JPH06336616A - Production of grain-oriented silicon steel sheet - Google Patents
Production of grain-oriented silicon steel sheetInfo
- Publication number
- JPH06336616A JPH06336616A JP5127039A JP12703993A JPH06336616A JP H06336616 A JPH06336616 A JP H06336616A JP 5127039 A JP5127039 A JP 5127039A JP 12703993 A JP12703993 A JP 12703993A JP H06336616 A JPH06336616 A JP H06336616A
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- annealing
- silicon steel
- grain
- steel sheet
- oriented silicon
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- Soft Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、方向性けい素鋼板の
製造方法に関し、特に脱炭焼鈍工程を工夫することによ
って、磁気特性を改善しようとするものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a grain-oriented silicon steel sheet, and particularly to improve the magnetic characteristics by devising a decarburizing annealing step.
【０００２】[0002]
【従来の技術】方向性けい素鋼板は軟磁性材料として、
主に変圧器あるいは回転機等の鉄心材料として使用され
るもので、磁気特性として磁束密度が高く、鉄損および
磁気歪が小さいことが要求される。2. Description of the Related Art Directional silicon steel sheets are used as soft magnetic materials.
It is mainly used as an iron core material for transformers and rotating machines, and is required to have high magnetic flux density as magnetic characteristics and small iron loss and magnetostriction.
【０００３】かかる方向性けい素鋼板は、２次再結晶に
必要なインヒビター、例えばMnS,MnSe,AlN等を含む、方
向性けい素鋼スラブを加熱して熱間圧延を行った後、必
要に応じて焼鈍を行い、１回あるいは中間焼鈍をはさむ
２回以上の冷間圧延によって最終製品板厚とし、次いで
脱炭焼鈍を行った後、鋼板にMgO などの焼鈍分離剤を塗
布し、仕上げ焼鈍を行って製造される。なお、この方向
性けい素鋼板の表面には、特殊な場合を除いて、フォル
ステライト（Mg2SiO4 ) 質絶縁被膜が形成されているの
が普通である。この被膜は表面の電気的絶縁だけでな
く、その低熱膨張性を利用して引張応力を鋼板に付与す
ることにより、鉄損さらには磁気歪をも、効果的に改善
している。Such a grain-oriented silicon steel sheet is obtained by heating a grain-oriented silicon steel slab containing an inhibitor necessary for secondary recrystallization, for example, MnS, MnSe, AlN, etc., and performing hot rolling. Annealing is performed accordingly, and the final product sheet thickness is obtained by cold rolling once or twice or more with intermediate annealing sandwiched, and then decarburization annealing is performed, then an annealing separator such as MgO is applied to the steel sheet, and finish annealing is performed. Is manufactured. The surface of this grain-oriented silicon steel sheet is usually provided with a forsterite (Mg 2 SiO 4 ) insulating coating, except in special cases. This coating not only electrically insulates the surface but also applies tensile stress to the steel sheet by utilizing its low thermal expansion property, thereby effectively improving iron loss and magnetostriction.
【０００４】この被膜は仕上げ焼鈍において形成される
が、その形成挙動は鋼中のMnS,MnSe,AlN等のインヒビタ
ーの挙動に影響するため、優れた磁性を得るための必須
の過程である２次再結晶そのものにも影響を及ぼす。さ
らに形成した被膜は、２次再結晶が完了して不要となっ
たインヒビター成分を被膜中に吸い上げ、鋼を純化する
ことによっても、鋼板の磁気特性の十分な発揮を助けて
いる。従って、この被膜形成過程を制御して被膜を均一
に形成することは、方向性けい素鋼板の製品品質を左右
する重要なポイントのひとつである。This coating is formed during finish annealing, but its formation behavior affects the behavior of inhibitors such as MnS, MnSe, AlN in steel, and is an essential process for obtaining excellent magnetism. It also affects recrystallization itself. Further, the formed coating film absorbs the inhibitor component which has become unnecessary after the secondary recrystallization is absorbed into the coating film to purify the steel, thereby helping the steel sheet to sufficiently exhibit its magnetic properties. Therefore, controlling the film formation process to form a uniform film is one of the important points that affect the product quality of grain-oriented silicon steel sheets.
【０００５】すなわち、形成した被膜は、当然のことな
がら、均一で欠陥がなく、かつ剪断、打抜きおよび曲げ
加工等に耐え得る密着性の優れたものでなければならな
い。また、平滑で鉄心として積層したときに、高い占積
率を示すものでなければならない。That is, the formed coating film must naturally be uniform, have no defects, and have excellent adhesiveness capable of withstanding shearing, punching, bending and the like. Further, it must be smooth and exhibit a high space factor when laminated as an iron core.
【０００６】方向性けい素鋼板にフォルステライト質絶
縁被膜を形成させるには、所望の最終厚みに冷間圧延し
た後、湿水素中で700 〜900 ℃の温度で連続焼鈍を行っ
て、冷間圧延後の組織を、適正な２次再結晶が起こるよ
うに、１次再結晶させると同時に、２次再結晶を完全に
行わせて磁気特性を向上させるため、鋼板に0.01〜0.10
％程度含まれる炭素を、 0.003％程度以下まで脱炭す
る。To form a forsterite insulating coating on a grain-oriented silicon steel sheet, after cold rolling to a desired final thickness, continuous annealing is performed in wet hydrogen at a temperature of 700 to 900 ° C. In order to improve the magnetic properties by performing secondary recrystallization at the same time as performing secondary recrystallization so that proper secondary recrystallization occurs in the structure after rolling, to improve the magnetic properties, the steel sheet is 0.01 to 0.10.
Decarburize the carbon contained in about 0.003% or less.
【０００７】さらに、これと同時に酸化によって、SiO2
を主成分とするサブスケールを鋼板表層に生成させる。
その後、MgO を主成分とする焼鈍分離剤を鋼板上に塗布
し、コイル状に巻取って還元または非酸化性雰囲気中に
て1000℃から1200℃程度の温度で、高温仕上げ焼鈍を施
すことにより、以下の式で示される固相反応によってフ
ォルステライト質絶縁被膜を形成させる。 ２MgO ＋SiO2→MgSiO4 Further, at the same time, by oxidation, SiO 2
A subscale mainly composed of is generated on the surface of the steel sheet.
After that, an annealing separator containing MgO as the main component is applied to the steel sheet, wound into a coil, and subjected to high-temperature finish annealing at a temperature of about 1000 to 1200 ° C in a reducing or non-oxidizing atmosphere. , A forsterite insulating coating is formed by a solid-phase reaction represented by the following formula. 2MgO + SiO 2 → MgSiO 4
【０００８】このフォルステライト質絶縁被膜は１μｍ
前後の微細結晶が緻密に集積したセラミックス被膜であ
り、上述の如く、脱炭焼鈍において、鋼板表層に生成し
た酸化物を一方の原料物質として、その鋼板上に生成す
るものであるから、この酸化物の種類，量，分布等は、
フォルステライトの核生成や粒成長挙動に関与するとと
もに被膜結晶粒の粒界や粒そのものの強度にも影響を及
ぼし、従って仕上げ焼鈍後の被膜品質にも多大な影響を
及ぼす。This forsterite insulating coating has a thickness of 1 μm.
This is a ceramic film in which fine crystals before and after are densely integrated.As described above, during decarburization annealing, the oxide formed on the surface layer of the steel sheet is used as one of the raw materials and is formed on the steel sheet. Type, quantity, distribution, etc.
It is involved in the nucleation and grain growth behavior of forsterite, and also affects the grain boundaries of the coated crystal grains and the strength of the grains themselves, and thus greatly affects the coating quality after finish annealing.
【０００９】また、他方の原料物質であるMgO を主体と
する焼鈍分離剤は、水に懸濁したスラリーとして鋼板に
塗布されるため、乾燥された後も物理的に吸着したH2O
を保有する他、一部が水和してMg(OH)2 に変化している
ため、仕上焼鈍中に 800℃あたりまで、少量ながらH2O
を放出し続ける。このため鋼板表面はこのH2O により、
いわゆる追加酸化を受ける。この酸化もフォルステライ
トの生成挙動に影響を及ぼすとともにインヒビターの酸
化や分解につながることから、これが多いと磁気特性を
劣化する要因となる。この追加酸化の受け易さも、脱炭
焼鈍で生じた鋼板表層の酸化物層の物性に大きく左右さ
れる。Further, since the annealing separating agent mainly composed of MgO, which is the other raw material, is applied to the steel sheet as a slurry suspended in water, H 2 O which is physically adsorbed even after being dried is adsorbed.
In addition to possessing a small amount of H 2 O, it is partially hydrated and converted to Mg (OH) 2
Keep emitting. Therefore steel sheet surface by the H 2 O,
It undergoes so-called additional oxidation. This oxidation also affects the generation behavior of forsterite and leads to the oxidation and decomposition of the inhibitor, so if it is large, it becomes a factor that deteriorates the magnetic properties. The susceptibility to this additional oxidation also largely depends on the physical properties of the oxide layer on the surface of the steel sheet produced by decarburization annealing.
【００１０】さらに、AlN をインヒビターとする方向性
けい素鋼板においては、この酸化物層の物性が、仕上げ
焼鈍中の脱Ｎ挙動あるいは焼鈍雰囲気からのＮの侵入挙
動に影響を及ぼして、磁気特性にも影響を与える。以
上、述べたように、脱炭焼鈍における鋼板表層の状態を
制御することは、方向性けい素鋼板の製造における重要
なポイントのひとつとなる。Further, in the grain-oriented silicon steel sheet using AlN as an inhibitor, the physical properties of the oxide layer affect the denitrification behavior during finish annealing or the penetration behavior of N from the annealing atmosphere, resulting in magnetic properties. Also affects. As described above, controlling the state of the steel sheet surface layer during decarburization annealing is one of the important points in the production of grain-oriented silicon steel sheets.
【００１１】方向性けい素鋼板の脱炭焼鈍に関しては、
例えば、特開昭59−185725号公報に開示されているよう
に、焼鈍雰囲気の露点を50〜75℃に制御する方法、特開
昭54−160514号公報に示されているように、雰囲気の酸
化度を、脱炭の前半では0.15以上とし、後半では0.75以
下でかつ前半より低くする方法などが知られている。Regarding decarburization annealing of grain-oriented silicon steel sheet,
For example, as disclosed in JP-A-59-185725, a method of controlling the dew point of the annealing atmosphere at 50 to 75 ° C., as shown in JP-A-54-160514, It is known that the degree of oxidation is set to 0.15 or more in the first half of decarburization and 0.75 or less in the latter half and lower than that in the first half.
【００１２】[0012]
【発明が解決しようとする課題】しかしながら、上記の
雰囲気制御によっても、必ずしも十分な品質を有するフ
ォルステライト被膜が生成するとは限らず、ストリップ
幅方向、あるいは長手方向で密着不良の部分を生じた
り、外観，被膜厚み，あるいはフォルステライト粒径等
が不均一な被膜となる場合が応々にして生じる。さら
に、局所的に点状−筋状に被膜が剥離したり、ポーラス
な被膜となる場合もあった。However, the above atmosphere control does not always produce a forsterite coating having sufficient quality, and causes a defective adhesion portion in the strip width direction or the longitudinal direction. Occasionally, a film with a non-uniform appearance, film thickness, forsterite particle size, etc., is formed. Furthermore, the coating film may be locally peeled off in a dot-streak shape or a porous coating film may be formed.
【００１３】この発明は、上記の問題点を有利に解決し
ようとするものであり、コイルの全幅および全長にわた
って、欠陥のない均一で密着性の優れた被膜を有する方
向性けい素鋼板を得るための、生産性の高い製造方法に
ついて提案することを目的とする。The present invention is intended to advantageously solve the above-mentioned problems, and to obtain a grain-oriented silicon steel sheet having a uniform coating having no defects and having excellent adhesion over the entire width and entire length of the coil. The purpose of the present invention is to propose a manufacturing method with high productivity.
【００１４】[0014]
【課題を解決するための手段】この発明は、方向性けい
素鋼素材を熱間圧延したのち、１回または中間焼鈍を挟
む２回の冷間圧延を施し、ついで脱炭焼鈍後、焼鈍分離
剤を塗布してから、最終仕上げ焼鈍を施す一連の工程よ
りなる方向性けい素鋼板の製造方法において、脱炭焼鈍
は、その均熱過程における水素分圧に対する水蒸気分圧
の比を 0.7未満に、かつ昇温過程における水素分圧に対
する水蒸気分圧の比を均熱過程よりも低く設定すること
を特徴とする方向性けい素鋼板の製造方法である。According to the present invention, a grain-oriented silicon steel material is hot-rolled and then cold-rolled once or twice with an intermediate annealing, followed by decarburization annealing and annealing separation. In the method for producing grain-oriented silicon steel sheet, which consists of a series of steps in which the agent is applied and then final finishing annealing is performed, decarburization annealing reduces the ratio of water vapor partial pressure to hydrogen partial pressure in the soaking process to less than 0.7. The method for producing a grain-oriented silicon steel sheet is characterized in that the ratio of the partial pressure of water vapor to the partial pressure of hydrogen in the temperature raising process is set lower than that in the soaking process.
【００１５】[0015]
【作用】発明者らは、ストリップにおけるフォルステラ
イト被膜の品質ばらつきの原因を詳細に調査した結果、
脱炭焼鈍において鋼板表層に生成するサブスケールの量
と質のばらつきが大きく影響していることを見出した。
このことは、ストリップの幅方向あるいは長手方向にお
いて、サブスケール形成反応が、必ずしも均一には起こ
っていないことを意味する。さらに、この原因として
は、特に脱炭焼鈍の昇温過程における雰囲気酸化性の変
動が関係していることも新たに判明した。そこで、脱炭
焼鈍における雰囲気酸化性、すなわち水素分圧に対する
水蒸気分圧の比（以下、Ｐ(H2O) ／Ｐ(H2)と示す）が、
フォルステライト被膜に及ぼす影響について調査するた
めの実験を行った。以下に、この実験結果について述べ
る。The inventors of the present invention have investigated in detail the cause of the quality variation of the forsterite coating on the strip,
It was found that variations in the amount and quality of subscales generated on the surface of steel sheets during decarburization annealing have a large effect.
This means that the subscale formation reaction does not necessarily occur uniformly in the width direction or the length direction of the strip. Furthermore, it has been newly found that the cause of this is particularly related to the fluctuation of the oxidizing property in the atmosphere during the temperature rising process of decarburization annealing. Therefore, the atmospheric oxidizability in decarburization annealing, that is, the ratio of the partial pressure of water vapor to the partial pressure of hydrogen (hereinafter referred to as P (H 2 O) / P (H 2 )) is
Experiments were conducted to investigate the effect on forsterite coatings. The results of this experiment will be described below.
【００１６】インヒビターとしてMnSeおよびSbを含む
3.3wt％けい素鋼板（板厚0.23mm）を、 840℃×２分
間、湿水素雰囲気中で脱炭焼鈍した。このとき昇温過程
および均熱過程の雰囲気酸化性を、露点とH2ガス濃度の
調整によって、Ｐ(H2O) ／Ｐ(H2)：0.2 〜0.8 の範囲
に、それぞれ別々に制御した。次いで、鋼板にMgO を主
成分とする焼鈍分離剤を塗布し、 850℃×50時間の２次
再結晶焼鈍と、引続くH2雰囲気中での1200℃×５時間の
鈍化焼鈍を行った。その後、フォルステライト被膜の均
一性を評価した。これらの結果を図１に示す。Includes MnSe and Sb as inhibitors
A 3.3 wt% silicon steel plate (sheet thickness 0.23 mm) was decarburized and annealed in a wet hydrogen atmosphere at 840 ° C for 2 minutes. The atmosphere oxidizing this time temperature rising process and soaking process, by adjusting the dew point and H 2 gas concentration, P (H 2 O) / P (H 2): 0.2 in the range of 0.8 were separately controlled . Then, an annealing separator containing MgO as a main component was applied to the steel sheet, and secondary recrystallization annealing at 850 ° C for 50 hours and subsequent annealing annealing at 1200 ° C for 5 hours in an H 2 atmosphere were performed. Then, the uniformity of the forsterite coating was evaluated. The results are shown in FIG.
【００１７】同図に示すように、均熱過程のＰ(H2O) ／
Ｐ(H2)が 0.7未満でかつ昇温過程のＰ(H2O) ／Ｐ(H2)が
均熱過程のそれよりも低いときに、光沢のある美麗な灰
色の均一な被膜が得られた。一方、均熱過程のＰ(H2O)
／Ｐ(H2)を0.7 以上とすると、昇温過程のＰ(H2O) ／Ｐ
(H2)を均熱過程のそれよりも低くしても、優れた特性の
被膜は得られなかった。As shown in the figure, P (H 2 O) /
When P (H 2 ) is less than 0.7 and P (H 2 O) / P (H 2 ) in the heating process is lower than that in the soaking process, a beautiful glossy gray uniform film is obtained. Was given. On the other hand, P (H 2 O) in the soaking process
If / P (H 2 ) is 0.7 or more, P (H 2 O) / P in the temperature rising process
Even if (H 2 ) was made lower than that in the soaking process, a film having excellent properties was not obtained.
【００１８】ここで、図２に示す、けい素鋼板の表面に
生成する酸化物の平衡状態図によると、Ｐ(H2O) ／Ｐ(H
2)：0.7 は明らかにFeO 生成域であり、このような条件
で形成するサブスケールは、保護性が悪くて仕上げ焼鈍
中の追加酸化が激しくなり、フォルステライト被膜の劣
化が生じるものと考えられる。なお、昇温過程の雰囲気
酸化性を低くすることによってフォルステライト被膜の
膜質が向上する理由は明らかではないが、昇温過程で生
成するサブスケールが均熱過程で生成するサブスケール
の保護性を高めるためと考えられる。Here, according to the equilibrium diagram of oxides formed on the surface of the silicon steel sheet shown in FIG. 2, P (H 2 O) / P (H
2 ): 0.7 is clearly the FeO formation region, and it is considered that the subscale formed under such conditions has poor protection properties and more additional oxidation during finish annealing, resulting in deterioration of the forsterite coating. . The reason why the film quality of the forsterite coating is improved by lowering the atmospheric oxidative property during the temperature rising process is not clear, but the subscale generated during the temperature rising process protects the subscale generated during the soaking process. It is thought to increase.
【００１９】また、昇温過程における雰囲気酸化性の低
下は、脱炭および酸化を促進する効果をも有すること
が、次の実験によって判明した。すなわち、Ｃ：0.045
wt％（以下、単に％と示す）を含む0.23mm厚のけい素鋼
板に、 840℃×２分間、湿水素雰囲気中で脱炭焼鈍を施
すに当たり、その均熱過程の雰囲気のＰ(H2O) ／Ｐ(H2)
を0.2 〜0.7 の範囲に調節し、得られた鋼板のＣ含有量
および表面の酸素目付量を測定した。その結果を表１に
示す。Further, it was found by the following experiment that the decrease in the atmospheric oxidative property during the temperature rising process also has the effect of promoting decarburization and oxidation. That is, C: 0.045
A 0.23 mm thick silicon steel sheet containing wt% (hereinafter simply referred to as%) is subjected to decarburization annealing in a wet hydrogen atmosphere at 840 ° C. for 2 minutes, and the P (H 2 O) / P (H 2 )
Was adjusted to a range of 0.2 to 0.7, and the C content and the oxygen basis weight of the surface of the obtained steel sheet were measured. The results are shown in Table 1.
【００２０】[0020]
【表１】 [Table 1]
【００２１】表１から、昇温過程の雰囲気Ｐ(H2O) ／Ｐ
(H2)を低下することによって、Ｃ含有量がより低くかつ
酸素目付量がより多くなる処理を実現できる。従って、
操業ラインにおける速度を高めることが可能であり、生
産性向上にも寄与するところが大きい。これは、昇温過
程のＰ(H2O) ／Ｐ(H2)を低下することによって、均熱過
程における表面反応が促進されるためと考えられる。From Table 1, the atmosphere P (H 2 O) / P in the temperature rising process
By lowering (H 2 ), it is possible to realize a treatment having a lower C content and a higher oxygen basis weight. Therefore,
It is possible to increase the speed of the operation line, which greatly contributes to productivity improvement. It is considered that this is because the surface reaction in the soaking process is promoted by lowering P (H 2 O) / P (H 2 ) in the temperature rising process.
【００２２】なお、方向性けい素鋼板は、２次再結晶の
ために利用するインヒビターのちがいによって、Mn−Sb
系，AlN −MnS 系，AlN −MnSe系，Mn−Ｓ系等の種類が
あるが、この発明はいずれの鋼種に対しても適用でき
る。The grain-oriented silicon steel sheet has Mn-Sb depending on the difference in the inhibitor used for secondary recrystallization.
The present invention can be applied to any steel type, although there are types such as a system, an AlN-MnS system, an AlN-MnSe system, and a Mn-S system.
【００２３】[0023]
実施例１ Ｃ；0.062 ％，Si；3.31％，Mn；0.078 ％，Se；0.024
％，sol.Al；0.023 ％，Ｎ；0.008 ％，Sb；0.027 ％を
含有する方向性けい素鋼素材を、2.8mm 厚に熱間圧延
後、1100℃で均一化焼鈍を行い、その後、１回の冷間圧
延で0.30mmの板厚とした。次いで 840℃で 130秒間、H2
−N2−H2O 雰囲気中で脱炭焼鈍を行った。このとき、H2
濃度および露点を変更することによって、昇温過程およ
び均熱過程の雰囲気のＰ(H2O) ／Ｐ(H2)を表２に示す値
に調整した。次いで、MgO にTiO2：３％を含む焼鈍分離
剤を塗布し、H2雰囲気中で、1200℃，10時間の２次再結
晶、純化焼鈍に供した。その後、りん酸マグネシウムと
コロイダルシリカを主成分とするコーティングを施し
た。Example 1 C; 0.062%, Si; 3.31%, Mn; 0.078%, Se; 0.024
%, Sol.Al; 0.023%, N; 0.008%, Sb; 0.027%, a grain-oriented silicon steel material is hot-rolled to a thickness of 2.8 mm, homogenized at 1100 ° C, and then 1 It was cold-rolled once to obtain a plate thickness of 0.30 mm. Then at 840 ° C for 130 seconds, H 2
Was decarburization annealed in -N 2 -H 2 O atmosphere. At this time, H 2
By changing the concentration and the dew point, P (H 2 O) / P (H 2 ) in the atmosphere during the temperature raising process and the soaking process was adjusted to the values shown in Table 2. Then, an annealing separator containing TiO 2 : 3% was applied to MgO and subjected to secondary recrystallization and purification annealing at 1200 ° C. for 10 hours in an H 2 atmosphere. Then, a coating containing magnesium phosphate and colloidal silica as main components was applied.
【００２４】かくして得られた製品の1.7 Ｔ, 50Hzにお
ける鉄損Ｗ17/50 値、磁界 800A/mにおける磁束密度Ｂ
8 値、被膜の曲げ密着性および被膜の外観について調査
した。被膜の曲げ密着性は、種々の径（５mm間隔）を有
する丸棒に試験片を巻きつけ、被膜の剥離しない最小径
で示した。また、脱炭焼鈍後の鋼板のＣ含有量および酸
素目付量についても分析を行った。これらの結果を表２
に併記する。The product thus obtained had an iron loss W 17/50 value at 1.7 T, 50 Hz and a magnetic flux density B at a magnetic field of 800 A / m.
Eight values, bending adhesion of the coating and appearance of the coating were investigated. The flexural adhesion of the coating was indicated by the minimum diameter at which the test piece was wound around a round bar having various diameters (interval of 5 mm) and the coating was not peeled off. In addition, the C content and oxygen basis weight of the steel sheet after decarburization annealing were also analyzed. These results are shown in Table 2.
Also described in.
【００２５】[0025]
【表２】 [Table 2]
【００２６】表２から明らかなように、昇温過程のＰ(H
2O) ／Ｐ(H2)が均熱過程のそれよりも高いＮo.８〜10お
よび均熱過程のＰ(H2O) ／Ｐ(H2)が0.70のFeO 生成域で
あったＮo.11は、いずれも被膜均一性、密着性および磁
気特性に劣るものであった。これに対し、この発明に従
って得られたＮo.１〜７は、被膜特性および磁気特性と
もに明らかに向上した。さらに、Ｎo.１〜７は比較例に
比べて、脱炭焼鈍後のＣ量が低くかつ酸素目付量が高い
ことから、脱炭および酸化が促進されたことがわかる。As is clear from Table 2, P (H
2 O) / P (H 2 ) was higher than that in the soaking process, and the No. 8-10 range was FeO, where P (H 2 O) / P (H 2 ) was 0.70. No. 11 was inferior in film uniformity, adhesion and magnetic properties. On the other hand, Nos. 1 to 7 obtained according to the present invention clearly improved both the coating property and the magnetic property. Further, in Nos. 1 to 7, the carbon content after decarburization annealing was low and the oxygen areal weight was high as compared with the comparative example, which indicates that decarburization and oxidation were promoted.
【００２７】実施例２ Ｃ；0.041 ％，Si；3.32％，Mn；0.07％，Se；0.023 ％
およびSb；0.024 ％を含有する方向性けい素鋼素材を、
2.0mm 厚に熱間圧延後、900 ℃で均一化焼鈍を施し、さ
らに 980℃で２分間の中間焼鈍をはさむ２回の冷間圧延
によって、0.23mmの板厚とした。次いで 820℃で 120秒
間、H2−N2−H2O 雰囲気中で脱炭焼鈍を行った。このと
き、H2濃度および露点を変更することによって、昇温過
程および均熱過程の雰囲気のＰ(H2O) ／Ｐ(H2)を表３に
示す値に調整した。次いで、MgOにTiO2：１％およびSrS
O4 ：２％を含む焼鈍分離剤を塗布し、H2雰囲気中で、1
180℃，７時間の２次再結晶，純化焼鈍に供した。その
後、実施例１と同様に処理し、得られた製品について実
施例１と同様の調査を行った。その結果を表３に併記す
る。Example 2 C: 0.041%, Si: 3.32%, Mn: 0.07%, Se: 0.023%
And Sb; grain oriented silicon steel material containing 0.024%,
After hot rolling to a thickness of 2.0 mm, uniform annealing was performed at 900 ° C., and further cold rolling was performed twice at 980 ° C. with intermediate annealing for 2 minutes to obtain a plate thickness of 0.23 mm. Then, decarburization annealing was performed at 820 ° C. for 120 seconds in an H 2 —N 2 —H 2 O atmosphere. At this time, by changing the H 2 concentration and the dew point, P (H 2 O) / P (H 2 ) in the atmosphere during the temperature raising process and the soaking process was adjusted to the values shown in Table 3. Then MgO TiO 2 : 1% and SrS
O 4: the annealing separator coating containing 2%, in H 2 atmosphere, 1
It was subjected to secondary recrystallization and purification annealing at 180 ° C for 7 hours. After that, the same treatment as in Example 1 was performed, and the obtained product was examined in the same manner as in Example 1. The results are also shown in Table 3.
【００２８】[0028]
【表３】 [Table 3]
【００２９】表３から明らかなように、昇温過程のＰ(H
2O) ／Ｐ(H2)を均熱過程のそれよりも低く、かつ均熱過
程のＰ(H2O) ／Ｐ(H2)を0.6 以下としたＮo.１〜６は、
比較例に比べて、いずれも被膜特性および磁気特性に優
れ、さらに脱炭および酸化速度が促進された。As is clear from Table 3, P (H
2 O) / P (H 2 ) is lower than that in the soaking process and P (H 2 O) / P (H 2 ) in the soaking process is 0.6 or less.
Compared to the comparative example, the coating properties and magnetic properties were all excellent, and the decarburization and oxidation rates were promoted.
【００３０】[0030]
【発明の効果】この発明によれば、被膜特性に優れかつ
磁気特性も良好な方向性けい素鋼板の安定生産が可能と
なる。また、脱炭および酸化速度も速くなるため、生産
性の向上に寄与することができる。According to the present invention, it is possible to stably produce a grain-oriented silicon steel sheet having excellent coating properties and magnetic properties. Further, the decarburization and oxidation rates are also increased, which can contribute to the improvement of productivity.
【図１】Ｐ(H2O) ／Ｐ(H2)と仕上げ焼鈍後のフォルステ
ライト被膜の外観との関係を示す図である。FIG. 1 is a diagram showing a relationship between P (H 2 O) / P (H 2 ) and the appearance of a forsterite coating film after finish annealing.
【図２】３％けい素鋼の湿水素中における生成酸化物の
平衡状態図である。FIG. 2 is an equilibrium diagram of oxides produced in wet hydrogen of 3% silicon steel.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 鈴木 隆史 千葉県千葉市中央区川崎町１番地 川崎製 鉄株式会社技術研究本部内 (72)発明者 鈴木 毅浩 岡山県倉敷市水島川崎通１丁目（番地な し） 川崎製鉄株式会社水島製鉄所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Takashi Suzuki 1 Kawasaki-cho, Chuo-ku, Chiba-shi, Chiba Kawasaki Steel Corporation Technical Research Division (72) Inventor Takehiro Suzuki 1-chome, Mizushima Kawasaki-dori, Kurashiki-shi, Okayama (No house number) Kawashima Steel Works Mizushima Works
Claims (1)
１回または中間焼鈍を挟む２回の冷間圧延を施し、つい
で脱炭焼鈍後、焼鈍分離剤を塗布してから、最終仕上げ
焼鈍を施す一連の工程よりなる方向性けい素鋼板の製造
方法において、 脱炭焼鈍は、その均熱過程における水素分圧に対する水
蒸気分圧の比を 0.7未満に、かつ昇温過程における水素
分圧に対する水蒸気分圧の比を均熱過程よりも低く設定
することを特徴とする方向性けい素鋼板の製造方法。1. A hot-rolled grain-oriented silicon steel material,
A method for producing a grain-oriented silicon steel sheet comprising a series of steps in which cold rolling is carried out once or twice with intermediate annealing, followed by decarburization annealing, application of an annealing separating agent, and then final finishing annealing. In decarburization annealing, it is necessary to set the ratio of steam partial pressure to hydrogen partial pressure in the soaking process to less than 0.7 and to set the ratio of steam partial pressure to hydrogen partial pressure in the heating process lower than that in the soaking process. A method for manufacturing a characteristic grain-oriented silicon steel sheet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5127039A JP2786576B2 (en) | 1993-05-28 | 1993-05-28 | Manufacturing method of grain-oriented silicon steel sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5127039A JP2786576B2 (en) | 1993-05-28 | 1993-05-28 | Manufacturing method of grain-oriented silicon steel sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06336616A true JPH06336616A (en) | 1994-12-06 |
| JP2786576B2 JP2786576B2 (en) | 1998-08-13 |
Family
ID=14950125
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5127039A Expired - Lifetime JP2786576B2 (en) | 1993-05-28 | 1993-05-28 | Manufacturing method of grain-oriented silicon steel sheet |
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| Country | Link |
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| JP (1) | JP2786576B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0761827A2 (en) * | 1995-09-07 | 1997-03-12 | Kawasaki Steel Corporation | Process for producing grain oriented silicon steel sheet, and decarburized sheet |
| JPH10212526A (en) * | 1997-01-28 | 1998-08-11 | Nippon Steel Corp | Production of grain oriented silicon steel sheet excellent in glass coating |
| KR100325534B1 (en) * | 1997-12-27 | 2002-07-18 | 이구택 | Method for manufacturing grain oriented silicon steel sheet |
| EP1281778A2 (en) * | 2001-08-02 | 2003-02-05 | Kawasaki Steel Corporation | Method of manufacturing grain-oriented electrical steel sheet |
| JP2018070974A (en) * | 2016-11-01 | 2018-05-10 | Ｊｆｅスチール株式会社 | Production method for grain-oriented electromagnetic steel sheet |
-
1993
- 1993-05-28 JP JP5127039A patent/JP2786576B2/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0761827A2 (en) * | 1995-09-07 | 1997-03-12 | Kawasaki Steel Corporation | Process for producing grain oriented silicon steel sheet, and decarburized sheet |
| EP0761827A3 (en) * | 1995-09-07 | 1998-05-27 | Kawasaki Steel Corporation | Process for producing grain oriented silicon steel sheet, and decarburized sheet |
| JPH10212526A (en) * | 1997-01-28 | 1998-08-11 | Nippon Steel Corp | Production of grain oriented silicon steel sheet excellent in glass coating |
| KR100325534B1 (en) * | 1997-12-27 | 2002-07-18 | 이구택 | Method for manufacturing grain oriented silicon steel sheet |
| EP1281778A2 (en) * | 2001-08-02 | 2003-02-05 | Kawasaki Steel Corporation | Method of manufacturing grain-oriented electrical steel sheet |
| EP1281778A3 (en) * | 2001-08-02 | 2008-09-10 | JFE Steel Corporation | Method of manufacturing grain-oriented electrical steel sheet |
| JP2018070974A (en) * | 2016-11-01 | 2018-05-10 | Ｊｆｅスチール株式会社 | Production method for grain-oriented electromagnetic steel sheet |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2786576B2 (en) | 1998-08-13 |
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