JPH0338323B2 - - Google Patents
Info
- Publication number
- JPH0338323B2 JPH0338323B2 JP17782082A JP17782082A JPH0338323B2 JP H0338323 B2 JPH0338323 B2 JP H0338323B2 JP 17782082 A JP17782082 A JP 17782082A JP 17782082 A JP17782082 A JP 17782082A JP H0338323 B2 JPH0338323 B2 JP H0338323B2
- Authority
- JP
- Japan
- Prior art keywords
- amount
- cold rolling
- annealing
- decarburization
- cooling
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Manufacturing & Machinery (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
Description
この発明は磁気特性の優れた一方向性珪素鋼板
を製造する方法に関するものである。
周知のように一方向性珪素鋼板は主として変圧
器その他の電気機器の鉄芯として使用されるもの
であり、磁気特性として磁化特性および鉄損特性
の優れていることが要求されている。最近では珪
素鋼板の製造技術の進歩により、磁化特性とし
て、B10値(すなわち磁場の強さ1000A/mのと
き発生する圧延方向の磁束密度)で代表される磁
束密度が1.89T(ステラ)を越える優れたものが
得られるようになり、また鉄損特性としては、板
厚0.30mmの一方向性珪素鋼板で、W17/50値(すな
わち磁束密度1.7T、周波数50Hzで磁化した場合
の鉄損)が、1.10w/Kg以下のごとき低鉄損のも
のが得られるようになつている。
上述のように優れた磁気特性を有する珪素鋼板
を得るための基本的要件としては、最終焼鈍過程
において(110)〔001〕方位の2次再結晶粒を充
分に発達させることが必要である。そのために
は、2次再結晶過程で(110)〔001〕方位以外の
好ましくない結晶方位を有する結晶粒の成長を強
く抑制するインヒビターの存在と、先鋭に揃つた
(110)〔001〕方位の2次再結晶粒が充分に発達す
るに好適な1次再結晶集合組織の形成とが必要で
あることが知られている。前記インヒビターとし
ては一般にMnS、MnSe、AlN等の微細析出物が
用いられており、また必要に応じて粒界偏析型元
素であるSb、As、Bi、Pb、Sn等をインヒビター
に併用して、そのインヒビターの効果を強化する
ことも従来から行なわれている。一方、適切な1
次再結晶集合組織の形成に関しては、従来から熱
間圧延および冷間圧延の各工程条件を適切に組合
せる方法が採用されており、このような目的から
中間焼鈍を挟んで2回の冷間圧延を施すが如き複
雑な工程も従来から採用されている。
ところで最近では珪素鋼板製造の素材である珪
素鋼スラブの製造方法が従来の造塊一分塊法から
連続鋳造法に転換される傾向にあるが、このよう
な連続鋳造製スラブを使用した場合には、従来の
造塊一分塊法によるスラブでは生じていなかつた
新たな問題が発生している。すなわち、インヒビ
ターとして有効に作用するMnS、MnSe、AlN等
の微細析出物を得ようとすれば、熱延前にスラブ
を1250℃以上の高温に長時間加熱してインヒビタ
ー元素を充分に解離固溶せしめた後、熱延時の冷
却過程を制御して適切な微細サイズに析出させる
ことを要するが、連鋳製スラブの場合には上記の
如くスラブを高温で加熱している間に結晶粒の異
常な粗大成長を招き易く、この異常粗大粒に起因
して珪素鋼板中に帯状細粒組織と称される2次再
結晶粒不完全発達部分が形成されて、磁気特性の
劣化を招くことがある。
上述の如き帯状細粒組織の発生を防止して磁気
特性を向上させる方法も既にいくつか提案されて
いる。例えば特開昭55−119126号公報によれば、
素材スラブを熱間圧延により所定の板厚に加工す
る際に、再結晶化圧延直前の組織がα相マトリツ
クス中にγ相を3%以上析出させた組織となるよ
うに制御し、これを1230〜960℃の温度範囲で圧
下率が1パス当り30%以上となるように再結晶化
高圧下圧延を施す方法が開示されている。また本
発明者等も既に特願昭56−31510号において、素
材スラブにSi量に応じた必要量のCを含有せし
め、熱延中の特定温度領域で所定量以上のγ相を
生成させることによつて、素材スラブの高温加熱
時に粗大成長した結晶粒を熱延工程で分裂・破壊
させ、成品に発生する帯状細粒組織を効果的に防
止する方法を開示している。
しかしながら所定量以上のγ相を熱延中に生成
せしめる上記各方法によれば、成品の帯状細粒組
織は防止し得るものの、所期の磁気特性は必ずし
も充分でない場合があり、しかも帯状細粒組織の
防止効果自体も甚だ不安定であつて、極端な場合
には成品に全面細粒組織が発生して著しく磁気特
性を劣化させることもあるなど、工業生産上最も
必要とされる安定性に欠ける問題があつた。
一方、近年に至り鋼中に含有される炭素もしく
は炭化物を有効利用して1次再結晶集合組織を改
善する方法が発達してきた。例えば特公昭38−
14009号公報には、第1回冷間圧延前の熱延板を
790℃以上の温度から540℃以下の温度に激しく急
冷した後310〜480℃の温度範囲に保持することに
よつて、結晶粒内に光学顕微鏡で可視サイズ(数
μm)のレンズ状炭化物を析出させる方法が開示
されている。このような方法により生成された比
較的大きなサイズの炭化物は、熱延工程で形成さ
れた粗大な熱延伸長粒を分裂細分化させるに有効
に作用するものであり、2次再結晶粒の発達に有
害な(110)〜(110)〔001〕方位の結晶粒を冷延
工程の初期段階で消滅させる役割を担うものと考
えられている。しかしながらこの方法だけでは未
だ充分に磁気特性を向上させることは困難であつ
た。
さらに最近に至り、冷延工程において結晶粒内
の固溶Cまたは微細炭化物を利用する方法が開発
されている。例えば特公昭54−13846号公報、特
公昭54−29182号公報には、インヒビターとして
AlNを用い、その熱延板を高温焼鈍後急冷して、
最終冷圧延下率が80%以上である1回の強冷延を
施す際に、冷延パス間で少なくとも1回以上の時
効処理を施す方法が開示されている。この場合の
時効処理としては、50〜350℃の温度範囲内で1
分以上の保持または300〜600℃の温度範囲内で1
〜30秒の保持が必要であり、かつ多数回施すこと
が効果的であるとされている。しかしながらこの
方法によれば冷延能率が大幅に低下し、かつ鋼板
の加熱処理費が増すため不経済である。また本願
出願人に係る特公昭56−19377号公報においては、
インヒビターとしてAlNとSbとを複合添加する
場合に、この複合添加の効果を充分に発揮させる
ため、中間焼鈍後の冷却に際して700〜900℃の温
度範囲を200〜2000秒間の範囲で徐冷してから直
ちに200℃以下まで急冷する方法が開示されてい
る。しかしながらこの方法に従つて700〜900℃の
間を200〜2000秒間で徐冷する処理を実現しよう
とすれば、連続焼鈍炉の冷却帯を大幅に改造し
て、鋼板をこの温度域に加熱保持する長尺な除冷
帯を設ける必要があるとともに、著しく低速度で
の連続操業が必要となり、そのため生産能率の著
しい低下と製造コストの上昇を招いて経済的に不
利となる問題がある。さらに、これらの方法とも
にAlNまたはAlN−Sbという特定のインヒビタ
ーを利用し、同時に80%以上の強冷延工程を組合
せて始めてその効果を発起し得るものであり、こ
のような方法で得られた集合組織は{111}<112
>方位が著しく強く集積しており、(110)〔001〕
方位は副方位として弱い集積を示すに過ぎず、
(110)〔001〕方位を強く集積させる方法とは根本
的に異つており、またインヒビターとして従来一
般に用いられているMnS、MnSeを利用して一方
向性珪素鋼板を製造するに際してこれらの方法を
適用することはできなかつた。
一方、SおよびSeをインヒビターとし、この
インヒビターに適した最終冷延圧下率の範囲内に
おいて集合組織の改善を図るために鋼中炭素の有
効活用を図る公知の方法の一つとして、例えば特
公昭56−3892号公報には、中間焼鈍後の冷却に際
して600〜300℃の間を150℃/min以上の冷却速
度で冷却し、最終冷延段階で時効処理を施す方法
が開示されている。この場合の時効処理は、100
〜400℃において5秒〜30分間とし、冷延パス間
で少くとも1回以上その時効処理を施す必要があ
り、したがつてこの場合も冷延能率の低下と加熱
処理費の増大を招き、経済的に不利となるから、
より効率的な方法の開発が強く望まれていた。
この発明は以上の事情に鑑みてなされたもの
で、鋼中Cの有効活用を図る従来方法の諸欠点を
除去、改善して、磁気特性の優れた一方向性珪素
鋼板を能率良くかつ経済的に工業的規模で製造し
得るようにした方法を提供することを目的とする
ものである。
すなわち本発明者等は上述の目的を達成するべ
く鋭意実験・検討を重ねた結果、第1には、熱延
中に生成するγ相の生成量を適正範囲内に制御す
るべく、C量をSi量に応じて調整すること、第2
には熱延工程終了後から最終冷延工程前の中間焼
鈍後に至るまでの間に所定量のCを脱炭させるこ
と、第3には最終冷延前の中間焼鈍後に鋼板の結
晶粒内炭化物を極微小の特定範囲内に制御しかつ
充分に分散させる処理を施すこと、以上3要件を
組合せることによつて優れた磁気特性を有する一
方向性珪素鋼板を能率的かつ経済的に製造し得る
ことを見出し、この発明をなすに至つたのであ
る。
具体的には、この発明の一方向性珪素鋼板の製
造方法は、
C0.015〜0.10%、Si2.8〜4.0%、Mn0.02〜0.15
%を含みかつS、Seのいずれか1種または2種
とSbとを合計量で0.008〜0.080%含有し、残部が
実質的にFeよりなる珪素鋼素材を熱間圧延し、
得られた熱延鋼板に対し中間焼鈍を挟む2回以上
の冷間圧延を最終冷延圧下率40〜80%の範囲内で
施して所定の最終板厚に仕上げ、さらにその冷延
鋼板に脱炭焼鈍および最終焼鈍を施す一連の一方
向性珪素鋼板の製造方法において、
前記珪素鋼素材のC量をSi量に応じて下記式で
表わされる範囲に調整し、かつ前記熱間圧延終了
後最終冷延終了前までの間においてCを0.006〜
0.020%脱炭させ、かつまた最終冷延前における
中間焼鈍後の冷却過程において770〜100℃の温度
範囲を30秒以内で急冷し、直ちに150〜250℃の温
度において2〜60秒間の時効処理を施すか、ある
いは同じく前記中間焼鈍後の冷却過程において
770〜300℃の温度範囲を20秒以内で急冷し、続い
て300〜150℃の間の冷却所要時間を8〜30秒の範
囲内に制御することによつて、鋼板の結晶粒内炭
化物を100〜500Åの大きさの微小かつ充分に分散
した析出状態に制御した後、最終冷延を施すこと
を特徴とするものである。
記
0.37[Si%]+0.27≦log([C%]×103)
≦0.37[Si%]+0.57
但し〔Si%〕、〔C%〕はそれぞれ鋼中に含まれ
るSi、Cの重量%を表わす。
以下この発明の製造方法をさらに詳細に説明す
る。
先ずこの発明をなすに至つた過程での知見を説
明すると、本発明者等は熱延中に生成されるγ相
の作用について検討を加えたところ、次のような
事実が確認された。すなわち、素材スラブの熱延
中に生成されるγ相は前述のように素材スラブの
高温加熱時に粗大成長した結晶粒を分裂・破壊さ
せるに有効である半面、インヒビターとして作用
するMnS、MnSe等の微細析出物に有害に作用
し、時に過剰なγ相生成はインヒビターの効果を
大幅に減退させて2次再結晶粒の充分な発達を阻
害するおそれがあり、したがつてγ相生成量は適
切な範囲とする必要があること、またγ相は、そ
の生成量が適切な範囲内にある場合でも、熱延中
に粗大成長粒を細分化する役割を果たした後に
は、冷延工程での適切な結晶組織、集合組織の形
成に対して有害となる等の事実を新規に見出し
た。そこで本発明者等はγ相の有益な作用は生か
しつつ、しかもその有害な作用を解消する方策を
種々研究した結果、熱延中のγ相の生成量を適正
な範囲とするべく素材中のC量をSi量に応じて調
整し、しかも熱延終了後最終冷延工程終了前まで
の間において適量の脱炭を行つて過剰なγ相生成
量を減少せしめ、さらには中間焼鈍後、最終冷延
前の鋼板の結晶粒内炭化物を、光学的顕微鏡によ
つては視ることのできない程度の従来留意された
ことのないような極微小の特定範囲内に制御しか
つ充分に析出分散させることによつて、最終冷延
および脱炭焼鈍を経た最終焼鈍前の鋼板の集合組
織を(110)〔001〕方位の集積度が強い状態に改
善することができ、その結果最終焼鈍における2
次再結晶過程において高度に揃つた(110)〔001〕
方位の2次再結晶粒を充分に成長させて、優れた
磁気特性を有する一方向性珪素鋼板が得られるこ
とを新規に知見し、この発明の完成に至つたので
ある。
上述のようにこの発明を完成するに至つた本発
明者等の実験結果に基いて、この発明の各要件を
さらに詳細に説明する。
第1図は、インヒビターとしてSeおよびSbを
合計量で0.020〜0.045%、Mn0.03〜0.09%を含
み、Si含有量を2.8〜3.1%、3.3〜3.5%、3.6〜3.8
%の3群とし、かつC含有量をいずれも0.01〜
0.10%の範囲で変化させた多数の珪素鋼連鋳スラ
ブ供試材を、1400℃で1時間加熱処理後に熱間圧
延して厚さ2.5mmの熱延板となし、次いで公知の
方法による中間焼鈍を挾む2回の冷延工程により
最終板厚0.30mmに仕上げ、さらに脱炭焼鈍および
最終焼鈍を施して得た一方向性珪素鋼板の各製品
について、鉄損W17/50を調べ、その鉄損値と各連
鋳スラブ供試材のSi量およびC量との関係を示し
たものである。なおこの試験における中間焼鈍の
雰囲気は脱炭性から非脱炭性のものに各種変更さ
せ、また最終冷延圧下率は50〜70%の範囲に設定
した。
第1図における記号◎、○、●、×は、製品の
鉄損W17/50の大小を、それぞれの供試材段階のSi
含有量に応じて次の第1表に示すように判定した
ものである。
The present invention relates to a method for manufacturing a unidirectional silicon steel sheet with excellent magnetic properties. As is well known, unidirectional silicon steel sheets are mainly used as iron cores for transformers and other electrical equipment, and are required to have excellent magnetic properties such as magnetization properties and iron loss properties. Recently, due to advances in manufacturing technology for silicon steel sheets, the magnetic flux density represented by the B10 value (i.e., the magnetic flux density in the rolling direction that occurs when the magnetic field strength is 1000 A/m) has increased to 1.89T (Stella). In addition, as for iron loss characteristics, the W 17/50 value (i.e., the iron loss property when magnetized at a magnetic flux density of 1.7 T and a frequency of 50 Hz with a unidirectional silicon steel sheet of 0.30 mm thickness) It is now possible to obtain products with low iron loss (loss) of 1.10w/Kg or less. As mentioned above, a basic requirement for obtaining a silicon steel sheet having excellent magnetic properties is to sufficiently develop secondary recrystallized grains with (110) [001] orientation in the final annealing process. To achieve this, the existence of an inhibitor that strongly suppresses the growth of crystal grains with unfavorable crystal orientations other than the (110) [001] orientation during the secondary recrystallization process, and the presence of an inhibitor that strongly suppresses the growth of crystal grains with unfavorable crystal orientations other than the (110) [001] It is known that formation of a suitable primary recrystallized texture is necessary for sufficient development of secondary recrystallized grains. As the inhibitor, fine precipitates such as MnS, MnSe, AlN, etc. are generally used, and if necessary, grain boundary segregation type elements such as Sb, As, Bi, Pb, Sn, etc. are used in combination with the inhibitor. It has also been conventionally attempted to enhance the effect of the inhibitor. On the other hand, a suitable one
Regarding the formation of the next recrystallization texture, a method has traditionally been adopted that appropriately combines each process condition of hot rolling and cold rolling. Complicated processes such as rolling have also been employed in the past. By the way, recently there has been a trend in the manufacturing method of silicon steel slabs, which are the raw material for manufacturing silicon steel sheets, to change from the conventional one-block ingot method to the continuous casting method. A new problem has arisen that did not occur with slabs produced by the conventional ingot-forming method. In other words, in order to obtain fine precipitates such as MnS, MnSe, and AlN that act effectively as inhibitors, the slab must be heated to a high temperature of 1250°C or higher for a long time before hot rolling to sufficiently dissociate the inhibitor elements into solid solution. After this, it is necessary to control the cooling process during hot rolling so that the crystal grains are precipitated to an appropriate fine size. Due to these abnormally coarse grains, incompletely developed secondary recrystallized grains called band-like fine grain structures are formed in the silicon steel sheet, which can lead to deterioration of magnetic properties. . Several methods have already been proposed for improving magnetic properties by preventing the generation of the band-like fine grain structure as described above. For example, according to Japanese Patent Application Laid-open No. 55-119126,
When processing a material slab to a predetermined thickness by hot rolling, the structure immediately before recrystallization rolling is controlled so that it becomes a structure in which 3% or more of the γ phase is precipitated in the α phase matrix, and this is A method is disclosed in which recrystallization high pressure rolling is performed in a temperature range of ~960° C. so that the rolling reduction is 30% or more per pass. In addition, the present inventors have already proposed in Japanese Patent Application No. 56-31510 that a material slab contains a necessary amount of C according to the amount of Si, and a predetermined amount or more of γ phase is generated in a specific temperature range during hot rolling. discloses a method of splitting and destroying crystal grains that have grown coarsely during high-temperature heating of a material slab during the hot rolling process, thereby effectively preventing the formation of band-like fine grain structures in finished products. However, according to each of the above methods in which a predetermined amount or more of γ phase is generated during hot rolling, although the band-like fine grain structure of the product can be prevented, the desired magnetic properties may not always be sufficient. The prevention effect of the microstructure itself is extremely unstable, and in extreme cases, a fine grain structure may occur over the entire surface of the product, significantly degrading the magnetic properties. There was a problem that was missing. On the other hand, in recent years, methods have been developed for improving the primary recrystallization texture by effectively utilizing carbon or carbides contained in steel. For example, special public relations
Publication No. 14009 describes a hot rolled sheet before the first cold rolling.
Lenticular carbides with a size visible under an optical microscope (several μm) are precipitated within the crystal grains by rapidly cooling rapidly from a temperature of 790°C or higher to a temperature of 540°C or lower and then maintaining the temperature in a temperature range of 310 to 480°C. A method is disclosed. The relatively large-sized carbides produced by this method effectively act to split and refine the coarse hot-drawn elongated grains formed in the hot-rolling process, and prevent the development of secondary recrystallized grains. It is thought that this plays a role in eliminating crystal grains with the (110) to (110) [001] orientation, which are harmful to the cold rolling process, at the early stage of the cold rolling process. However, it has still been difficult to sufficiently improve magnetic properties using this method alone. More recently, methods have been developed that utilize solid solution C or fine carbides within crystal grains in the cold rolling process. For example, in Japanese Patent Publication No. 54-13846 and Japanese Patent Publication No. 54-29182, there are
Using AlN, the hot-rolled sheet is annealed at high temperature and then rapidly cooled.
A method is disclosed in which, when performing one hard cold rolling with a final cold rolling reduction of 80% or more, aging treatment is performed at least once between cold rolling passes. In this case, the aging treatment is carried out at a temperature of 50 to 350℃.
Hold for more than 1 minute or within the temperature range of 300-600℃
It is said that it is necessary to hold for ~30 seconds and that it is effective to apply it multiple times. However, this method is uneconomical because the cold rolling efficiency is significantly reduced and the cost for heat treatment of the steel sheet is increased. Furthermore, in Japanese Patent Publication No. 19377, filed by the applicant,
When adding a combination of AlN and Sb as an inhibitor, in order to fully demonstrate the effect of this combination addition, slow cooling is performed at a temperature range of 700 to 900°C for 200 to 2000 seconds during cooling after intermediate annealing. A method is disclosed in which the temperature is immediately quenched to below 200°C. However, in order to achieve gradual cooling between 700 and 900 degrees Celsius for 200 to 2000 seconds using this method, the cooling zone of the continuous annealing furnace must be significantly modified to keep the steel plate heated to this temperature range. It is necessary to provide a long cooling zone for cooling, and continuous operation at extremely low speeds is required, resulting in a significant decrease in production efficiency and an increase in manufacturing costs, which is economically disadvantageous. Furthermore, both of these methods utilize a specific inhibitor, AlN or AlN-Sb, and can only be effective when combined with a strong cold rolling process of 80% or more. The texture is {111}<112
>Directions are extremely concentrated, (110) [001]
The direction only shows weak accumulation as a subdirection;
This method is fundamentally different from the method of strongly accumulating the (110) [001] orientation, and these methods are used when manufacturing unidirectional silicon steel sheets using MnS and MnSe, which have been commonly used as inhibitors. It could not be applied. On the other hand, as one of the known methods for effectively utilizing carbon in steel to improve the texture within the range of the final cold rolling reduction suitable for this inhibitor, for example, Publication No. 56-3892 discloses a method in which cooling after intermediate annealing is performed between 600 and 300°C at a cooling rate of 150°C/min or more, and aging treatment is performed in the final cold rolling stage. In this case, the statute of limitations is 100
It is necessary to perform the aging treatment at ~400℃ for 5 seconds to 30 minutes at least once between cold rolling passes. Therefore, this also results in a decrease in cold rolling efficiency and an increase in heat treatment costs. Because it is economically disadvantageous,
There was a strong desire to develop a more efficient method. This invention was made in view of the above circumstances, and it eliminates and improves the various drawbacks of the conventional method for effectively utilizing C in steel, and makes it possible to efficiently and economically produce unidirectional silicon steel sheets with excellent magnetic properties. The purpose of this invention is to provide a method that enables production on an industrial scale. In other words, as a result of extensive experiments and studies in order to achieve the above-mentioned objectives, the present inventors found that, firstly, in order to control the amount of γ phase generated during hot rolling within an appropriate range, the amount of C was Adjust according to the amount of Si, the second
The third step is to decarburize a predetermined amount of C between the end of the hot rolling process and the intermediate annealing before the final cold rolling process, and the third step is to remove carbides in the grains of the steel sheet after the intermediate annealing before the final cold rolling process. By combining the above three requirements, we can efficiently and economically produce grain-oriented silicon steel sheets with excellent magnetic properties. They found that it could be obtained and came up with this invention. Specifically, the method for producing a unidirectional silicon steel sheet of the present invention includes C0.015~0.10%, Si2.8~4.0%, Mn0.02~0.15
% and contains one or two of S, Se, and Sb in a total amount of 0.008 to 0.080%, with the balance substantially consisting of Fe, hot-rolled;
The obtained hot-rolled steel sheet is cold-rolled two or more times with intermediate annealing at a final cold-rolling reduction of 40 to 80% to achieve a predetermined final thickness. In a method for manufacturing a series of unidirectional silicon steel sheets that undergoes charcoal annealing and final annealing, the amount of C in the silicon steel material is adjusted to the range expressed by the following formula according to the amount of Si, and the final annealing is performed after the hot rolling is completed. C from 0.006 to before the end of cold rolling
Decarburize by 0.020%, and in the cooling process after intermediate annealing before final cold rolling, rapidly cool within 30 seconds at a temperature range of 770 to 100℃, and immediately undergo aging treatment at a temperature of 150 to 250℃ for 2 to 60 seconds. or in the cooling process after the intermediate annealing.
By rapidly cooling the temperature range from 770 to 300℃ within 20 seconds, and then controlling the cooling time between 300 and 150℃ within the range of 8 to 30 seconds, carbides in the grains of the steel sheet can be removed. It is characterized in that the final cold rolling is carried out after controlling the precipitation state to be fine and sufficiently dispersed with a size of 100 to 500 Å. Note: 0.37 [Si%] + 0.27≦log ([C%] × 10 3 ) ≦0.37 [Si%] + 0.57 However, [Si%] and [C%] represent the amount of Si and C contained in the steel, respectively. Represents weight %. The manufacturing method of the present invention will be explained in more detail below. First, to explain the findings in the process that led to this invention, the present inventors investigated the effect of the γ phase generated during hot rolling, and the following facts were confirmed. In other words, as mentioned above, the γ phase generated during hot rolling of the material slab is effective in splitting and destroying the crystal grains that have grown coarsely when the material slab is heated to high temperatures. It has a detrimental effect on fine precipitates, and sometimes excessive γ phase formation can significantly reduce the inhibitor's effectiveness and inhibit the sufficient development of secondary recrystallized grains. Therefore, the amount of γ phase formed must be appropriate. In addition, even if the amount of γ phase produced is within an appropriate range, after it plays the role of finely growing coarse grains during hot rolling, it will not be produced in the cold rolling process. We have newly discovered the fact that it is harmful to the formation of an appropriate crystal structure and texture. Therefore, the present inventors have conducted various research into ways to take advantage of the beneficial effects of the γ phase while also eliminating its harmful effects.As a result, the inventors have found that the amount of γ phase produced in the material during hot rolling should be within an appropriate range. The amount of C is adjusted according to the amount of Si, and an appropriate amount of decarburization is performed between the end of hot rolling and before the end of the final cold rolling process to reduce the amount of excessive γ phase formed. Control the intragrain carbides of a steel sheet before cold rolling to within a specific extremely small range that cannot be seen with an optical microscope, which has never been considered before, and sufficiently precipitate and disperse them. By this, the texture of the steel sheet after final cold rolling and decarburization annealing before final annealing can be improved to a state where the degree of accumulation of (110) [001] orientation is strong, and as a result, the
Highly aligned in the next recrystallization process (110) [001]
It was newly discovered that a unidirectional silicon steel sheet having excellent magnetic properties can be obtained by sufficiently growing oriented secondary recrystallized grains, leading to the completion of this invention. Each requirement of the present invention will be explained in more detail based on the experimental results of the present inventors that led to the completion of the present invention as described above. Figure 1 shows a total of 0.020 to 0.045% of Se and Sb and 0.03 to 0.09% of Mn as inhibitors, and Si contents of 2.8 to 3.1%, 3.3 to 3.5%, and 3.6 to 3.8%.
%, and the C content is 0.01~
A large number of continuously cast silicon steel slab specimens with changes in the range of 0.10% were heat-treated at 1400°C for 1 hour, then hot-rolled into hot-rolled sheets with a thickness of 2.5 mm, and then intermediately rolled by a known method. The iron loss W 17/50 was investigated for each product of unidirectional silicon steel plate obtained by finishing the final plate thickness to 0.30 mm through two cold rolling processes with annealing, and then performing decarburization annealing and final annealing. The relationship between the iron loss value and the Si content and C content of each continuously cast slab specimen is shown. In this test, the intermediate annealing atmosphere was varied from decarburizing to non-decarburizing, and the final cold rolling reduction was set in the range of 50 to 70%. The symbols ◎, ○, ●, and × in Fig. 1 indicate the size of the iron loss W 17/50 of the product, and the Si of each sample material stage.
Judgments were made according to the content as shown in Table 1 below.
【表】
また第1図中に併記した破線A,B,C,D,
Eは、熱延中の1150℃におけるγ相生成量の推定
値であり、それぞれγ相生成量40%、30%、20
%、10%および0%の場合を示す。ここでγ相生
成量は実質的にはSi量およびC量と温度に応じて
変化するものであり、前記各破線A,B,C,
D,Eは、各種のSi量、C量の珪素鋼供試材につ
いて実験により求めた1150℃の平衡状態で生成す
るγ相量実測値と、鋼中のSi量、C量との相関関
係から導き出された下記(1)式より求めたものであ
る。
γ%=67log(〔C%〕×103)−25〔Si%〕−8……(1
)
第1図および第1表から明らかな如く、Si含有
量によつて良好と判定される絶対的な鉄損水準は
異なるが、各Si量に応じて鉄損W17/50の優れるC
量の適正範囲は、いずれも破線DとBの間、すな
わちγ相生成量が10〜30%の範囲内にあるときに
限られることを見出した。但し熱延工程中に生成
されるγ相は平衡状態とは異なり準安定的であつ
て、実際の1150℃の熱延中に生成するγ相量を正
確に把握することは困難である。したがつてγ相
生成量によつて限定することは実際的ではないか
ら、前記(1)式で与えられる推定γ相生成量が10〜
30%の範囲内となるような素材中のSi量に応じた
C量の範囲を以つて限定することが妥当と考えら
れる。この考え方に基づき、この発明においては
γ%が10〜30%となるような素材Si量に応じたC
量の範囲を前記(1)式から導き出し、これを優れた
鉄損水準を得るためのC量の適正範囲とした。す
なわちこのC量の適正範囲は次の(2)式で表わされ
る。
0.37〔Si%〕+0.27≦log(〔C%〕×103)
≦0.37〔Si%〕+0.57 ……(2)
これがこの発明の第1の特徴的な要件である。
上記(2)式で示されるSi量に応じた適正C量範囲
の下限よりもC量が不足する場合、従つて熱延中
のγ相生成量が10%未満に対応する組成の場合に
は、製品の結晶組織が明瞭な帯状細粒組織を示
し、磁気特性の劣化が認められた。また熱延中の
γ相生成量が第1図においてD線で示す10%以上
となる組成の製品は、帯状細粒の発生が殆どな
く、大半が正常に発達した2次再結晶粒で構成さ
れていることが判明した。したがつてスラブ高温
加熱の際に異常成長した粗大結晶粒を熱延工程中
に分裂、破壊し、製品の帯状細粒発生を防止する
ためには、所定量以上のγ相生成が必要であり、
このγ相の必要所定量は、含有Si量に応じて熱延
中に平衡状態であれば10%以上のγ相を生成させ
るようC量を含ませることによつて実現できるこ
とが判明した。一方、C量が著しく過剰の場合、
すなわち熱延中のγ相生成量が30%を越える組成
に対応する場合は、製品の結晶組織は2次再結晶
の発達が不完全な全面細粒組織となり、極端に劣
悪な磁気特性を示した。
上述のように、Si量に応じて、熱延中に平衡状
態であれば10〜30%の範囲内のγ相を生成するよ
うなC量を含有する場合にのみ、製品における帯
状粒組織の発生もしくは2次再結晶粒の発達が不
完全な全面細粒組織の生成を防止でき、したがつ
て前記(2)式によりSi量に応じたC量を限定するこ
とが磁気特性の向上に極めて有効であることが判
明した。
しかしながら、第1図のγ相生成量10〜30%の
範囲内においてもなお一部には鉄損特性の不充分
なものが含まれており、磁気特性の安定性を期す
べき工業生産の観点からは、前記(2)式によるC、
Si量の規制だけでは未だ満足すべきものとは言え
ない。そこで本発明者等はさらにこれを改良すべ
く研究を重ねた結果、素材スラブの熱延工程終了
後から最終冷延工程前の中間焼鈍後に至るまでの
工程途中でCを0.006〜0.020%脱炭させることが
優れた磁気特性を安定して得るために有効である
ことを見出し、これをこの発明の第2の特徴的要
件としたのである。
この要件は本発明者等の次のような実験結果か
ら明らかにされたものである。すなわち、第1図
の実験で用いた供試材のうち、Si2.8〜3.1%およ
びSi3.3〜3.5%の2群のSi含有量であり、かつこ
れらSi量に対応するC量が、熱延中1150℃におけ
るγ相生成量が10〜30%に相当する範囲内にある
組成の供試材について、製品の磁気特性と、熱延
工程終了直後および最終冷延前中間焼鈍後のC含
有量の差すなわちその間の脱炭量ΔCとの関係を
詳細に調査した結果、第2図A,Bに示す結果が
得られた。なお、第2図において白丸はSi含有量
が2.8〜3.1%の群を、黒丸はSi含有量が3.3〜3.5%
の群をそれぞれ示す。第2図A,Bから明らかな
ように、脱炭量ΔCが0.006%以上、0.020%以下で
あるときに優れた磁気特性が安定して得られ、C
が0.006%未満もしくは0.020%を越える場合には
磁束密度が不足するとともに鉄損も大きい値を示
し、充分な磁気特性が得られないことが判明し
た。
なお通常の珪素鋼板の製造における熱延後から
最終冷延前までの間の脱炭量は0.005%程度以下
であり、したがつてこの発明の方法における脱炭
量0.006〜0.020%は常法における通常の脱炭量よ
りも大きいから、この発明の方法を実施するにあ
たつては通常は中間焼鈍の雰囲気を脱炭性のもの
とするごとく、積極的な脱炭処理を行うことを要
する。このように熱間圧延終了後から最終冷延前
までの間において適量の強脱炭を行うことによつ
て、先に説明した第1要件の不満足点を補い、優
れた磁気特性を安定して得ることが可能となつた
のである。
上述のように適量の脱炭が磁気特性の改善およ
び安定化に有効なことは、次のような結晶組織、
集合組織観察結果からも明らかである。すなわ
ち、脱炭量が適切な場合、最終冷延前の結晶粒度
が均一かつ適正であり、また1次再結晶集合組織
は(110)〔001〕方位の強い集積を示す好適な状
態に改善されており、その結果製品の結晶組織は
正常な2次再結晶粒が充分に発達したものとなつ
ている。一方、脱炭量が不足する場合、1次再結
晶組織は粒が不揃いで塊状の炭化物が残留してお
り、1次再結晶集合組織は(110)〔001〕方位の
集積が弱く(111)<112>方位が分散する不適切
な組織となつており、その結果細粒が混在する2
次再結晶発達不良の状態となつている。また脱炭
過多の場合には最終冷延前の結晶粒度が不均一で
粗大粒が分散する不適切なものとなつており、そ
の1次再結晶集合組織も(110)〔001〕方位が減
少するため、2次再結晶後には著しく粗大な結晶
粒で占められ、これ等の結晶方位は(110)〔001〕
方位からやや偏倚した方位が多く、したがつて磁
気特性も不充分となつた。
上述のように本発明者等は適量の脱炭が磁気特
性の向上と安定化に有効であることを見出した
が、さらに本発明者等はより高い磁束密度と鉄損
がW17/50値で1.00W/Kg以下という著しく優れた
特性を有する一方向性珪素鋼板の開発に取組んだ
結果、最終冷延前の中間焼鈍後に鋼板の結晶粒内
炭化物を光学顕微鏡によつては視ることのできな
い極微小の特定範囲内に制御しかつ充分多量に析
出させる処理を前記2要件に組合せることによつ
て、最終焼鈍前の集合組織を(110)〔001〕方位
の集積が一段と強い状態に改善することができ、
その結果として最終焼鈍での2次再結晶過程にお
いて高度に揃つた(110)〔001〕方位の2次再結
晶粒の形成がなされ、優れた磁気特性が得られる
ことを新規に知見し、このような結晶粒内炭化物
制御のための処理をこの発明の第3の特徴的要件
としたのである。
以下本発明者等の実験結果に基づいて第3の要
件の効果を説明する。実験に用いた素材はC0.045
%、Si3.20%、Mn0.06%、Se0.025%、および
Sb0.020%の組成を有し、通常の製鋼、連鋳およ
び熱間圧延を経て仕上げられた板厚3.0mmの熱延
板である。このような熱延板を950℃×2分間の
焼鈍後、酸洗して第1回冷間圧延を施し、中間板
厚0.75mmとなした後900℃×3分間の中間焼鈍後、
圧下率60%の最終冷延を施し、最終板厚0.30mmに
仕上げた。次いで800℃の湿水素雰囲気中で脱炭
焼鈍し、MgO塗布後最終焼鈍として1200℃×10
時間保持焼鈍を行ない、一方向性珪素鋼板の製品
を得た。
上記実験において冷延工程間の中間焼鈍での脱
炭量ΔCを、従来の通常の水準である0.002%、こ
の発明の限定範囲内である0.012%、および過脱
炭の0.025%の3水準に変化させ、かつ中間焼鈍
後の冷却過程における770℃以下の冷却を油焼入
れ(770〜100℃における冷却時間約10秒に相当す
る急冷)とし、直ちに200℃での時効処理を、2
〜200秒の間で変化させて実施した。この時効処
理後の鋼板、すなわち中間焼鈍後最終冷延前の鋼
板における結晶粒内炭化物析出サイズと磁気特性
との関係、および同じく炭化物析出サイズと200
℃での時効処理時間との関係を第3図に示す。な
お第3図の磁気特性プロツトは、脱炭量ΔCが
0.002%の場合を○印、ΔC0.012%の場合を●印、
ΔC0.025%の場合を◎印でそれぞれ示した。また
第3図における比較材としては、工業的な連続焼
鈍で一般に実用されている770〜100℃間の冷却時
間98秒に相当する冷却速度で強制空冷した試料に
ついて示した。
第3図から明らかなように、脱炭量が前記第2
の要件の範囲内の適切な量(●印)でしかも200
℃における時効処理時間が10〜20秒間程度の場合
に、磁束密度B10値が1.94T以上、鉄損W17/50が
1.00W/Kg以下と極めて優れた磁気特性を示し、
またこの場合の炭化物の析出サイズは、100〜500
Åの範囲にあることが明らかである。またこの場
合の炭化物析出状態の電子顕微鏡写真(1万倍)
を第4図Aに示す。但しこの電子顕微鏡写真は、
最終冷延前の中間焼鈍後、770〜100℃間を22秒で
急冷後、直ちに200℃×10秒間の時効処理を施し
た試料についてのものであり、その炭化物平均粒
径は200Åで、炭化物が均一かつ多量に分散して
いることが明らかである。
一方、中間焼鈍後油焼入れのまま(時効処理な
し)および200℃時効処理2秒間の場合には、い
ずれの脱炭量の場合も磁気特性が不充分であるこ
とが明らかであり、この場合結晶粒内炭化物は観
察されないかまたは局部的に僅少量のみ析出して
いる状態であつた。また200℃時効処理が30秒間
以上の場合も、いずれの脱炭量でも磁気特性が不
充分であることが明らかであり、この場合結晶粒
内炭化物の析出サイズは500Åを越えていた。ま
た参考のため、中間焼鈍後工業的な標準冷却
(770〜100℃間の冷却時間約98秒)を施した比較
材についての最終冷延前の炭化物析出状態の電子
顕微鏡写真(1万倍)を第4図Bに示す。この場
合結晶粒内炭化物析出平均粒径は約700Åであり、
また磁気特性は中間焼鈍後急冷して200℃時効処
理を30秒間以上施した場合と同程度に劣るもので
あつた。
さらに第3図から、脱炭量ΔCが従来の通常の
水準の場合(○印)および脱炭過多の場合(◎
印)には、中間焼鈍後急冷して直ちに10〜20秒程
度の200℃時効処理を施した場合でも磁気特性は
若干の改善効果は認められるものの顕著ではない
ことが明らかである。
以上の実験結果から、中間焼鈍後最終冷延前の
結晶粒内炭化物サイズが100〜500Åの範囲内とな
るような処理を、時に脱炭量が適切な材料につい
て施すことによつて磁気特性を顕着に改善できる
ことが判明したのである。
さらに本発明者等は(A)中間焼鈍工程で積極的に
脱炭を行なわず、かつ最終冷延前の中間焼鈍後冷
却過程で急冷せずに標準冷却(770〜100℃間の冷
却所要時間約90秒)した場合、(B)中間焼鈍工程で
0.006〜0.020%の脱炭を行ない、最終冷延前の中
間焼鈍後冷却過程で急冷せずに標準冷却した場
合、(C)中間焼鈍工程で積極的に脱炭せず、最終冷
延前の中間焼鈍後冷却過程で770〜100℃の温度範
囲を30秒以内で急冷し、直ちに200℃で10〜20秒
程度の時効処理を行つた場合、(D)中間焼鈍工程で
0.006〜0.020%の脱炭を行ない、かつ最終冷延前
の中間焼鈍後冷却過程で前記(C)と同様な急冷およ
び時効処理を行つた場合、以上(A)〜(D)の4種類の
処理により得られた冷延板につき、最終焼鈍前の
脱炭焼鈍板表層のゴス方位強度を調べたところ、
第5図に示す結果が得られた。第5図から、脱炭
および急冷−時効処理のいずれも行なわない場合
(A)と比較して、脱炭のみの場合(B)および急冷−時
効処理のみの場合(C)には約1.5倍のゴス方位強度
を示し、さらにこの発明の方法にしたがつて脱炭
および急冷−時効処理の両者を施した場合(D)に
は、(A)と比較して約1.7倍のゴス方位強度を示す
ことが確認された。このようにこの発明の方法に
よりゴス方位強度が増す理由は次のように考えら
れる。すなわち、適切な量の脱炭によつて最終冷
延前の中間焼鈍において再結晶開始温度がより低
温となり、そのため、より定温で再結晶すると言
われているゴス粒の成長に有利となり、さらに再
結晶後の均熱時のα−γ変態量の減少によつて集
合組織のランダム化が阻止されて、ゴス方位に強
い集積をもつ集合組織に改善される。また、最終
冷延前に超微小炭化物が均一に析出分散すること
によつて、最終冷延時に初期結晶方位に依存した
内部歪蓄積量の差異を拡大する役割を果たし、続
く脱炭焼鈍の昇温過程で再結晶する際、冷延後の
結晶内部に蓄積した歪量の多い(110)〔001〕方
位とその近傍の結晶方位を有する結晶粒ほど初期
に優先的に再結晶を開始し、より強いゴス方位を
もつ1次再結晶組織を形成するものと推定され、
したがつてこの発明の方法では上記2作用の相乗
効果によつて、よりゴス方位の強い集積をもつ集
合組織に改善される。
一方最終冷延前までの脱炭量が不足する場合
は、最終冷延前の1次再結晶組織は結晶粒度が不
均一で、微細な結晶粒が塊状に分布し、1次再結
晶集合組織は(110)〔001〕方位の集積が弱く、
比較的強い(111)<112>方位が分散する不適切
な組織となつており、最終冷延前に急冷を施して
100〜500Åの微細炭化物を均一に析出分散させて
も効果は少なく、その結果として製品の結晶組織
は細粒が混在する2次再結晶不良の状態となる。
また脱炭過多の場合、最終冷延前の結晶粒度が
不均一で粗大な結晶粒が分散する不適切なものと
なり、その1次再結晶集合組織も(110)〔001〕
方位が減少している。また脱炭過多によつて、最
終冷延前の中間昇鈍での冷却の際、炭化物の析出
量が不充分となり、急冷によつて目的とする微細
炭化物の量を充分に確保できず、したがつてこの
状態から得られた製品の結晶組織は著しく粗大な
2次再結晶粒で占められ、またこれらの粗大結晶
粒は(110)〔001〕方位からやや偏倚した方位が
多く、従つて磁気特性が不充分となり、鉄損値も
増大する傾向がみられる。
以上詳述したように、最終冷延前の適量の脱炭
と所期の結晶粒内炭化物サイズとが組合わされた
場合にのみ、著しく低い低損値と充分に高い磁束
密度が得られるのであり、脱炭量が適切な範囲で
あつても粒内炭化物が未析出あるいは500Åを越
えて成長した場合、あるいは逆に粒内炭化物析出
サイズが100〜500Åの範囲内であつても最終冷延
前の脱炭量が過不足した場合には初期の磁気特性
が得られない。
次に、前述の如く最終冷延前に100〜500Åの範
囲内の超微小炭化物を結晶粒内に充分に析出させ
るための具体的方法について説明する。
第6図は、中間昇鈍後770〜100℃の間を冷却所
要時間22秒で急冷し、直ちに100〜300℃の温度範
囲で時効処理を施した場合の時効処理温度および
処理時間と粒内炭化物析出サイズとの関係を示
す。第6図から、急冷後の時効処理により100〜
500Åの範囲内の超微小炭化物を析出させるため
には、150〜250℃の温度範囲で2〜60秒間、但し
温度が低い程度長く保持するように選択すること
が適切であることが判明した。ここで、最終冷延
前の中間昇鈍後の冷却の際においては、770℃で
Cの固溶量が最大となるため、770℃以下の領域
の冷却速度が遅ければ微細炭化物の析出開始まで
に結晶粒界等に粗大炭化物が析出してしまい、所
定量の微細炭化物の析出分散が得られなくなつて
集合組織の改善を図ることができなくなるから、
時効処理前の冷却は、770〜100℃の間を30秒以内
で急冷することとした。
さらに本発明者等は、中間昇鈍後の冷却過程の
うち、特に従来は看過されてきた温度範囲である
300℃以下の冷却過程を厳密に制御することによ
つて、冷却後の時効処理を不要とする方法の開発
を試みた。すなわち第6図から理解されるように
超微小炭化物は300℃以下、150℃程度以上の温度
範囲で粒内析出することに着目し、770〜300℃間
は前記同様に急冷して300〜150℃の温度範囲を各
種の冷却速度で冷却し、その300〜150℃の間の冷
却中に粒内超微小炭化物を析出させることを試み
た。具体的には、最終冷延前の中間焼鈍後の冷却
に際して、770〜300℃間はミストジエツト冷却に
より冷却所要時間15秒で急冷した後、続いて300
℃以下の温度域を水冷から自然放冷まで種々の冷
却速度で冷却させ、300〜150℃間の冷却所要時間
と粒内炭化物析出サイズおよび製品の磁気特性と
の関係を調べたところ、第7図に示す結果が得ら
れた。但しここで最終冷延前の中間焼鈍における
脱炭量はこの発明の範囲内である0.012%である。
第7図から、100〜500Åの粒内炭化物析出サイ
ズを得るためには、300〜150℃間の冷却所要時間
を8〜30秒の範囲内に選択すべきであることが判
明し、またその場合に著しく低い鉄損値と充分に
高い磁速密度が得られることが明らかとなつた。
以上のように、最終冷延前の鋼板の結晶粒内に
100〜500Åのサイズの超微小炭化物を分散析出さ
せるための工業的な方法としては、最終焼鈍前の
中間焼鈍の冷却過程において、770〜100℃の間を
30秒以内で急冷した後直ちに150〜250℃の温度に
おいて2〜60秒間の時効処理する方法、あるいは
770〜300℃の間を20秒以内で急冷し、続いて300
〜150℃の間の冷却所要時間を8〜30秒の範囲内
に制御する方法が適当であることが明らかとなつ
た。なおこれらの方法はいずれも工業的に容易に
実施可能なものであるが、特に後者の方法によれ
ば冷却時間の短縮により連続炉操業を効率良く行
ない得る利点がある。
次にこの発明の方法に適用される珪素鋼素材の
成分限定理由について説明する。
Siは比抵抗を高めて鉄損を低減させるに有効な
元素であり、2.8%よりも少なければ充分な低鉄
損値を達成することができず、逆に4.0%を越え
れば著しく脆くなつて冷延加工性が低下し、通常
の工業的冷延が困難となるから2.8〜4.0%の範囲
に限定した。なおSiは2.8〜4.0%の範囲内におい
てその含有量を高める程、一般に低徹損の製品を
得ることができるが、実際操業においてはSi量を
高めればSi原料費が上昇することはもちろんのこ
と、冷延歩留の低下によるコスト上昇を招くか
ら、Si含有量は得るべき所期の鉄損水準に応じて
適宜選定することが必要である。
CはSi量に応じて前記(2)式の範囲内に調整すべ
きことは前述の通りである。すなわち第1図に示
した熱延中1150℃におけるγ相生成量がほぼ10〜
30%に相当するC含有量範囲とする必要がある。
前記(2)式による具体的数値を例示すれば次の第2
表の通りである。[Table] Also, the broken lines A, B, C, D,
E is the estimated value of the amount of γ phase formed at 1150℃ during hot rolling, and the amount of γ phase formed is 40%, 30%, and 20%, respectively.
%, 10% and 0% cases are shown. Here, the amount of γ phase produced substantially changes depending on the amount of Si, the amount of C, and the temperature.
D and E are the correlations between the measured values of the amount of γ phase generated in the equilibrium state at 1150°C and the amount of Si and C in the steel, which were determined by experiments for silicon steel specimens with various amounts of Si and C. This is calculated from the following equation (1) derived from . γ%=67log([C%]×10 3 )−25[Si%]−8……(1
) As is clear from Figure 1 and Table 1, the absolute iron loss level that is judged to be good differs depending on the Si content, but depending on the Si content, the iron loss W 17/50 is excellent.
It has been found that the appropriate range of the amounts is limited between the dashed lines D and B, that is, when the amount of γ phase produced is within the range of 10 to 30%. However, unlike the equilibrium state, the γ phase generated during the hot rolling process is metastable, and it is difficult to accurately grasp the amount of γ phase generated during actual hot rolling at 1150°C. Therefore, it is not practical to limit the amount by the amount of γ phase produced, so if the estimated γ phase produced by the above equation (1) is 10~
It is considered appropriate to limit the range of the amount of C according to the amount of Si in the material so that it falls within the range of 30%. Based on this idea, in this invention, C
The range of C content was derived from the above equation (1), and this was determined as the appropriate range of C content to obtain an excellent level of iron loss. That is, the appropriate range of this C amount is expressed by the following equation (2). 0.37[Si%]+0.27≦log([C%]×10 3 )≦0.37[Si%]+0.57...(2) This is the first characteristic requirement of this invention. If the C amount is insufficient than the lower limit of the appropriate C amount range according to the Si amount shown by the above formula (2), and therefore the composition corresponds to less than 10% of the γ phase formation amount during hot rolling, , the crystal structure of the product showed a clear band-like fine grain structure, and deterioration of magnetic properties was observed. In addition, products with a composition in which the amount of γ phase produced during hot rolling is 10% or more, as shown by line D in Figure 1, have almost no band-like fine grains and are mostly composed of normally developed secondary recrystallized grains. It turned out that it was. Therefore, in order to split and destroy the coarse crystal grains that have grown abnormally during the hot rolling process when heating the slab at high temperatures, and to prevent the generation of band-like fine grains in the product, it is necessary to generate a γ phase of a predetermined amount or more. ,
It has been found that the required predetermined amount of the γ phase can be achieved by including an amount of C so that 10% or more of the γ phase is generated during hot rolling in an equilibrium state depending on the amount of Si contained. On the other hand, if the amount of C is significantly excessive,
In other words, if the composition corresponds to a composition in which the amount of γ phase produced during hot rolling exceeds 30%, the crystal structure of the product becomes a fine-grained structure with incomplete development of secondary recrystallization, and exhibits extremely poor magnetic properties. Ta. As mentioned above, depending on the amount of Si, the band-shaped grain structure in the product can only be improved if the amount of C is such that γ phase will be produced in the range of 10 to 30% in equilibrium during hot rolling. It is possible to prevent the generation of a fine-grained structure on the entire surface where the generation or development of secondary recrystallized grains is incomplete, and therefore, limiting the amount of C according to the amount of Si using equation (2) above is extremely effective in improving magnetic properties. It turned out to be effective. However, even within the range of 10 to 30% of the amount of γ phase produced in Figure 1, there are still some particles with insufficient iron loss characteristics, and this is seen from the viewpoint of industrial production where stability of magnetic properties is required. From, C according to the above formula (2),
Regulation of the amount of Si alone is still not satisfactory. Therefore, the present inventors conducted research to further improve this and found that 0.006 to 0.020% of C was decarburized during the process from the end of the hot rolling process to the intermediate annealing before the final cold rolling process. They found that it is effective to stably obtain excellent magnetic properties, and made this the second characteristic requirement of the present invention. This requirement was clarified from the following experimental results by the inventors. That is, among the test materials used in the experiment shown in FIG. The magnetic properties of the product and the C characteristics immediately after the end of the hot rolling process and after the intermediate annealing before the final cold rolling of the sample material whose composition is within the range corresponding to 10 to 30% of the amount of γ phase formed at 1150°C during hot rolling. As a result of a detailed investigation of the relationship between the content difference, that is, the decarburization amount ΔC, the results shown in FIG. 2A and B were obtained. In Figure 2, the white circles indicate the group with Si content of 2.8 to 3.1%, and the black circles indicate the group with Si content of 3.3 to 3.5%.
Each group is shown below. As is clear from Figure 2 A and B, excellent magnetic properties are stably obtained when the decarburization amount ΔC is 0.006% or more and 0.020% or less, and C
It has been found that when the ratio is less than 0.006% or more than 0.020%, the magnetic flux density is insufficient and the iron loss also shows a large value, making it impossible to obtain sufficient magnetic properties. In addition, the amount of decarburization during the period from hot rolling to final cold rolling in the production of ordinary silicon steel sheets is about 0.005% or less, so the amount of decarburization in the method of this invention is 0.006 to 0.020% compared to that in the conventional method. Since the amount of decarburization is larger than the normal decarburization amount, when carrying out the method of the present invention, it is usually necessary to carry out active decarburization treatment such as making the intermediate annealing atmosphere decarburizing. In this way, by performing a suitable amount of strong decarburization between the end of hot rolling and before the final cold rolling, it is possible to compensate for the unsatisfactory points of the first requirement explained earlier and to maintain stable excellent magnetic properties. It became possible to obtain it. As mentioned above, the fact that an appropriate amount of decarburization is effective in improving and stabilizing magnetic properties is due to the following crystal structure,
This is also clear from the texture observation results. In other words, when the amount of decarburization is appropriate, the grain size before final cold rolling is uniform and appropriate, and the primary recrystallization texture is improved to a favorable state showing strong accumulation of (110) [001] orientation. As a result, the crystal structure of the product is one in which normal secondary recrystallized grains are sufficiently developed. On the other hand, when the amount of decarburization is insufficient, the grains in the primary recrystallized texture are irregular and lumpy carbides remain, and the primary recrystallized texture has a weak accumulation of (110) [001] orientations. <112> The structure has an inappropriate structure with dispersed orientation, resulting in a mixture of fine grains.
The next recrystallization is in a state of poor development. In addition, in the case of excessive decarburization, the grain size before the final cold rolling is uneven and coarse grains are dispersed, making it inappropriate, and the primary recrystallization texture also decreases in the (110) [001] orientation. Therefore, after the secondary recrystallization, the crystal grains are extremely coarse, and the crystal orientation of these is (110) [001]
Many of the bearings were slightly deviated from the normal direction, and the magnetic properties were therefore insufficient. As mentioned above, the present inventors have found that an appropriate amount of decarburization is effective in improving and stabilizing magnetic properties. As a result of our efforts to develop a grain-oriented silicon steel sheet with extremely excellent properties of less than 1.00W/Kg, we have discovered that carbides within the grains of the steel sheet cannot be seen with an optical microscope after intermediate annealing before final cold rolling. By combining the above two requirements with a process that controls the precipitation within a specific extremely small range that cannot be achieved and causes the precipitation to occur in a sufficiently large amount, the texture before final annealing can be made into a state where the accumulation of (110) [001] orientation is even stronger. can be improved,
As a result, we newly discovered that secondary recrystallized grains with highly aligned (110) [001] orientation are formed in the secondary recrystallization process during final annealing, resulting in excellent magnetic properties. The third characteristic requirement of the present invention is a treatment for controlling carbides within the crystal grains. The effect of the third requirement will be explained below based on the experimental results of the present inventors. The material used in the experiment was C0.045
%, Si3.20%, Mn0.06%, Se0.025%, and
It is a hot-rolled plate with a thickness of 3.0 mm that has a composition of 0.020% Sb and is finished through normal steel manufacturing, continuous casting, and hot rolling. After annealing such a hot-rolled plate at 950°C for 2 minutes, it was pickled and subjected to the first cold rolling to give an intermediate plate thickness of 0.75mm. After intermediate annealing at 900°C for 3 minutes,
The final cold rolling was carried out with a rolling reduction of 60%, resulting in a final thickness of 0.30 mm. Next, decarburization annealing was performed in a wet hydrogen atmosphere at 800℃, and after coating with MgO, final annealing was performed at 1200℃×10
Time holding annealing was performed to obtain a unidirectional silicon steel plate product. In the above experiment, the decarburization amount ΔC in the intermediate annealing between the cold rolling processes was set to three levels: 0.002%, which is the conventional standard, 0.012%, which is within the limited range of this invention, and 0.025%, which is excessive decarburization. In addition, cooling to 770℃ or less in the cooling process after intermediate annealing is oil quenching (rapid cooling corresponding to a cooling time of about 10 seconds at 770 to 100℃), and immediately aging treatment at 200℃.
It was carried out by varying the time between ~200 seconds. The relationship between the intragrain carbide precipitate size and magnetic properties in the steel sheet after this aging treatment, that is, the steel sheet after intermediate annealing and before final cold rolling, and also the relationship between the carbide precipitate size and 200
Figure 3 shows the relationship with the aging treatment time at °C. The magnetic property plot in Figure 3 shows that the amount of decarburization ΔC is
If 0.002%, mark ○; if ΔC0.012%, mark ●;
The case where ΔC is 0.025% is indicated by a mark ◎. Moreover, as a comparative material in FIG. 3, a sample is shown which was forced air cooled at a cooling rate corresponding to a cooling time of 98 seconds between 770 and 100° C., which is generally used in industrial continuous annealing. As is clear from Fig. 3, the amount of decarburization is
Appropriate amount (● mark) within the requirements of 200
When the aging treatment time at °C is about 10 to 20 seconds, the magnetic flux density B 10 value is 1.94T or more, and the iron loss W 17/50 is
Exhibits extremely excellent magnetic properties of less than 1.00W/Kg,
In addition, the carbide precipitation size in this case is 100 to 500
It is clear that it is in the range of Å. Also, an electron micrograph of the carbide precipitation state in this case (10,000x magnification)
is shown in Figure 4A. However, this electron micrograph is
After intermediate annealing before final cold rolling, the samples were rapidly cooled from 770 to 100°C for 22 seconds, and then immediately aged at 200°C for 10 seconds.The average carbide grain size was 200 Å, and the carbide It is clear that the particles are uniformly and abundantly dispersed. On the other hand, in the case of oil quenching after intermediate annealing (no aging treatment) and aging treatment at 200℃ for 2 seconds, it is clear that the magnetic properties are insufficient regardless of the amount of decarburization, and in this case, the crystallization No intragranular carbide was observed or only a small amount of intragranular carbide was precipitated locally. Furthermore, when the aging treatment at 200°C was performed for 30 seconds or longer, it was clear that the magnetic properties were insufficient regardless of the amount of decarburization, and in this case, the precipitated size of intracrystalline carbides exceeded 500 Å. For reference, an electron micrograph (10,000x magnification) of the state of carbide precipitation before the final cold rolling of a comparative material subjected to industrial standard cooling (cooling time between 770 and 100°C for approximately 98 seconds) after intermediate annealing. is shown in Figure 4B. In this case, the average grain size of intragrain carbide precipitation is approximately 700 Å,
In addition, the magnetic properties were as poor as those obtained when the material was rapidly cooled after intermediate annealing and then subjected to aging treatment at 200°C for 30 seconds or more. Furthermore, from Fig. 3, we can see that when the amount of decarburization ΔC is at the conventional normal level (○ mark) and when there is excessive decarburization (◎
It is clear from the mark) that even if the material is rapidly cooled after intermediate annealing and then immediately subjected to aging treatment at 200°C for about 10 to 20 seconds, the magnetic properties are slightly improved, but not significantly. From the above experimental results, it is possible to improve the magnetic properties by applying a treatment that reduces the carbide size within the crystal grains within the range of 100 to 500 Å after intermediate annealing and before final cold rolling, sometimes on materials with an appropriate amount of decarburization. It turned out that the problem could be improved significantly. Furthermore, the present inventors (A) did not actively decarburize in the intermediate annealing process, and did not perform rapid cooling in the cooling process after the intermediate annealing before the final cold rolling, but instead carried out standard cooling (cooling time required between 770 and 100°C). (approximately 90 seconds), (B) intermediate annealing process
If 0.006 to 0.020% decarburization is performed and standard cooling is performed without rapid cooling in the cooling process after intermediate annealing before final cold rolling, (C) without active decarburization in intermediate annealing process, (D) If the temperature range of 770 to 100℃ is rapidly cooled within 30 seconds in the cooling process after intermediate annealing, and then immediately subjected to aging treatment at 200℃ for about 10 to 20 seconds, (D)
If 0.006 to 0.020% decarburization is performed and the same rapid cooling and aging treatment as in (C) above is performed in the cooling process after intermediate annealing before final cold rolling, the above four types of (A) to (D) When examining the Goss orientation strength of the surface layer of the decarburized annealed sheet before final annealing for the cold rolled sheet obtained by the treatment, it was found that:
The results shown in FIG. 5 were obtained. From Figure 5, when neither decarburization nor rapid cooling-aging treatment is performed
Compared to (A), the Goss orientation strength is about 1.5 times higher in the case of decarburization only (B) and the case of quenching-aging treatment only (C), and furthermore, the It was confirmed that when both the quenching and quenching-aging treatments were applied (D), the Goss orientation strength was approximately 1.7 times higher than that of (A). The reason why the Goss orientation strength is increased by the method of the present invention is considered to be as follows. That is, by decarburizing an appropriate amount, the recrystallization initiation temperature becomes lower in the intermediate annealing before the final cold rolling, which is advantageous for the growth of Goss grains, which are said to recrystallize at a constant temperature, and further increases the recrystallization temperature. The reduction in the amount of α-γ transformation during soaking after crystallization prevents the randomization of the texture and improves the texture to one with strong accumulation in the Goss orientation. In addition, the uniform precipitation and dispersion of ultrafine carbides before the final cold rolling plays a role in expanding the difference in the amount of internal strain accumulation depending on the initial crystal orientation during the final cold rolling, and the subsequent decarburization annealing. When recrystallizing during the heating process, crystal grains with the (110) [001] orientation and crystal orientations in its vicinity, which have a large amount of strain accumulated inside the crystal after cold rolling, start recrystallizing early and preferentially. , it is estimated that a primary recrystallized structure with a stronger Goss orientation is formed.
Therefore, in the method of the present invention, the synergistic effect of the above two effects improves the texture to have a stronger accumulation of Goss orientation. On the other hand, if the amount of decarburization before the final cold rolling is insufficient, the primary recrystallized texture before the final cold rolling will have uneven grain size, fine crystal grains will be distributed in clusters, and the primary recrystallized texture will be has a weak accumulation of (110)[001] directions,
It has an unsuitable structure with relatively strong (111) <112> orientations dispersed, and it is necessary to perform rapid cooling before the final cold rolling.
Even if fine carbides of 100 to 500 Å are precipitated and dispersed uniformly, the effect is small, and as a result, the crystal structure of the product is in a state of poor secondary recrystallization in which fine grains are mixed. In addition, in the case of excessive decarburization, the grain size before the final cold rolling becomes uneven and inappropriate with coarse grains dispersed, and the primary recrystallization texture also becomes (110) [001].
Orientation is decreasing. In addition, due to excessive decarburization, the amount of carbides precipitated was insufficient during cooling during the intermediate elevating and slowing before the final cold rolling, and the desired amount of fine carbides could not be secured by rapid cooling, resulting in However, the crystal structure of the product obtained from this state is dominated by extremely coarse secondary recrystallized grains, and many of these coarse grains have an orientation slightly deviated from the (110) [001] orientation, and therefore are magnetically There is a tendency for the characteristics to become insufficient and the iron loss value to increase. As detailed above, extremely low loss values and sufficiently high magnetic flux densities can be obtained only when a suitable amount of decarburization before the final cold rolling is combined with the desired intra-grain carbide size. Even if the amount of decarburization is within an appropriate range, intragranular carbides are not precipitated or have grown to a size exceeding 500 Å, or conversely, even if the intragranular carbide precipitation size is within the range of 100 to 500 Å, it is necessary to If the amount of decarburization is too much or too little, the initial magnetic properties cannot be obtained. Next, a specific method for sufficiently precipitating ultrafine carbides within the range of 100 to 500 Å within the crystal grains before the final cold rolling as described above will be described. Figure 6 shows the aging treatment temperature, treatment time, and grain interior when the cooling time is 22 seconds between 770 and 100 degrees Celsius after intermediate aging, and the aging treatment is immediately performed in the temperature range of 100 to 300 degrees Celsius. The relationship with carbide precipitation size is shown. From Figure 6, 100 ~
In order to precipitate ultrafine carbides within the range of 500 Å, it was found that it is appropriate to hold the temperature in the temperature range of 150 to 250°C for 2 to 60 seconds, but as long as the temperature is low. . During the cooling after the intermediate elevating and slowing before the final cold rolling, the amount of solid solution of C reaches its maximum at 770°C, so if the cooling rate in the region below 770°C is slow, it will take until the precipitation of fine carbides begins. Coarse carbides precipitate at grain boundaries etc., making it impossible to obtain a predetermined amount of precipitated and dispersed fine carbides, making it impossible to improve the texture.
Cooling before aging treatment was performed by rapidly cooling between 770 and 100°C within 30 seconds. Furthermore, the present inventors have discovered that the temperature range of the cooling process after the intermediate rise and slowing has been particularly overlooked in the past.
We attempted to develop a method that eliminates the need for aging treatment after cooling by strictly controlling the cooling process below 300℃. In other words, as can be understood from Fig. 6, we focused on the fact that ultrafine carbides precipitate within the grains at a temperature range of 300°C or lower and approximately 150°C or higher, and from 770°C to 300°C, we rapidly cooled in the same manner as above. An attempt was made to precipitate intragranular ultrafine carbides during cooling between 300 and 150 degrees Celsius by cooling at various cooling rates over a temperature range of 150 degrees Celsius. Specifically, during cooling after intermediate annealing before final cold rolling, the temperature between 770 and 300°C is rapidly cooled by mist jet cooling for a cooling time of 15 seconds, and then quenched at 300°C.
When cooling the temperature range below ℃ at various cooling rates from water cooling to natural cooling, we investigated the relationship between the cooling time between 300 and 150℃, the size of intragranular carbide precipitation, and the magnetic properties of the product. The results shown in the figure were obtained. However, the amount of decarburization in the intermediate annealing before the final cold rolling is 0.012%, which is within the scope of this invention. From Figure 7, it is clear that in order to obtain an intragranular carbide precipitate size of 100 to 500 Å, the required cooling time between 300 and 150°C should be selected within the range of 8 to 30 seconds; It has become clear that extremely low iron loss values and sufficiently high magnetic velocity densities can be obtained in this case. As mentioned above, within the grains of the steel sheet before the final cold rolling,
An industrial method for dispersing and precipitating ultrafine carbides with a size of 100 to 500 Å is to heat between 770 and 100°C during the cooling process of intermediate annealing before final annealing.
A method of rapidly cooling within 30 seconds and then immediately aging at a temperature of 150 to 250℃ for 2 to 60 seconds, or
Rapid cooling between 770 and 300℃ within 20 seconds, followed by 300℃
It has become clear that a method of controlling the time required for cooling between 8 and 30 seconds between temperatures of 150 DEG C. and 150 DEG C. is appropriate. All of these methods can be easily implemented industrially, but the latter method in particular has the advantage of allowing efficient continuous furnace operation due to shortening of cooling time. Next, the reason for limiting the composition of the silicon steel material applied to the method of the present invention will be explained. Si is an effective element for increasing resistivity and reducing iron loss; if it is less than 2.8%, a sufficiently low iron loss value cannot be achieved, and on the other hand, if it exceeds 4.0%, it becomes extremely brittle. The content was limited to a range of 2.8 to 4.0% because cold rolling workability would be reduced and normal industrial cold rolling would be difficult. In general, products with lower penetration loss can be obtained by increasing the Si content within the range of 2.8 to 4.0%, but in actual operation, increasing the Si content not only increases the Si raw material cost. In other words, a decrease in cold rolling yield leads to an increase in cost, so it is necessary to appropriately select the Si content depending on the desired iron loss level to be obtained. As mentioned above, C should be adjusted within the range of formula (2) according to the amount of Si. In other words, the amount of γ phase formed at 1150°C during hot rolling as shown in Figure 1 is approximately 10~
It is necessary to keep the C content within the range equivalent to 30%.
An example of a specific numerical value based on the above formula (2) is the following second value.
As shown in the table.
【表】
但しC量が0.015%未満では、Si量が2.8〜4.0%
の範囲での必要量のγ相量が確保されず、一方C
量が0.10%を越えれば脱炭工程に長時間を要し、
経済的に不利となるから、Cが0.015〜0.10%の
範囲内で前記(2)式を満足させる必要がある。
Mn、S、Se、Sbはいずれもインヒビターとし
て添加され、最終焼鈍において1次再結晶粒の成
長を抑制し、(110)〔001〕方位の2次再結晶粒を
先鋭に発達させるに必要な元素である。しかしな
がらMn0.02〜0.15%、S、Seのいずれか1種ま
たは2種とSbとを合計量で0.008〜0.080%の範囲
を逸脱して過不足すれば、2次再結晶が不安定と
なり、目的とする優れた磁気特性が得られなくな
るから、上記範囲に限定した。
この発明の方法が適用される珪素鋼素材は、上
述の各成分のほかは特に限定されるものはない
が、さらに適宜粒界偏析型元素例えばAs、Bi、
Pb、Sn、Te等を単独もしくは複合して添加し
て、インヒビターの効果を補強しても良い。但し
これらの粒界偏析型元素の添加は、この発明の特
有の効果発揮に特別に影響を及ぼすものではな
い。
次にこの発明の方法による一方向性珪素鋼板の
製造過程の全体を工程順に説明する。
この発明において使用される珪素鋼スラブは従
来の造塊−分塊法によつて得られたものでも、ま
た連続鋳造法によつて得られたものでも良いが、
この発明の方法は特に連鋳製スラブを用いた場合
に効果的な磁気特性の安定化および向上効果が得
られる。この発明の方法においては、珪素鋼スラ
ブを1250℃程度以上に加熱後、公知の方法により
熱間圧延を施し、板厚1.2〜5.0mmの熱延板に仕上
げ、必要に応じて750〜1100℃のノルマライジン
グ焼鈍を施し、次いで750〜1100℃の中間焼鈍を
挾む2回以上の冷間圧延を施して最終板厚0.15〜
0.50mmの最終冷延板とする。そしてこの工程の途
中、熱延後から最終冷延前までの工程間におい
て、すなわち熱延巻取後の自己焼鈍中あるいは前
記ノルマライジング焼鈍または中間焼鈍のうちの
少くとも一つの工程において雰囲気を脱炭性に調
整し、合計で0.006〜0.020%の脱炭を行う。脱炭
焼鈍雰囲気の脱炭性の強さは、素材の組成、板
厚、焼鈍時間等により適宜調整すべきであり、ま
た熱延コイル巻取後の自己焼鈍時を利用する場
合、コイル層間にFe2O3等の酸化物を塗布する等
の方法により熱延板の脱炭焼鈍を行うことも可能
である。
また前記冷延工程における最終冷延前の中間焼
鈍の冷却過程においては、前述した各冷却方法を
用いて、最終冷延前の鋼板の結晶粒内に100〜500
Åのサイズの超微小炭化物を充分に析出させてお
き、次いで最終冷延圧下率40〜80%にて製品厚に
冷延する。この発明においては最終冷延前までに
適度の脱炭と炭化物の微細析出処理を行うことで
結晶組織を均一化し、集合組織中の(110)〔001〕
方位の強い集積を促進させるのであるが、この効
果は最終冷延圧下率40%未満もしくは80%を越す
場合には得られず、40〜80%の最終冷延圧下率範
囲によつてはじめて達成されるのである。
上述のような冷延工程終了後には、通常は湿水
素雰囲気中で750〜850℃の温度範囲においてCを
0.003%以下まで脱炭させる脱炭焼鈍を行う。そ
の後MgO等の焼鈍分離剤を塗布した後、最終焼
鈍を施す。この最終焼鈍は、S、Se、N等の不
純物元素の除去ならびにフオルステライトを主体
とする電気絶縁被覆の形成を図るため、1000℃程
度以上、望ましくは1050〜1250℃の温度範囲にて
数時間以上保持することが望ましい。なおこの最
終焼鈍は、900℃以上の高温焼鈍のときは不純物
の除去を促すために焼鈍雰囲気として水素を用い
ることが必要であるが、その高温焼鈍の前に予め
820〜900℃程度で低温保定焼鈍を行う場合、その
雰囲気としては水素、窒素、アルゴンのいずれを
用いても良い。
以下この発明の実施例を記す。
実施例 1
Si3.35%、C0.050%、Mn0.06%、Se0.023%お
よびSb0.020%を含有する連鋳スラブに公知の熱
間圧延を施して得られた多数の2.5mm厚の熱延板
をそれぞれ950℃×2分間の焼鈍後酸洗して、第
1回冷間圧延により中間板厚0.75mmとし、引続い
て950℃×2分間の焼鈍時にPH2O/PH2=0.003〜
0.35の範囲の湿水素雰囲気で処理して、脱炭量
ΔCをこの発明の範囲外の0.002%、0.025%および
この発明の範囲内の0.013%にそれぞれ調整し、
続く冷却過程において770〜100℃間の冷却所要時
間を22秒となるように冷却し、その後直ちに200
℃の時効処理を(A)なし、(B)10秒間、(C)40秒間の3
種類で施した。次いで圧下率60%の最終圧延によ
り板厚0.30mmに仕上げ、湿水素雰囲気中で830℃
×3分間を脱炭焼鈍を施し、MgOスラリー塗布
後、最終焼鈍として120℃×10時間の純化焼鈍を
施し、その後絶縁コーテイングを塗布して、一方
向性珪素鋼板の製品を得た。これらの製品の磁気
特性を測定した結果を、各工程条件と対応させて
第3表に示す。[Table] However, if the C content is less than 0.015%, the Si content will be 2.8 to 4.0%.
The required amount of γ phase is not secured within the range of C.
If the amount exceeds 0.10%, the decarburization process will take a long time,
Since this is economically disadvantageous, it is necessary to satisfy the above formula (2) within the range of 0.015 to 0.10% of C. Mn, S, Se, and Sb are all added as inhibitors and are necessary to suppress the growth of primary recrystallized grains in the final annealing and to sharply develop secondary recrystallized grains with (110) [001] orientation. It is an element. However, if the total amount of Mn 0.02 to 0.15%, one or two of S and Se, and Sb exceeds the range of 0.008 to 0.080%, secondary recrystallization will become unstable. Since the desired excellent magnetic properties would not be obtained, it was limited to the above range. The silicon steel material to which the method of the present invention is applied is not particularly limited other than the above-mentioned components, but may contain grain boundary segregated elements such as As, Bi, etc.
Pb, Sn, Te, etc. may be added alone or in combination to enhance the effect of the inhibitor. However, the addition of these grain boundary segregation type elements does not particularly affect the specific effects of this invention. Next, the entire process of manufacturing a unidirectional silicon steel plate by the method of the present invention will be explained in order of process. The silicon steel slab used in this invention may be obtained by the conventional ingot-blowing method or by the continuous casting method, but
The method of the present invention is particularly effective in stabilizing and improving magnetic properties when continuously cast slabs are used. In the method of this invention, a silicon steel slab is heated to about 1250°C or higher, then hot rolled by a known method to form a hot rolled plate with a thickness of 1.2 to 5.0 mm, and heated to 750 to 1100°C as necessary. Normalizing annealing at 750-1100℃ followed by cold rolling two or more times with intermediate annealing at 750-1100℃ to achieve a final plate thickness of 0.15~
The final cold-rolled sheet is 0.50mm. During this process, during the process from after hot rolling to before final cold rolling, that is, during self-annealing after hot-rolling, or at least one of the normalizing annealing or intermediate annealing, the atmosphere is removed. Adjust to carbonaceous properties and decarburize by 0.006 to 0.020% in total. The decarburizing strength of the decarburizing annealing atmosphere should be adjusted appropriately depending on the composition of the material, plate thickness, annealing time, etc. Also, when using the self-annealing time after winding the hot-rolled coil, there is a It is also possible to perform decarburization annealing of the hot rolled sheet by a method such as applying an oxide such as Fe 2 O 3 or the like. In addition, in the cooling process of intermediate annealing before the final cold rolling in the cold rolling process, each of the cooling methods described above is used to form a 100 to 500
Ultrafine carbides with a size of 100 Å are precipitated sufficiently, and then cold rolled to a product thickness at a final cold rolling reduction of 40 to 80%. In this invention, the crystal structure is made uniform by performing appropriate decarburization and fine carbide precipitation treatment before the final cold rolling, and the (110) [001]
This effect promotes a strong accumulation of orientation, but this effect cannot be obtained when the final cold rolling reduction is less than 40% or exceeds 80%, and is only achieved when the final cold rolling reduction is in the range of 40 to 80%. It will be done. After the cold rolling process described above is completed, C is usually heated in a wet hydrogen atmosphere at a temperature range of 750 to 850°C.
Perform decarburization annealing to decarburize to 0.003% or less. Then, after applying an annealing separator such as MgO, final annealing is performed. This final annealing is performed at a temperature of approximately 1000°C or higher, preferably in the range of 1050 to 1250°C, for several hours in order to remove impurity elements such as S, Se, and N, and to form an electrically insulating coating mainly composed of forsterite. It is desirable to maintain the above. In this final annealing, when performing high-temperature annealing at 900°C or higher, it is necessary to use hydrogen as an annealing atmosphere to promote the removal of impurities.
When low temperature holding annealing is performed at about 820 to 900°C, any of hydrogen, nitrogen, and argon may be used as the atmosphere. Examples of this invention will be described below. Example 1 A large number of 2.5 mm thick continuous cast slabs containing 3.35% Si, 0.050% C, 0.06% Mn, 0.023% Se and 0.020% Sb were subjected to known hot rolling. After annealing at 950°C for 2 minutes, each hot-rolled sheet was pickled, the intermediate plate thickness was 0.75 mm by the first cold rolling, and then P H2O /P H2 = 0.003〜
The decarburization amount ΔC was adjusted to 0.002% and 0.025%, which are outside the range of this invention, and 0.013%, which is within the range of this invention, respectively, by treatment in a wet hydrogen atmosphere in the range of 0.35%.
In the subsequent cooling process, the cooling time between 770 and 100℃ is 22 seconds, and then the temperature is immediately increased to 200℃.
℃ aging treatment (A) without, (B) 10 seconds, (C) 40 seconds
It was applied in different types. Then, final rolling was carried out at a reduction rate of 60% to a thickness of 0.30 mm, and the plate was heated at 830°C in a wet hydrogen atmosphere.
Decarburization annealing was performed for 3 minutes, and after applying MgO slurry, purification annealing was performed at 120°C for 10 hours as a final annealing, and then an insulating coating was applied to obtain a unidirectional silicon steel sheet product. The results of measuring the magnetic properties of these products are shown in Table 3 in correspondence with each process condition.
【表】
第3表から明らかなように、脱炭量ΔCがこの
発明の範囲よりも少ない0.002%である試料7、
8、9はいずれも充分に低い鉄損値が得られてい
ない。なおこれらの試料7、8、9のうち、炭化
物析出サイズがこの発明の範囲内となつている試
料8は製品における細粒発生率が0%であるため
わずかに磁性が改善されてはいるが、目的とする
充分な低鉄損値が得られなかつた。また脱炭量
ΔCが0.025%と脱炭量が過多であつた試料13、
14、15は、いずれも細粒発生率は0%であつた
が、2次再結晶粒が粗大化し、磁束密度は充分で
あつたが低鉄損値は得られなかつた。これに対し
この発明の要件を全て満足する試料11は、充分に
低い鉄損値と高い磁束密度が得られた。なお脱炭
量ΔCはこの発明の範囲内であるが炭化物析出サ
イズがこの発明の範囲を外れる試料10、12は、い
ずれも磁束密度が高くしかも鉄損値が相当に低か
つたが、本発明例(試料11)の如き超低鉄損値、
超高磁束密度を得るには至らなかつた。
実施例 2
Si3.35%、C0.050%、Mn0.06%、Se0.023%、
およびSb0.020%を含有する連鋳スラブに公知の
熱間圧延を施して得られた多数の2.5mm厚の熱延
板をそれぞれ950℃×2分間の焼鈍後、酸洗して
第1回冷間圧延により中間板厚0.75mmとし、引続
き950℃×2分間の中間焼鈍時にその連続焼鈍雰
囲気を公知の方法によりPH2O/PH2=0.003〜0.35
の範囲で変化させて処理し、脱炭量をこの発明の
範囲外の0.002%、0.025%、およびこの発明の範
囲内の0.013%にそれぞれ調整し、続く冷却過程
において770〜300℃の間の冷却所要時間を17秒ま
たは70秒とし、次いで300〜150℃間の冷却所要時
間を15秒または50秒に制御して冷却した。次いで
圧下率60%の最終冷延により板厚0.30mmに仕上げ
た後、湿水素中にて830℃×3分間の脱炭焼鈍を
施し、MgOスラリー塗布後、最終焼鈍として
1200℃×10時間の純化焼鈍を施し、その後絶縁コ
ーテイングを塗布して一方向性珪素鋼板の製品を
得た。これらの製品の磁気特性を調べた結果を各
条件と対応して第4表に示す。[Table] As is clear from Table 3, Sample 7 has a decarburization amount ΔC of 0.002%, which is less than the range of this invention.
In both No. 8 and No. 9, sufficiently low iron loss values were not obtained. Of these samples 7, 8, and 9, sample 8, in which the carbide precipitate size is within the range of this invention, has a slightly improved magnetism because the fine grain generation rate in the product is 0%. However, the desired low iron loss value could not be obtained. In addition, sample 13 had an excessive decarburization amount ΔC of 0.025%.
In both Nos. 14 and 15, the fine grain generation rate was 0%, but the secondary recrystallized grains became coarse, and although the magnetic flux density was sufficient, a low iron loss value could not be obtained. On the other hand, Sample 11, which satisfied all the requirements of the present invention, had a sufficiently low iron loss value and high magnetic flux density. Samples 10 and 12, in which the amount of decarburization ΔC is within the range of the present invention but the carbide precipitation size is outside the range of the present invention, both had high magnetic flux density and considerably low iron loss values, but were not in accordance with the present invention. Ultra-low iron loss value as shown in example (sample 11),
However, it was not possible to obtain an ultra-high magnetic flux density. Example 2 Si3.35%, C0.050%, Mn0.06%, Se0.023%,
A large number of 2.5 mm thick hot-rolled plates obtained by performing known hot rolling on continuous cast slabs containing 0.020% Sb were annealed at 950°C for 2 minutes, and then pickled. The intermediate plate thickness was made 0.75 mm by cold rolling, and then during intermediate annealing at 950°C for 2 minutes, the continuous annealing atmosphere was changed to P H2O /P H2 = 0.003 to 0.35 using a known method.
The amount of decarburization was adjusted to 0.002%, 0.025%, which is outside the range of this invention, and 0.013%, which is within the range of this invention, and in the subsequent cooling process, the amount of decarburization was varied within the range of 770 to 300°C. The required cooling time was set to 17 seconds or 70 seconds, and then the required cooling time between 300 and 150°C was controlled to 15 seconds or 50 seconds. Then, after final cold rolling with a rolling reduction of 60% to a thickness of 0.30 mm, decarburization annealing was performed at 830°C for 3 minutes in wet hydrogen, and after applying MgO slurry, final annealing was performed.
Purification annealing was performed at 1200°C for 10 hours, and then an insulating coating was applied to obtain a unidirectional silicon steel plate product. The results of examining the magnetic properties of these products are shown in Table 4 in correspondence with each condition.
【表】
第4表から明らかなようにこの発明の各要件を
満足する試料18は、その他の試料、すなわちこの
発明の各要件のうち1つ以上を欠いている比較例
の試料と比較して、著しく高い磁束密度と著しく
低い鉄損値が得られ、満足すべき一方向性珪素鋼
板となつている。
実施例 3
C0.049%、Si3.30%、Mn0.080%、S0.026%、
Sb0.026%を含有する連鋳スラブに公知の熱間圧
延を施して得られた2.7mm厚の熱延板について、
酸洗後、0.77mm厚に中間冷延し、次いで980℃×
1.5分間の中間焼鈍をPH2O/PH2=0.25の湿水素雰
囲気で施して、脱炭量ΔCを0.015%とし、かつそ
の中間焼鈍後の冷却は770℃〜300℃間の所要時間
を12秒、300℃〜150℃の間の所要時間を20秒と
し、その後圧下率65%の最終冷延により0.27mm厚
に仕上げた。その後湿水素雰囲気中で830℃×3
分間の脱炭焼鈍を施し、MgOスラリーを塗布し
た後、最終焼鈍として、昇温途中で840℃×60時
間保定後1200℃×10時間の純化焼鈍を施し、その
後絶縁コーテイングを施して本発明例による一方
向性珪素鋼板の製品(試料No.31)を得た。
比較のため、上記の本発明例で用いたと同じ成
分組成、厚みの熱延板について、酸洗後、0.77mm
厚に中間冷延し、その後980℃×1.5分間の中間焼
鈍を通常の雰囲気で施して脱炭量0.002%とし、
その中間焼鈍後の冷却は、770℃〜300℃の間の所
要時間を47秒、300℃〜150℃の間の所要時間を45
秒とし、その後圧下率65%の最終冷延により0.27
mm厚に仕上げた。その後、前記の本発明例の場合
と同様に脱炭焼鈍、MgOスラリー塗布、最終焼
鈍、絶縁コーテイングを施して、比較例による一
方向性珪素鋼板の製品(試料No.30)を得た。
これらの製品について磁気特性を測定した結果
を第5表に示す。[Table] As is clear from Table 4, sample 18 that satisfies each requirement of this invention is compared with other samples, that is, samples of comparative examples that lack one or more of the requirements of this invention. , a significantly high magnetic flux density and a significantly low core loss value were obtained, making it a satisfactory unidirectional silicon steel sheet. Example 3 C0.049%, Si3.30%, Mn0.080%, S0.026%,
Regarding a 2.7 mm thick hot rolled plate obtained by performing known hot rolling on a continuously cast slab containing 0.026% Sb,
After pickling, intermediate cold rolling to 0.77mm thickness, then 980℃×
Intermediate annealing for 1.5 minutes was performed in a wet hydrogen atmosphere with P H2O /P H2 = 0.25 to achieve a decarburization amount ΔC of 0.015%, and cooling after the intermediate annealing took 12 seconds from 770℃ to 300℃. The time required between 300°C and 150°C was 20 seconds, and the final cold rolling was then carried out to a thickness of 0.27 mm at a rolling reduction of 65%. After that, 830℃ x 3 in a wet hydrogen atmosphere
After applying decarburization annealing for 1 minute and applying MgO slurry, as final annealing, purification annealing was performed at 1200°C x 10 hours after holding at 840°C for 60 hours during heating, and then an insulating coating was applied. A unidirectional silicon steel plate product (sample No. 31) was obtained. For comparison, a hot-rolled sheet with the same composition and thickness as used in the above-mentioned inventive example was 0.77 mm after pickling.
It is intermediately cold rolled to a thick thickness and then subjected to intermediate annealing at 980°C for 1.5 minutes in a normal atmosphere to achieve a decarburization amount of 0.002%.
Cooling after intermediate annealing takes 47 seconds between 770℃ and 300℃, and 45 seconds between 300℃ and 150℃.
0.27 seconds and then final cold rolling with a rolling reduction of 65%.
Finished in mm thickness. Thereafter, decarburization annealing, application of MgO slurry, final annealing, and insulation coating were performed in the same manner as in the case of the present invention example, to obtain a unidirectional silicon steel sheet product (sample No. 30) according to the comparative example. Table 5 shows the results of measuring the magnetic properties of these products.
【表】
第5表から明らかなように、この発明の方法に
より製造された本発明例の製品(試料No.31)は、
比較例の製品(試料No.30)と比較して磁気特性に
優れていることが判明した。
実施例 6
C0.051%、Si3.25%、Mn0.085%、S0.021%、
Se0.005%、Sb0.026%を含有する連鋳スラブに公
知の熱間圧延を施して得られた2.0mm厚の熱延板
について、酸洗後、PH2O/PH2=0.20の湿水素雰
囲気で930℃×2.5分間の熱延板焼鈍(脱炭量ΔC
=0.008%)を施し、次いで0.70mm厚に中間冷延
した後、PH2O/PH2=0.20の湿水素雰囲気で950℃
×2分間の中間焼鈍(脱炭量ΔC=0.009%)を施
し、かつその中間焼鈍後の冷却は、770℃〜100℃
間の所要時間を13秒として冷却した後、直ちに
225℃×30秒間の時効処理を施し、さらに圧下率
67%の最終冷延を施して0.23mm厚に仕上げた。そ
の後湿水素雰囲気中で830℃×3分間の脱炭焼鈍
を施し、さらにMgOスラリーを塗布した後、最
終焼鈍として、850℃×55時間保定後1200℃×10
時間の純化焼鈍を施し、その後絶縁コーテイング
を塗布して、本発明例による一方向性珪素鋼板の
製品(試料No.33)を得た。
比較のため、上記本発明例と同じ成分組成、同
じ厚みの熱延板について、930℃×2.5分間の焼鈍
(脱炭量ΔC=0.002%)を施した後、酸洗し、0.70
mm厚に中間圧延した後、950℃×2分間の中間焼
鈍(脱炭量ΔC=0.002%)を施し、かつその中間
焼鈍後の冷却は770℃〜100℃間の所要時間を67秒
として行ない、時効処理は行なわなかつた。さら
に圧下率67%の最終冷延を施して0.23mm厚に仕上
げた後、前記の本発明例の場合と同様に脱炭焼
鈍、MgOスラリー塗布、最終焼鈍、絶縁コーテ
イングを施した。
これらの製品について磁気特性を測定した結果
を第6表に示す。[Table] As is clear from Table 5, the product of the present invention example (sample No. 31) manufactured by the method of the present invention is:
It was found that the magnetic properties were superior to that of the comparative product (sample No. 30). Example 6 C0.051%, Si3.25%, Mn0.085%, S0.021%,
A 2.0 mm thick hot-rolled plate obtained by performing known hot rolling on a continuously cast slab containing 0.005% Se and 0.026% Sb was washed with wet hydrogen at P H2O /P H2 = 0.20 after pickling. Hot-rolled plate annealing at 930°C for 2.5 minutes in an atmosphere (decarburization amount ΔC
= 0.008%), then intermediate cold rolled to a thickness of 0.70 mm, and then heated at 950°C in a wet hydrogen atmosphere with P H2O /P H2 = 0.20.
x Intermediate annealing for 2 minutes (decarburization amount ΔC = 0.009%), and cooling after the intermediate annealing is from 770℃ to 100℃
Immediately after cooling, the time required for
Aging treatment was performed at 225°C for 30 seconds, and the reduction rate was further reduced.
It was finished with a final cold rolling of 67% to a thickness of 0.23mm. After that, decarburization annealing was performed at 830°C for 3 minutes in a wet hydrogen atmosphere, and after applying MgO slurry, the final annealing was performed at 850°C for 55 hours and then at 1200°C for 10 minutes.
A unidirectional silicon steel sheet product (sample No. 33) according to an example of the present invention was obtained by subjecting it to purification annealing for a period of time and then applying an insulating coating. For comparison, a hot-rolled sheet with the same composition and thickness as the above-mentioned inventive example was annealed at 930°C for 2.5 minutes (decarburization amount ΔC = 0.002%), and then pickled and
After intermediate rolling to a thickness of mm, intermediate annealing was performed at 950°C for 2 minutes (decarburization amount ΔC = 0.002%), and cooling after the intermediate annealing was performed for 67 seconds between 770°C and 100°C. , the statute of limitations was not applied. Further, after final cold rolling with a rolling reduction of 67% to a thickness of 0.23 mm, decarburization annealing, application of MgO slurry, final annealing, and insulating coating were performed in the same manner as in the example of the present invention. Table 6 shows the results of measuring the magnetic properties of these products.
【表】
第6表から明らかなように、この発明の方法に
より得られた本発明例の製品(試料No.33)は、比
較例による製品(試料No.32)と比較して優れた磁
気特性を有している。
以上の説明で明らかなようにこの発明の製造方
法によれば、素材のC量をSi量に応じて適切な範
囲に調整しかつ熱延後最終冷延前までの脱炭量を
適切な範囲とししかも最終冷延前の鋼板の結晶粒
内炭化物を適切に制御することによつて、従来得
られなかつた著しい高磁束密度、著しい低鉄損値
の極めて優れた磁気特性を有する一方向性珪素鋼
板を安定して得ることが可能となり、また工程的
にも特殊な高温での除冷や長時間の時効処理を要
さずに極めて優れた特性の一方向性珪素鋼板が得
られるから、工業的規模での実施においても生産
性が高く経済的となる等、各種の効果が得られ
る。[Table] As is clear from Table 6, the product of the example of the present invention (sample No. 33) obtained by the method of the invention has superior magnetic properties compared to the product of the comparative example (sample No. 32). It has characteristics. As is clear from the above explanation, according to the manufacturing method of the present invention, the amount of C in the material is adjusted to an appropriate range according to the amount of Si, and the amount of decarburization after hot rolling and before final cold rolling is adjusted to an appropriate range. Moreover, by appropriately controlling the carbides in the grains of the steel sheet before final cold rolling, unidirectional silicon has extremely excellent magnetic properties such as a significantly high magnetic flux density and a significantly low iron loss value that were previously unobtainable. It is possible to stably obtain steel sheets, and unidirectional silicon steel sheets with extremely excellent properties can be obtained without requiring slow cooling at a special high temperature or long-term aging treatment, making it suitable for industrial use. Even when implemented on a large scale, various effects such as high productivity and economy can be obtained.
第1図は素材に含まれるSi量およびC量が製品
の鉄損値に及ぼす影響を示すグラフ、第2図は熱
延後最終冷延前までの脱炭量ΔCが製品の磁気特
性に及ぼす影響を示すグラフ、第3図は中間焼鈍
における脱炭量および中間焼鈍後急冷して200℃
時効処理した時の時効処理時間と磁気特性および
炭化物析出サイズとの関係を示すグラフ、第4図
は最終冷延前の鋼板の炭化物析出状態を示すため
の倍率1万倍の電子顕微鏡写真で、Aはこの発明
にしたがつて中間焼鈍後急冷および時効処理した
場合、Bは従来法にしたがつて中間焼鈍後標準冷
却した場合についてそれぞれ示すもの、第5図は
脱炭焼鈍後の鋼板表層部のゴス方位強度を、中間
焼鈍工程における脱炭の有無および中間焼鈍後の
急冷−時効処理の有無に応じて比較したグラフ、
第6図は最終冷延前の中間焼鈍後急冷しさらに時
効処理した場合の時効処理条件と炭化物析出サイ
ズとの関係を示すグラフ、第7図は最終冷延前の
中間焼鈍後の冷却過程において770〜300℃間は急
冷し300〜150℃間の冷却所要時間を変化させた場
合の300〜150℃間における冷却所要時間と炭化物
析出サイズおよび磁気特性との関係を示すグラフ
である。
Figure 1 is a graph showing the influence of the amount of Si and C contained in the material on the iron loss value of the product, and Figure 2 is a graph showing the effect of the amount of decarburization ΔC after hot rolling before final cold rolling on the magnetic properties of the product. A graph showing the influence, Figure 3 shows the amount of decarburization during intermediate annealing and the amount of decarburization at 200℃ after intermediate annealing.
A graph showing the relationship between aging treatment time, magnetic properties, and carbide precipitation size during aging treatment. Figure 4 is an electron micrograph at a magnification of 10,000 times showing the carbide precipitation state of the steel sheet before final cold rolling. A shows the case where intermediate annealing is followed by rapid cooling and aging treatment according to the present invention, B shows the case where intermediate annealing is followed by standard cooling according to the conventional method, and Figure 5 shows the surface layer of the steel sheet after decarburization annealing. A graph comparing the Goss orientation strength of according to the presence or absence of decarburization in the intermediate annealing process and the presence or absence of rapid cooling-aging treatment after intermediate annealing,
Figure 6 is a graph showing the relationship between aging treatment conditions and carbide precipitation size when the intermediate annealing before the final cold rolling is followed by rapid cooling and further aging treatment. This is a graph showing the relationship between the required cooling time between 300 and 150°C, the carbide precipitation size, and the magnetic properties when the cooling time between 770 and 300°C is rapidly cooled and the required cooling time between 300 and 150°C is varied.
Claims (1)
〜4.0%、Mn0.02〜0.15%を含み、かつS、Seの
いずれか1種または2種とSbとを合計量で0.008
〜0.080%含有し、残部が実質的にFeよりなる珪
素鋼素材を熱間圧延し、得られた熱延鋼板に対し
中間焼鈍を挟む2回以上の冷間圧延を最終冷延圧
下率40〜80%の範囲内で施して所定の板厚に仕上
げ、さらにその冷延板に脱炭焼鈍および最終焼鈍
を施す一連の一方向性珪素鋼板の製造方法におい
て、 前記珪素鋼素材中に含まれるC量をSi量に応じ
て次の式 0.37[Si%]+0.27≦log([C%]×103) ≦0.37[Si%]+0.57 によつて表わされる範囲内とし、かつ熱間圧延終
了後、最終冷延終了前までの間にCを0.006〜
0.020%脱炭させ、かつまた最終冷延前の中間焼
鈍後の冷却過程において、770〜100℃の間の冷却
所要時間が30秒以内となるように中間焼鈍後に鋼
板を急冷し、直ちに150〜250℃の温度範囲内にお
いて2〜60秒間の時効処理を施した後、最終冷延
を施すことを特徴とする磁気特性の優れた一方向
性珪素鋼板の製造方法。 2 C0.015〜0.10%(重量%、以下同じ)、Si2.8
〜4.0%、Mn0.02〜0.15%を含み、かつS、Seの
いずれか1種または2種とSbとを合計量で0.008
〜0.080%含有し、残部が実質的にFeよりなる珪
素鋼素材を熱間圧延し、得られた熱延鋼板に対し
中間焼鈍を挟む2回以上の冷間圧延を最終冷延圧
下率40〜80%の範囲内で施して所定の板厚に仕上
げ、さらにその冷延板に脱炭焼鈍および最終焼鈍
を施す一連の一方向性珪素鋼板の製造方法におい
て、 前記珪素鋼素材中に含まれるC量をSi量に応じ
て次の式 0.37[Si%]+0.27≦log([C%]×103) ≦0.37[Si%]+0.57 によつて表わされる範囲内とし、かつ熱間圧延終
了後、最終冷延終了前までの間にCを0.006〜
0.020%脱炭させ、かつまた最終冷延前の中間焼
鈍後の冷却過程において770〜300℃の間の冷却所
要時間を20秒以内に制御しかつそれに続く300〜
150℃の間の冷却所要時間を8〜30秒の範囲内に
制御して冷却した後、最終冷延を施すことを特徴
とする磁気特性の優れた一方向性珪素鋼板の製造
方法。[Claims] 1 C0.015 to 0.10% (weight%, same hereinafter), Si2.8
~4.0%, Mn0.02~0.15%, and one or both of S and Se and Sb in a total amount of 0.008
A silicon steel material containing ~0.080% Fe with the remainder being substantially Fe is hot rolled, and the resulting hot rolled steel sheet is cold rolled two or more times with intermediate annealing in between to achieve a final cold rolling reduction of 40~ In a series of methods for manufacturing unidirectional silicon steel sheets, the C contained in the silicon steel material is applied within a range of 80% to finish the sheet to a predetermined thickness, and the cold rolled sheet is then subjected to decarburization annealing and final annealing. The amount is determined according to the amount of Si within the range expressed by the following formula: 0.37 [Si%] + 0.27 ≦ log ([C%] × 10 3 ) ≦ 0.37 [Si%] + 0.57, and hot After the end of rolling and before the end of final cold rolling, increase C from 0.006 to
0.020% decarburization, and in the cooling process after intermediate annealing before final cold rolling, the steel plate is rapidly cooled after intermediate annealing so that the cooling time from 770 to 100℃ is within 30 seconds, and immediately after intermediate annealing to 150 to 100℃. A method for producing a unidirectional silicon steel sheet with excellent magnetic properties, which comprises subjecting the steel sheet to an aging treatment for 2 to 60 seconds within a temperature range of 250°C, and then subjecting it to final cold rolling. 2 C0.015-0.10% (weight%, same below), Si2.8
~4.0%, Mn0.02~0.15%, and one or both of S and Se and Sb in a total amount of 0.008
A silicon steel material containing ~0.080% Fe with the remainder being substantially Fe is hot rolled, and the resulting hot rolled steel sheet is cold rolled two or more times with intermediate annealing in between to achieve a final cold rolling reduction of 40~ In a series of methods for manufacturing unidirectional silicon steel sheets, the C contained in the silicon steel material is applied within a range of 80% to finish the sheet to a predetermined thickness, and the cold rolled sheet is then subjected to decarburization annealing and final annealing. The amount is determined according to the amount of Si within the range expressed by the following formula: 0.37 [Si%] + 0.27 ≦ log ([C%] × 10 3 ) ≦ 0.37 [Si%] + 0.57, and hot After the end of rolling and before the end of final cold rolling, increase C from 0.006 to
0.020% decarburization, and in the cooling process after intermediate annealing before final cold rolling, the cooling time between 770 and 300°C is controlled within 20 seconds, and the subsequent 300 to 300°C
1. A method for producing a unidirectional silicon steel sheet with excellent magnetic properties, which comprises cooling at 150° C. by controlling the cooling time within a range of 8 to 30 seconds, and then performing final cold rolling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17782082A JPS5967316A (en) | 1982-10-09 | 1982-10-09 | Production of unidirectional silicon steel plate having excellent magnetic characteristic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17782082A JPS5967316A (en) | 1982-10-09 | 1982-10-09 | Production of unidirectional silicon steel plate having excellent magnetic characteristic |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62-294637A Division JPH066748B2 (en) | 1982-10-09 | Manufacturing method for grain-oriented silicon steel sheet with excellent magnetic properties |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5967316A JPS5967316A (en) | 1984-04-17 |
| JPH0338323B2 true JPH0338323B2 (en) | 1991-06-10 |
Family
ID=16037667
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17782082A Granted JPS5967316A (en) | 1982-10-09 | 1982-10-09 | Production of unidirectional silicon steel plate having excellent magnetic characteristic |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5967316A (en) |
-
1982
- 1982-10-09 JP JP17782082A patent/JPS5967316A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5967316A (en) | 1984-04-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0089195B1 (en) | Method of producing grain-oriented silicon steel sheets having excellent magnetic properties | |
| CN113166836A (en) | Oriented electrical steel sheet and method for manufacturing the same | |
| JPWO2019131853A1 (en) | Low iron loss grain-oriented electrical steel sheet and its manufacturing method | |
| JP3392664B2 (en) | Manufacturing method of grain-oriented electrical steel sheet with extremely low iron loss | |
| JP3392579B2 (en) | Manufacturing method of grain-oriented electrical steel sheet with extremely low iron loss | |
| KR930011405B1 (en) | Method of manufacturing an oriented silicon steel sheet having improved magnetic flux density | |
| JP3928275B2 (en) | Electrical steel sheet | |
| JP3474741B2 (en) | Manufacturing method of grain-oriented electrical steel sheet with excellent magnetic properties | |
| KR970007031B1 (en) | Method for manufacturing orient electrical steel sheet having excellent magnetic properties | |
| JPH0338323B2 (en) | ||
| JP2819994B2 (en) | Manufacturing method of electrical steel sheet with excellent magnetic properties | |
| JPS6242968B2 (en) | ||
| KR100240989B1 (en) | Manufacturing method of high magnetic flux density oriented electrical steel sheet | |
| KR101263843B1 (en) | Grain-oriented electrical steel sheets with extremely low core-loss and high flux-density and Method for manufacturing the same | |
| KR101318275B1 (en) | Method for manufacturing grain-oriented electrical steel sheets with extremely low core-loss and high flux-density | |
| KR100360096B1 (en) | The method of manufacturing grain oriented silicon steel by low heating | |
| JPH01201425A (en) | Manufacture of grain-oriented silicon steel sheet excellent in magnetic property | |
| JPH066748B2 (en) | Manufacturing method for grain-oriented silicon steel sheet with excellent magnetic properties | |
| KR970007162B1 (en) | Method for manufacturing oriented electrical steel sheet of low temperature slab heating method with excellent iron loss characteristics | |
| JPH10183249A (en) | Manufacturing method of grain-oriented electrical steel sheet with excellent magnetic properties | |
| JPH04362138A (en) | Manufacture of grain-oriented thick electrical steel sheet excellent in magnetic property | |
| KR101263847B1 (en) | Grain-oriented electrical steel sheets with extremely low core-loss and high flux-density and method for manufacturing the same | |
| JPH029089B2 (en) | ||
| JPH06136446A (en) | Manufacturing method of grain-oriented electrical steel sheet with excellent iron loss without glass coating | |
| JPH10158740A (en) | Manufacturing method of grain-oriented electrical steel sheet with excellent magnetic properties |