Yoshinori Kobayashi 1 Kawasaki-cho, Chiba-shi Kawasaki Steel Co., Ltd. Research headquarters

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】含けい素鋼スラブを、熱間圧延し、ついで
1回または中間焼鈍を挟む2回以上の冷間圧延を施して
最終板厚としたのち、脱炭・1次再結晶焼鈍を施し、そ
の後鋼板表面に焼鈍分離剤を塗布してから、2次再結晶
焼鈍ついで純化焼鈍を施す一連の工程によって一方向性
けい素鋼板を製造するに当り、 上記の焼鈍分離剤塗布工程において、焼鈍分離剤中にS
およびSeならびにそれらの化合物のうちから選んだ少な
くとも一種を含有させるものとし、鋼板の一端から他端
にかけて、連続的に該分離剤中のSおよび/またはSe濃
度が変化する領域を設けその領域の初めと終わりの濃度
差を0.01%以上とするか、あるいは段階的に該分離剤中
のSおよび/またはSe濃度が0.01%以上なる領域を形成
させるか、いずれか一方または両方の手段により、板幅
方向ないし長手方向にわたって2次再結晶開始温度に勾
配または段差を与え、 しかるのち上記2次再結晶開始温度の勾配よりも大きい
温度勾配の下に、2次再結晶開始温度が低い鋼板端部か
ら2次再結晶を開始させる傾斜焼鈍を施すことを特徴と
する、磁気特性に優れた一方向性けい素鋼板の製造方
法。
1. A slab containing silicon steel is hot-rolled, and then cold-rolled once or twice or more with intermediate annealing to obtain a final plate thickness, followed by decarburization / primary recrystallization annealing. In order to manufacture a unidirectional silicon steel sheet by a series of steps in which the annealing separation agent is applied to the surface of the steel sheet, and then secondary recrystallization annealing and then purification annealing are performed, , S in the annealing separator
And Se and at least one selected from those compounds are contained, and a region where the S and / or Se concentration in the separating agent continuously changes is provided from one end to the other end of the steel sheet. The difference in concentration between the beginning and the end is set to 0.01% or more, or a region where the S and / or Se concentration in the separating agent is set to 0.01% or more is formed stepwise, either one or both means, A gradient or step is given to the secondary recrystallization start temperature across the width direction or the longitudinal direction, and then, under the temperature gradient larger than the gradient of the secondary recrystallization start temperature, the steel plate end portion having a low secondary recrystallization start temperature A method for producing a unidirectional silicon steel sheet having excellent magnetic properties, which comprises performing a gradient anneal for initiating secondary recrystallization.
【請求項2】傾斜焼鈍における温度勾配が、単位長さ1
cm当り2℃以上である特許請求の範囲第1項記載の方
法。
2. The temperature gradient in the gradient annealing has a unit length of 1
The method according to claim 1, wherein the temperature is 2 ° C or more per cm.
JP62112408A 1987-05-11 1987-05-11 Method for producing unidirectional silicon steel sheet with excellent magnetic properties Expired - Lifetime JPH0668133B2 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
JP62112408A JPH0668133B2 (en) 1987-05-11 1987-05-11 Method for producing unidirectional silicon steel sheet with excellent magnetic properties
US07/190,280 US4975127A (en) 1987-05-11 1988-05-04 Method of producing grain oriented silicon steel sheets having magnetic properties
EP88304050A EP0292150B1 (en) 1987-05-11 1988-05-05 Method of producing grain oriented silicon steel sheets having excellent magnetic properties
DE3888725T DE3888725T2 (en) 1987-05-11 1988-05-05 Process for the production of grain-oriented silicon steel sheets with excellent magnetic properties.
CA000566363A CA1332344C (en) 1987-05-11 1988-05-10 Method of producing grain oriented silicon steel sheets having excellent magnetic properties
KR1019880005531A KR960003173B1 (en) 1987-05-11 1988-05-11 Method of producing grain oriented silicon steel sheets having magnetic properties

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62112408A JPH0668133B2 (en) 1987-05-11 1987-05-11 Method for producing unidirectional silicon steel sheet with excellent magnetic properties

Publications (2)

Publication Number Publication Date
JPS63277716A JPS63277716A (en) 1988-11-15
JPH0668133B2 true JPH0668133B2 (en) 1994-08-31

Family

ID=14585901

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Link
JP (1) JPH0668133B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220195553A1 (en) * 2019-03-26 2022-06-23 Jfe Steel Corporation Method of producing grain-oriented electrical steel sheet and annealing separator application line

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5353234B2 (en) * 2008-12-26 2013-11-27 Jfeスチール株式会社 Method for producing grain-oriented electrical steel sheet

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220195553A1 (en) * 2019-03-26 2022-06-23 Jfe Steel Corporation Method of producing grain-oriented electrical steel sheet and annealing separator application line
US12467106B2 (en) * 2019-03-26 2025-11-11 Jfe Steel Corporation Method of producing grain-oriented electrical steel sheet and annealing separator application line

Also Published As

Publication number Publication date
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