JPH06220590A - High silicon steel sheet excellent in workability - Google Patents

High silicon steel sheet excellent in workability

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Publication number
JPH06220590A
JPH06220590A JP5028562A JP2856293A JPH06220590A JP H06220590 A JPH06220590 A JP H06220590A JP 5028562 A JP5028562 A JP 5028562A JP 2856293 A JP2856293 A JP 2856293A JP H06220590 A JPH06220590 A JP H06220590A
Authority
JP
Japan
Prior art keywords
less
concentration
grain boundary
crystal grain
steel sheet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP5028562A
Other languages
Japanese (ja)
Other versions
JP2956406B2 (en
Inventor
Yasushi Tanaka
靖 田中
Tatsuhiko Hiratani
多津彦 平谷
Masahiro Abe
正広 阿部
Katsuji Kasai
勝司 笠井
Kazuhisa Okada
和久 岡田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Engineering Corp
Original Assignee
NKK Corp
Nippon Kokan Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NKK Corp, Nippon Kokan Ltd filed Critical NKK Corp
Priority to JP5028562A priority Critical patent/JP2956406B2/en
Priority to DE69312233T priority patent/DE69312233T2/en
Priority to EP93119720A priority patent/EP0601549B1/en
Priority to KR1019930026779A priority patent/KR960006447B1/en
Priority to CN93120804A priority patent/CN1035889C/en
Publication of JPH06220590A publication Critical patent/JPH06220590A/en
Application granted granted Critical
Publication of JP2956406B2 publication Critical patent/JP2956406B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PURPOSE:To provide an inexpensive high silicon steel sheet excellent in workability. CONSTITUTION:This high silicon steel sheet has a composition containing, by weight, 4-10% Si, containing, preferably, <=0.01% C, <=0.5% Mn, <=0.01% P, <=0.01% S, <=0.2% Sol.Al, <=0.01% N, and <=0.02% O, and having the balance Fe with inevitable impurities or a composition containing 4-10% (Si+Al) and preferably containing the C, Mn, P, S, N, and O by the above quantities, respectively. In this steel sheet, O concentration in the elements segregating in crystalline grain boundaries is <=30at% and S concentration in the elements segregating in crystalline grain boundaries is <=0.2at%, and further preferably, sheet thickness is <=0.5mm and average grain size viewed from sheet surface is <=2.0mm.

Description

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

【0001】[0001]

【産業上の利用分野】この発明は、トランスやモータの
鉄心材料等に使用される高珪素電磁鋼板に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high silicon electromagnetic steel sheet used as a core material for transformers and motors.

【従来の技術】モータやトランスの鉄心材料として広く
用いられている電磁鋼板には、通常、集合組織制御およ
び固有抵抗増大のために珪素が添加される。珪素が6.
5wt%含まれる鉄合金は、磁歪がほぼ零になるために
最も優れた軟磁性を示すが、珪素の添加量が多くなると
材料が脆くなるため、珪素を4wt%以上含む高珪素鋼
は通常の圧延法により薄鋼板とすることは不可能であ
る。これに対し、近年高珪素薄鋼板を得る方法として、
溶融状態から直接薄板に鋳造する融体急冷法(例えば、
特公昭60−32705号)、特殊な圧延法を適用する
方法(例えば、特公平3−80846号)、圧延により
得られた低Siの鋼板にSiを富化する所謂浸珪法(例
えば、特公平2−60041号)等が提案され、特に浸
珪法は工業的に実用化されている。
2. Description of the Related Art Silicon is generally added to magnetic steel sheets, which are widely used as a core material for motors and transformers, in order to control texture and increase specific resistance. Silicon is 6.
The iron alloy containing 5 wt% exhibits the most excellent soft magnetism because the magnetostriction becomes almost zero, but the material becomes brittle when the added amount of silicon becomes large. Therefore, high-silicon steel containing 4 wt% or more of silicon is usually used. It is impossible to make a thin steel sheet by the rolling method. On the other hand, in recent years, as a method for obtaining a high-silicon thin steel sheet,
A melt quenching method that directly casts a thin plate from the molten state (for example,
Japanese Patent Publication No. 60-32705), a method of applying a special rolling method (for example, Japanese Patent Publication No. 3-80846), a so-called siliconizing method for enriching Si in a low-Si steel plate obtained by rolling (for example, Proposal No. 2-60041) and the like have been proposed, and especially the siliconizing method has been industrially put to practical use.

【0002】ところで、上記のような方法で製造される
高珪素鋼板を、実際にモータやトランスに使用するため
には、鋼板に打ち抜き、剪断、曲げといった加工を加え
る必要がある。しかし、高珪素鋼板は脆性であるため打
ち抜きや剪断端面で割れや欠損を生じたり、曲げ加工で
割れを生じやすいという問題がある。このような高珪素
鋼板の加工改善を目的として、従来いくつかの提案がな
されている。
By the way, in order to actually use the high silicon steel sheet manufactured by the above-mentioned method for a motor or a transformer, it is necessary to add punching, shearing or bending to the steel sheet. However, since the high silicon steel plate is brittle, there is a problem that cracks and defects occur at punching and shearing end faces, and cracks easily occur during bending. Several proposals have hitherto been made for the purpose of improving the processing of such a high silicon steel sheet.

【0003】例えば、特公昭61−15136号では、
結晶粒径が1〜100μmで且つ結晶粒が薄板表面に対
し垂直に成長した柱状晶からなり、規則格子が実質的に
存在しないことで加工性と磁気特性の優れた高珪素鋼帯
が得られるとしている。また、特開昭62−27072
3号では、圧延組織の状態で製品形状に加工成形し、そ
の後焼鈍することにより実質的に加工性の良好な高珪素
鋼板を製造できるとしている。さらに、特開平4−16
5050号では、Mnを固溶Sの悪影響を抑えるために
添加し、結晶粒の方位集積度を高めることにより加工性
の優れた高珪素方向性珪素鋼板を製造できるとしてい
る。
For example, in Japanese Patent Publication No. 61-15136,
A high silicon steel strip excellent in workability and magnetic properties can be obtained because the crystal grain size is 1 to 100 μm and the crystal grains are columnar crystals grown perpendicularly to the surface of the thin plate, and the ordered lattice is substantially absent. I am trying. Also, JP-A-62-27072
In No. 3, it is stated that a high silicon steel sheet having substantially good workability can be manufactured by forming the product into a product shape in the rolled structure and then annealing. Furthermore, JP-A-4-16
According to No. 5050, Mn is added to suppress the adverse effect of solid solution S and the orientation integration degree of crystal grains is increased to produce a highly silicon-oriented silicon steel sheet having excellent workability.

【0004】[0004]

【発明が解決しようとする課題】しかし、これらの提案
のうち特公昭61−15136号は、結晶粒径が100
μm以上ではその効果が得られず、しかも、高珪素鋼で
は規則相が実質的に存在しないようにするためには90
0℃以上から水焼き入れ等の急冷を施す必要があること
から、製造工程上困難を伴う技術である。また、特開昭
62−270723号の方法では、加工時に圧延組織を
有しているために加工後に高温の焼鈍が必要であり、現
状のトランス、モータの製造工程から考えると工程が一
つ追加されることになるため経済上好ましくない。ま
た、特開平4−165050号では方位集積が高いこと
が必要であるが、高い集積度を得ることはインヒビタを
用いた二次再結晶の安定性からみて困難であり、また、
この技術は無方向性珪素鋼板には適用できない欠点があ
る。
However, among these proposals, Japanese Patent Publication No. 61-15136 discloses a crystal grain size of 100.
If the thickness is more than μm, the effect cannot be obtained, and in order to make the ordered phase substantially absent in high silicon steel, 90
Since it is necessary to perform quenching such as water quenching from 0 ° C. or higher, this is a technique with difficulty in the manufacturing process. Further, in the method disclosed in Japanese Patent Laid-Open No. 62-270723, high temperature annealing is required after working because it has a rolling structure during working, and one process is added considering the current manufacturing process of transformers and motors. Therefore, it is not economically preferable. Further, in Japanese Unexamined Patent Publication No. 4-165050, it is necessary to have a high orientation integration, but it is difficult to obtain a high integration degree in view of the stability of secondary recrystallization using an inhibitor, and
This technique has a drawback that it cannot be applied to non-oriented silicon steel sheets.

【0005】本発明はこのような従来技術の問題点に鑑
みなされたもので、打ち抜き、剪断、曲げ等の工程にお
いて必要とされる高珪素電磁鋼板の加工性を、材料面か
ら経済性を考慮して改善しようとするものであり、安価
でしかも加工性に優れた、すなわち、打ち抜きや剪断端
面における割れや欠損が少なく、或いは曲げ加工におい
て曲げ可能半径を小さくできる高珪素電磁鋼板を提供し
ようとするものである。
The present invention has been made in view of the above problems of the prior art, and considers the workability of the high-silicon electrical steel sheet required in the steps of punching, shearing, bending, etc. from the viewpoint of the material and the economical efficiency. It is an object of the present invention to provide a high-silicon electrical steel sheet that is inexpensive and has excellent workability, that is, has few cracks and defects in punching and shearing end faces, or can have a small bendable radius in bending. To do.

【0006】[0006]

【課題を解決するための手段】高珪素鋼板は珪素量が多
く母相が本来的に脆いため、従来、加工性の改善はほと
んど不可能であると考えられてきた。本発明者らは高珪
素鋼板の加工性向上を目指して種々の実験研究を行って
きたが、最終の熱処理雰囲気中の露点および酸素濃度を
変化させた種々の高珪素鋼板の加工性を調査するうち
に、同じ珪素量でありながら加工性が他の鋼板に較べて
比較的良好なものが存在することを発見した。図1にそ
の際の試験結果を示す。この試験では、焼鈍雰囲気中の
露点、酸素濃度を変えるために真空度を変化させた。同
図の横軸にはこの真空度を、また、縦軸には加工性の指
標として三点曲げ試験(図2に示す方法で試料を押し込
み、割れずに押し込めるストローク距離を測定する試
験)において試片が破壊するまでの押し込み量を示して
いる。焼鈍は各真空度の下で1200℃×15分の条件
で行った。この試験結果から、真空度が良くなればなる
ほど加工性は良好になることが判った。
High silicon steel sheets have a large amount of silicon and the mother phase is inherently brittle, and it has heretofore been thought that improvement in workability is almost impossible. The present inventors have conducted various experimental studies with the aim of improving the workability of high silicon steel sheets, and investigate the workability of various high silicon steel sheets with varying dew point and oxygen concentration in the final heat treatment atmosphere. Among them, it was discovered that there is a steel having the same silicon content but relatively good workability as compared with other steel sheets. FIG. 1 shows the test result in that case. In this test, the degree of vacuum was changed to change the dew point and oxygen concentration in the annealing atmosphere. In the figure, the horizontal axis represents this degree of vacuum, and the vertical axis represents the workability index in a three-point bending test (a test in which the sample is pushed in by the method shown in FIG. 2 and the stroke distance at which the sample can be pushed in without cracking is measured). The amount of pushing until the specimen breaks is shown. Annealing was performed under the conditions of 1200 ° C. for 15 minutes under each vacuum degree. From this test result, it was found that the better the degree of vacuum, the better the workability.

【0007】これらの試料をもとに高珪素鋼の破壊のメ
カニズムを詳細に検討したところ、破面の形態が加工性
と強い相関があること、具体的には、加工性の劣ったも
のは結晶粒の粒界破面が多く現れ、一方、加工性の優れ
たものは劈開破面が多く現れるという事実が判明した。
さらに、加工性の優れた試料と劣った試料について粒界
破面の偏析元素濃度をオージェ電子分光で調査したとこ
ろ、加工性の優れた試料は総じて結晶粒界での酸素濃度
が低く、結晶粒界での酸素濃度が高い試料は加工性に劣
ることが明らかとなった。
A detailed study of the fracture mechanism of high silicon steel based on these samples revealed that the morphology of the fracture surface had a strong correlation with the workability, and specifically, those with poor workability were found. It was revealed that many grain boundary fracture surfaces of crystal grains appeared, while those of excellent workability showed many cleavage fracture surfaces.
In addition, when the segregation element concentration of the grain boundary fracture surface was investigated by Auger electron spectroscopy between the samples with excellent workability and the sample with inferior workability, the samples with excellent workability generally have a low oxygen concentration at the crystal grain boundaries and It was revealed that the sample with high oxygen concentration in the interface was inferior in workability.

【0008】本発明者らは、さらに粒界を詳細に調査す
ることにより粒界酸素濃度以外に加工性と相関する因子
を明かにすることを試みた。すなわち、粒界酸素濃度が
一定であるような試料群について種々の粒界偏析元素の
加工性に対する影響を調査した。その結果、粒界におけ
る硫黄が酸素の効果とは独立に加工性に重大な影響を及
ぼしていることが判明した。図3は、Si:6.49w
t%、Mn:0.005wt%、S:0.0015wt
%、O:0.0022wt%の成分組成を有する板厚
0.35mmの試料について、0.1vol%H2Sを
含むN2雰囲気中で熱処理を施し、熱処理後の試料の三
点曲げ性(上述した三点曲げ試験での押し込み量)と、
オージェ電子分光装置により粒界において検出された硫
黄濃度との関係を示したものである。なお、上記熱処理
を施した後の試料中のトータルの硫黄量は分析誤差内で
ほぼ一定であった。また、オージェ電子分光装置により
測定した粒界での酸素濃度はいずれも3〜5at%の範
囲であった。図3によれば、加工性は結晶粒界の硫黄濃
度と強い相関をもっており、結晶粒界の硫黄が加工性を
劣化させていることが推測できる。このように粒界硫黄
濃度と加工性とが強い相関を有することの詳細なメカニ
ズムは不明であるが、粒界にMn等の硫化物形成元素が
含まれていないことから、硫黄はおそらく固溶した状態
で粒界に存在しているもの考えられる。
The present inventors have tried to clarify factors other than the grain boundary oxygen concentration, which are correlated with the workability, by further examining the grain boundaries in detail. That is, the influence of various grain boundary segregation elements on the workability was investigated for a sample group in which the grain boundary oxygen concentration was constant. As a result, it was found that sulfur at the grain boundaries had a significant effect on workability, independent of the effect of oxygen. FIG. 3 shows Si: 6.49w
t%, Mn: 0.005 wt%, S: 0.0015 wt
%, O: 0.0022 wt% of a sample having a plate thickness of 0.35 mm was heat-treated in an N 2 atmosphere containing 0.1 vol% H 2 S, and the three-point bendability of the sample after heat treatment ( Indentation amount in the above three-point bending test),
It shows the relationship with the sulfur concentration detected at grain boundaries by Auger electron spectroscopy. The total amount of sulfur in the sample after the heat treatment was almost constant within the analytical error. Further, the oxygen concentration at the grain boundaries measured by Auger electron spectroscopy was in the range of 3 to 5 at%. According to FIG. 3, the workability has a strong correlation with the sulfur concentration in the crystal grain boundaries, and it can be inferred that the sulfur in the crystal grain boundaries deteriorates the workability. The detailed mechanism of the strong correlation between the grain boundary sulfur concentration and the workability is unknown, but since the sulfide forming element such as Mn is not contained in the grain boundary, sulfur is probably a solid solution. It is considered that they exist in the grain boundary in the state of being formed.

【0009】また、焼鈍温度を変化させることにより結
晶粒径をコントロールすることは容易であるが、上記試
験においても焼鈍温度を変化させると加工性も大きく変
化することが判った。このように本発明者らは、従来加
工性が基本的に劣ると考えられてきた高珪素鋼板の加工
性が、実は粒界の性質と極めて大きな相関を有してお
り、これを制御することにより加工性に優れた高珪素鋼
板が得られることを見出した。
Further, although it is easy to control the crystal grain size by changing the annealing temperature, it was found in the above-mentioned test that the workability also greatly changes when the annealing temperature is changed. As described above, the present inventors have found that the workability of a high-silicon steel sheet, which has been conventionally considered to be basically inferior in workability, has an extremely large correlation with the properties of grain boundaries, and it is necessary to control this. It was found that a high silicon steel sheet excellent in workability can be obtained by the above.

【0010】本発明はかかる知見に基づきなされたもの
で、以下のような構成を有する。 (1) Si:4〜10wt%を含有し、結晶粒界にお
けるO濃度(結晶粒界に偏析する元素中のO濃度)が3
0at%以下、結晶粒界におけるS濃度(結晶粒界に偏
析する元素中のS濃度)が0.2at%以下である加工
性の優れた高珪素電磁鋼板。 (2) C:0.01wt%以下、Si:4〜10wt
%、Mn:0.5wt%以下、P:0.01wt%以
下、S:0.01wt%以下、Sol.Al:0.2w
t%以下、N:0.01wt%以下、O:0.02wt
%以下、残部Feおよび不可避不純物からなり、結晶粒
界におけるO濃度(結晶粒界に偏析する元素中のO濃
度)が30at%以下、結晶粒界におけるS濃度(結晶
粒界に偏析する元素中のS濃度)が0.2at%以下で
ある加工性の優れた高珪素電磁鋼板。 (3) Si+Al:4〜10wt%を含有し、結晶粒
界におけるO濃度(結晶粒界に偏析する元素中のO濃
度)が30at%以下、結晶粒界におけるS濃度(結晶
粒界に偏析する元素中のS濃度)が0.2at%以下で
ある加工性の優れた高珪素電磁鋼板。 (4) C:0.01wt%以下、Si+Al:4〜1
0wt%、Mn:0.5wt%以下、P:0.01wt
%以下、S:0.01wt%以下、N:0.01wt%
以下、O:0.02wt%以下、残部Feおよび不可避
不純物からなり、結晶粒界におけるO濃度(結晶粒界に
偏析する元素中のO濃度)が30at%以下、結晶粒界
におけるS濃度(結晶粒界に偏析する元素中のS濃度)
が0.2at%以下である加工性の優れた高珪素電磁鋼
板。 (5) 上記(1)〜(4)の鋼板において、板厚が
0.5mm以下、板面から見た平均結晶粒径が2.0m
m以下である加工性の優れた高珪素電磁鋼板。
The present invention has been made on the basis of such findings and has the following constitution. (1) Si: 4 to 10 wt% is contained, and the O concentration in the grain boundaries (O concentration in the elements segregated in the grain boundaries) is 3
A high silicon magnetic steel sheet having an excellent workability of 0 at% or less and an S concentration at a crystal grain boundary (S concentration in an element segregated at the crystal grain boundary) of 0.2 at% or less. (2) C: 0.01 wt% or less, Si: 4 to 10 wt
%, Mn: 0.5 wt% or less, P: 0.01 wt% or less, S: 0.01 wt% or less, Sol. Al: 0.2w
t% or less, N: 0.01 wt% or less, O: 0.02 wt
% Or less, the balance consists of Fe and unavoidable impurities, and the O concentration in the crystal grain boundaries (O concentration in the elements segregated in the crystal grain boundaries) is 30 at% or less, the S concentration in the crystal grain boundaries (in the elements segregated in the crystal grain boundaries). S silicon concentration) is 0.2 at% or less, and is a high-silicon electrical steel sheet with excellent workability. (3) Si + Al: 4 to 10 wt% is contained, the O concentration in the crystal grain boundary (O concentration in the element segregated in the crystal grain boundary) is 30 at% or less, and the S concentration in the crystal grain boundary (segregated in the crystal grain boundary). A high silicon electrical steel sheet having an excellent workability and having an S concentration in the element) of 0.2 at% or less. (4) C: 0.01 wt% or less, Si + Al: 4-1
0 wt%, Mn: 0.5 wt% or less, P: 0.01 wt
% Or less, S: 0.01 wt% or less, N: 0.01 wt%
Hereinafter, O: 0.02 wt% or less, consisting of balance Fe and unavoidable impurities, O concentration in the crystal grain boundary (O concentration in the element segregated to the crystal grain boundary) is 30 at% or less, S concentration in the crystal grain boundary (crystal (S concentration in elements segregated at grain boundaries)
Of 0.2 at% or less is a high-silicon electrical steel sheet with excellent workability. (5) In the steel plates of (1) to (4) above, the plate thickness is 0.5 mm or less, and the average crystal grain size viewed from the plate surface is 2.0 m.
A high-silicon electrical steel sheet with an excellent workability of m or less.

【0011】[0011]

【作用】以下、本発明の詳細をその限定理由とともに説
明する。Siは、添加量が略6.5wt%で磁歪が零と
なり最も優れた軟磁性を示す。Siが4wt%未満では
高珪素鋼板としての所望の磁気特性が得られず、また、
鋼板の加工性も特に問題とならない。一方、Siが10
wt%を超えると飽和磁束密度が著しく減少する。この
ため、Siは4〜10wt%とする。また、Siはその
一部をAlで置換することも可能であり、この場合には
Si+Al量を規定する必要がある。Si+Alが4w
t%未満では本発明が目的とする磁気特性が得られず、
また、鋼板の加工性は特に問題とならない。一方、Si
+Alが10wt%を超えると飽和磁束密度の著しく減
少する。このため、Siの一部をAlで置換する場合に
は、Si+Al:4〜10wt%とする。
The details of the present invention will be described below together with the reasons for limitation. When Si is added in an amount of approximately 6.5 wt%, the magnetostriction becomes zero and the most excellent soft magnetism is exhibited. If Si is less than 4 wt%, the desired magnetic properties as a high silicon steel sheet cannot be obtained, and
The workability of the steel sheet is also not a particular problem. On the other hand, Si is 10
When it exceeds wt%, the saturation magnetic flux density is significantly reduced. Therefore, Si is 4 to 10 wt%. It is also possible to replace a part of Si with Al, and in this case, it is necessary to regulate the amount of Si + Al. Si + Al is 4w
If it is less than t%, the magnetic properties aimed by the present invention cannot be obtained,
Further, the workability of the steel sheet is not a particular problem. On the other hand, Si
When + Al exceeds 10 wt%, the saturation magnetic flux density is significantly reduced. Therefore, when a part of Si is replaced with Al, Si + Al: 4 to 10 wt%.

【0012】Cは軟磁性に有害な元素であり、また、C
が0.01wt%超えると経時的に軟磁性が劣化する所
謂時効劣化現象が生じる。このためCは0.01wt%
以下とすることが好ましい。MnはSと結合してMnS
となり、スラブ段階での熱間加工性を改善する作用があ
る。しかし、Mnが0.5wt%を超えると飽和磁束密
度の減少が大きくなるため適当でない。このためMnは
0.5wt%以下とすることが好ましい。
C is an element harmful to soft magnetism, and C
If it exceeds 0.01 wt%, a so-called aging deterioration phenomenon occurs in which the soft magnetism deteriorates with time. Therefore, C is 0.01 wt%
The following is preferable. Mn combines with S to MnS
And has the effect of improving hot workability in the slab stage. However, when Mn exceeds 0.5 wt%, the saturation magnetic flux density is greatly reduced, which is not suitable. Therefore, Mn is preferably 0.5 wt% or less.

【0013】Pは軟磁気特性を劣化させる元素であり、
その含有量はできるだけ低いほうが好ましい。経済性お
よびPが0.01wt%以下であれば実質的にその悪影
響は無視できることから、Pは0.01wt%以下とす
ることが好ましい。Sは熱間圧延時の脆性を増大させる
元素であるとともに、軟磁気特性も劣化させるため、そ
の含有量はできるだけ低いほうが好ましい。後述するよ
うに本発明において最も重要な要件は粒界における硫黄
濃度であるが、ここで述べる硫黄量は粒界および粒内を
含む全体の硫黄量である。経済性およびSが0.01w
t%以下であれば実質的にその悪影響は無視できること
から、Sは0.01wt%以下とすることが好ましい。
P is an element that deteriorates the soft magnetic characteristics,
The content is preferably as low as possible. Since P is 0.01 wt% or less and the adverse effect thereof can be substantially ignored, P is preferably 0.01 wt% or less. Since S is an element that increases brittleness during hot rolling and also deteriorates soft magnetic properties, its content is preferably as low as possible. As will be described later, the most important requirement in the present invention is the sulfur concentration at the grain boundary, but the sulfur amount described here is the total sulfur amount including the grain boundary and the inside of the grain. Economy and S is 0.01w
If it is t% or less, the adverse effect can be substantially ignored, so S is preferably 0.01 wt% or less.

【0014】Alは脱酸により鋼を清浄化する作用を有
するとともに、磁気特性上も電気抵抗を高める作用を有
する。Siを4〜10wt%添加する鋼では、Siによ
り磁気特性の改善を図り、Alは鋼の脱酸作用のみを果
たせばよいことから、Sol.Alは0.2wt%以下
とすることが好ましい。一方、Siの一部をAlで置換
する場合には、上述したようにSi+Alを4〜10w
t%とする。Nは軟磁気特性を劣化させる元素であり、
時効による磁気特性の経時的変化も引き起こすため、そ
の含有量はできるだけ低いほうが好ましい。経済性およ
びNが0.01wt%以下であれば実質的にその悪影響
は無視できることから、Nは0.01wt%以下とする
ことが好ましい。
Al has a function of cleaning steel by deoxidation and also has a function of increasing electric resistance in terms of magnetic characteristics. In steel containing 4 to 10 wt% of Si, Si improves the magnetic properties, and Al only has to perform the deoxidizing action of steel. Al is preferably 0.2 wt% or less. On the other hand, when replacing a part of Si with Al, as described above, Si + Al is 4 to 10 w.
t%. N is an element that deteriorates the soft magnetic characteristics,
The content thereof is preferably as low as possible because it also causes a change in the magnetic properties over time due to aging. It is preferable to set N to 0.01 wt% or less because the economical efficiency and the adverse effect thereof can be substantially ignored if N is 0.01 wt% or less.

【0015】Oは軟磁気特性を劣化させる元素であり、
その含有量はできるだけ低いほうが好ましい。本発明で
は粒界における酸素濃度を規定しているが、ここでいう
O量は粒界および粒内を含む全体のO量である。後述す
るように本発明は、鋼板中に不可避的に含まれるOとS
の粒界での濃度を規制することにより優れた加工性を得
るものであるが、鋼板中のO量が増加すると、熱処理条
件に拘りなく酸素は粒内および粒界のいずれにも存在す
るようになり、粒界酸素濃度を30at%以下に制御す
ることが難しくなる。鋼板中のO量が0.02wt%以
下であれば、熱処理条件(例えば、熱処理雰囲気の真空
度)によって酸素の存在する箇所(粒内または粒界)を
選択的に制御することが比較的容易であり、このためO
は0.02wt%以下とすることが好ましい。一方、O
の下限に特別な限定はなく、また、O量を単純に低減さ
せても、粒界酸素濃度の低減化には結び付かない。但
し、Oを過度に低減することはコスト高を招くため、経
済性の観点からは0.0005wt%未満まで低減化さ
せることは得策ではない。以上の成分以外に、鋼中の不
可避不純物としてCr、Ni、Cu、Sn、Mo等が含
まれる場合があり、これらがそれぞれ0.03wt%程
度を限度に含まれても本発明の効果は損なわれない。
O is an element that deteriorates the soft magnetic characteristics,
The content is preferably as low as possible. In the present invention, the oxygen concentration at the grain boundary is defined, but the O amount here is the total O amount including the grain boundary and the inside of the grain. As will be described later, the present invention relates to O and S which are unavoidably contained in the steel sheet.
It is possible to obtain excellent workability by controlling the concentration at the grain boundary. However, if the amount of O in the steel sheet increases, oxygen appears to exist both inside the grain and at the grain boundary regardless of heat treatment conditions. Therefore, it becomes difficult to control the grain boundary oxygen concentration to 30 at% or less. When the amount of O in the steel sheet is 0.02 wt% or less, it is relatively easy to selectively control the location (intragrain or grain boundary) where oxygen is present depending on the heat treatment conditions (for example, vacuum degree of heat treatment atmosphere). And therefore O
Is preferably 0.02 wt% or less. On the other hand, O
There is no particular limitation on the lower limit of the above, and simple reduction of the O amount does not lead to reduction of the grain boundary oxygen concentration. However, excessive reduction of O leads to high cost, and therefore it is not a good idea to reduce O to less than 0.0005 wt% from the economical point of view. In addition to the above components, there are cases where Cr, Ni, Cu, Sn, Mo, etc. are contained as inevitable impurities in the steel, and the effect of the present invention is impaired even if each of them is contained up to about 0.03 wt%. I can't.

【0016】本発明の鋼板は結晶粒界の硫黄濃度(結晶
粒界に偏析した元素中の硫黄濃度)が0.2at%(at
omic %)以下であることが必要であり、これが本発明
における最も重要な要件である。ここで、結晶粒界の硫
黄量とは、粒界に偏析している元素中の硫黄含有量(a
t%)である。通常、この硫黄量の測定にはオージェ電
子分光装置が用いられる。この装置による測定では、真
空度1×(1/109)torr以下に保った真空容器
中において試料を破壊させ、大気に汚染されていない清
浄な粒界破面を観察しながらオージェ電子を分光するも
のであり、これにより清浄な粒界破面における元素の分
析が可能である。
In the steel sheet of the present invention, the sulfur concentration at the grain boundaries (sulfur concentration in the elements segregated at the grain boundaries) is 0.2 at% (at
Omic%) or less, which is the most important requirement in the present invention. Here, the amount of sulfur at the grain boundaries means the sulfur content (a in the elements segregated at the grain boundaries.
t%). Usually, an Auger electron spectroscope is used to measure the amount of sulfur. In this measurement, the sample was destroyed in a vacuum container kept at a vacuum degree of 1 × (1/10 9 ) torr or less, and the Auger electron was spectroscopically observed while observing a clean grain boundary fracture surface not polluted by the atmosphere. This makes it possible to analyze elements on a clean grain boundary fracture surface.

【0017】一般にオージェ電子分光法により元素の定
量を行う場合、以下に述べるような方法がとられる
(「ユーザのための実用オージェ電子分光法」共立出版
社 1989参照)。すなわち、材料表面における元素の定
量を行う場合は、測定されたオージェ電子強度(エネル
ギーに対して微分されたもので、ピークの高さで示され
る)と各元素のオージェ電子の放出効率を示す指標であ
る相対感度を用いて、以下のように計算される。 [X](at%)={(X/x)/[(A/a)+(B/b)+(C/c) +・・・・・+(X/x)+・・・・]}×100 但し A,B,C,D,・・・・・ :各元素のオージェ電
子強度 a,b,c,d,・・・・・ :各元素の相対感度
In general, when the element is quantified by Auger electron spectroscopy, the following method is used (see "Practical Auger electron spectroscopy for users", Kyoritsu Shuppan 1989). That is, when quantifying an element on the material surface, the measured Auger electron intensity (differentiated with respect to energy, indicated by the peak height) and an index showing the Auger electron emission efficiency of each element It is calculated as follows using a relative sensitivity of [X] (at%) = {(X / x) / [(A / a) + (B / b) + (C / c) + ... + (X / x) + ... ] × 100 However, A, B, C, D, ...: Auger electron intensity of each element a, b, c, d, .....: Relative sensitivity of each element

【0018】このオージェ電子強度を測定するエネルギ
ー位置は元素によって決められており、例えば、Feは
3本あるLMM遷移のうち一番高エネルギー側のピー
ク、OはKLL遷移、CはKLL遷移、SはLVV遷移
を使用する。また、相対感度も各元素の遷移について既
にその値が得られており、上記文献にその値が記載され
ているが、ファイの装置ではFe:0.220,C:
0.140,O:0.400,S:0.750という値
が使われている。このようにオージェ電子分光結果から
元素の定量値を求めることは一般的に行われており、本
発明でもこの方法を採用して結晶粒界の元素の定量を行
った。先に述べたように、本発明者らはこのような方法
で加工性の優れた材料と加工性の劣った材料について粒
界面を探し、この粒界面における元素分析を行ったとこ
ろ、粒界における硫黄濃度が加工性の優劣と極めて大き
な相関を有することを見出したものである。
The energy position for measuring the Auger electron intensity is determined by the element. For example, Fe is the peak on the highest energy side of the three LMM transitions, O is the KLL transition, C is the KLL transition, and S is the S peak. Uses LVV transitions. Also, the relative sensitivity has already been obtained for the transition of each element, and the value is described in the above document, but in the apparatus of Phi, Fe: 0.220, C:
Values of 0.140, O: 0.400, S: 0.750 are used. As described above, the quantitative value of the element is generally obtained from the Auger electron spectroscopy result, and the present invention also employs this method to quantify the element at the crystal grain boundary. As described above, the inventors of the present invention searched for a grain boundary between a material with excellent workability and a material with poor workability by such a method, and performed elemental analysis at this grain boundary. The inventors have found that the sulfur concentration has an extremely large correlation with the processability.

【0019】一例として、表1に示す化学成分を有する
板厚0.1mmの高珪素鋼板であって、オージェ電子分
光により測定した結晶粒界の酸素濃度が略同じものにつ
いて、引張り伸びとオージェ電子分光により測定した結
晶粒界の硫黄濃度との相関を調べた結果を図4に示す。
同図によれば、明らかに結晶粒界の硫黄濃度が低いもの
ほど引張り伸びが良好である。この試験の試料中、引張
り伸びが3%以上あったものは塑性変形を起こしてい
た。さらに、破面の走査電子顕微鏡観察を行ったとこ
ろ、引張り伸びの優れたものほど粒界破壊よりも劈開破
壊が多く、一方、引張り伸びの劣るものほど粒界割れの
傾向が強くなることが判った。従来、このような高珪素
鋼板は塑性変形を起こさないものと考えられてきたが、
結晶粒界における硫黄濃度が0.2at%以下であれば
塑性変形を起こすことが明らかとなった。以上のことか
ら本発明では、結晶粒界における硫黄濃度を0.2at
%以下と限定する。
As an example, for a high silicon steel sheet having a thickness of 0.1 mm having the chemical composition shown in Table 1 and having substantially the same oxygen concentration at the crystal grain boundaries measured by Auger electron spectroscopy, tensile elongation and Auger electron FIG. 4 shows the result of examining the correlation with the sulfur concentration of the crystal grain boundary measured by spectroscopy.
According to the figure, the tensile elongation is better as the sulfur concentration in the crystal grain boundary is obviously lower. Among the samples of this test, those having a tensile elongation of 3% or more caused plastic deformation. Further, when the fracture surface was observed with a scanning electron microscope, it was found that those with better tensile elongation had more cleavage fractures than intergranular fractures, while those with poorer tensile elongation had a greater tendency for intergranular cracking. It was Conventionally, it has been considered that such a high silicon steel sheet does not cause plastic deformation.
It was revealed that plastic deformation occurs when the sulfur concentration at the crystal grain boundary is 0.2 at% or less. From the above, in the present invention, the sulfur concentration at the crystal grain boundary is 0.2 at.
% Or less.

【0020】また、本発明は上記のように粒界における
硫黄濃度を規定するだけでなく、結晶粒界の酸素濃度
(結晶粒界に偏析した元素中の酸素含有量)を30at
%(atomic %)以下とする必要がある。つまり、上記
粒界硫黄濃度低減化による効果は、粒界酸素濃度が十分
に低い場合においてのみ得られるものであり、このため
粒界酸素濃度は30at%以下とすることが必要とな
る。図5はSi:6.66wt%、S:0.001wt
%、Sol.Al:0.001wt%、O:0.002
5wt%の成分組成を有し、且つ粒界における酸素濃度
が異なる鋼板(板厚0.35mm)について、粒界にお
ける硫黄濃度と三点曲げ性(上述した三点曲げ試験での
押込み量)との関係を示したものである。これによれ
ば、粒界酸素濃度が30at%以下では粒界硫黄濃度と
三点曲げ性の相関は認められるが、粒界酸素濃度が30
at%を超えると、粒界硫黄濃度を0.2at%以下に
低減させても三点曲げ性に殆ど変化は見られない。この
ため本発明では、粒界酸素濃度を30at%以下、好ま
しくは15at%以下と規定する。
The present invention not only regulates the sulfur concentration at the grain boundaries as described above, but also sets the oxygen concentration at the grain boundaries (oxygen content in the elements segregated at the grain boundaries) to 30 at.
% (Atomic%) or less. That is, the effect of reducing the grain boundary sulfur concentration can be obtained only when the grain boundary oxygen concentration is sufficiently low, and therefore the grain boundary oxygen concentration needs to be 30 at% or less. Fig. 5 shows Si: 6.66 wt%, S: 0.001 wt%
%, Sol. Al: 0.001 wt%, O: 0.002
With respect to steel plates having a composition of 5 wt% and different oxygen concentrations at grain boundaries (sheet thickness 0.35 mm), the sulfur concentration at the grain boundaries and the three-point bendability (indentation amount in the above-mentioned three-point bending test) It shows the relationship of. According to this, when the grain boundary oxygen concentration is 30 at% or less, the correlation between the grain boundary sulfur concentration and the three-point bendability is recognized, but the grain boundary oxygen concentration is 30
When it exceeds at%, even if the grain boundary sulfur concentration is reduced to 0.2 at% or less, the three-point bendability hardly changes. Therefore, in the present invention, the grain boundary oxygen concentration is defined as 30 at% or less, preferably 15 at% or less.

【0021】また、上記のような結晶粒界における硫黄
濃度および酸素濃度の影響のほかに、結晶粒径も加工性
に影響を及ぼし、板面から見た平均結晶粒径が2.0m
m以下であれば、加工性がさらに向上することが明かと
なった。この効果は、結晶粒界における硫黄の効果によ
り粒界が強くなった分だけ粒内の強さが相対的に低下
し、そのため粒内を貫通する割れが多くなる傾向がある
ため、あまり粒径が大きくなると加工性が劣化すること
が原因と考えられる。表1に示した化学成分を有する高
珪素鋼板の中で、粒界酸素濃度が略5at%、粒界炭素
濃度が略1at%、粒界硫黄濃度が略0.05at%の
ものについて結晶粒径を種々変化させ、板面から見た平
均結晶粒径と三点曲げ特性との関係を調べた。その結果
を図6に示す。これによれば、平均結晶粒径を2.0m
m以下とすることにより加工性が良好となることが判
る。
Further, in addition to the effects of the sulfur concentration and the oxygen concentration at the crystal grain boundaries as described above, the crystal grain size also affects the workability, and the average crystal grain size seen from the plate surface is 2.0 m.
It was revealed that the workability was further improved when the thickness was m or less. This effect is due to the effect of sulfur at the crystal grain boundaries, and the strength of the grain boundaries is relatively reduced by the amount of the strengthening of the grain boundaries, which tends to increase the number of cracks penetrating the grains. It is considered that the workability is deteriorated as the value increases. Among the high silicon steel sheets having the chemical components shown in Table 1, those having a grain boundary oxygen concentration of about 5 at%, a grain boundary carbon concentration of about 1 at% and a grain boundary sulfur concentration of about 0.05 at% have a crystal grain size. The relationship between the average grain size as seen from the plate surface and the three-point bending property was investigated by varying the value. The result is shown in FIG. According to this, the average crystal grain size is 2.0 m
It can be seen that workability is improved by setting the thickness to m or less.

【0022】上記の種々の実験に供した高珪素鋼板は熱
処理による結晶粒成長性が極めて良好で、粗大な粒を形
成しやすく、板厚方向に結晶粒が貫通するいわゆるバン
ブー構造をとりやすい。しかし、上述したように加工性
の観点からは鋼板の結晶粒径は2.0mm以下であるこ
とが好ましく、結晶粒が大きくなり過ぎないように熱処
理条件をコントロールする必要がある。本発明者らは、
高珪素鋼板の結晶組織がバンブー構造をとる場合、鋼板
の板厚のほぼ3〜4倍の結晶粒径で事実上の結晶粒成長
が停止することを見出した。したがって、結晶粒径を
2.0mm以下に保つためには板厚を0.5mm以下に
すればよく、この場合には熱処理上の配慮も必要がなく
なる。このような理由から、鋼板の板厚は0.5mm以
下とすることが好ましい。
The high silicon steel sheets used in the various experiments described above have extremely good crystal grain growth properties by heat treatment, are likely to form coarse grains, and have a so-called bamboo structure in which crystal grains penetrate in the plate thickness direction. However, as described above, the crystal grain size of the steel sheet is preferably 2.0 mm or less from the viewpoint of workability, and it is necessary to control the heat treatment conditions so that the crystal grains do not become too large. We have
It has been found that when the crystal structure of the high silicon steel sheet has a bamboo structure, the actual crystal grain growth stops at a grain size of 3 to 4 times the plate thickness of the steel sheet. Therefore, in order to keep the crystal grain size at 2.0 mm or less, the plate thickness may be set at 0.5 mm or less, and in this case, it is not necessary to consider heat treatment. For these reasons, the plate thickness of the steel plate is preferably 0.5 mm or less.

【0023】なお、本発明の効果は珪素鋼板の結晶方位
分布に関係なく得られるものであり、したがって、本発
明の対象は方向性珪素鋼板であるか無方向性珪素鋼板で
あるかを問わない。また、通常電磁鋼板の表面には絶縁
を目的とした皮膜が形成されるが、本発明の効果は皮膜
の有無にも影響されない。また、本発明では薄板を得る
方法に特別な制約はなく、先に述べた特殊な圧延法や浸
珪法等、適宜な方法で製造された高珪素鋼板に適用でき
る。
The effect of the present invention is obtained regardless of the crystal orientation distribution of the silicon steel sheet, and therefore the present invention does not matter whether it is a grain-oriented silicon steel sheet or a non-oriented silicon steel sheet. . In addition, although a film for the purpose of insulation is usually formed on the surface of the electromagnetic steel sheet, the effect of the present invention is not affected by the presence or absence of the film. Further, in the present invention, there is no particular restriction on the method of obtaining a thin plate, and the present invention can be applied to a high silicon steel plate manufactured by an appropriate method such as the above-described special rolling method or siliconizing method.

【0024】[0024]

【実施例】【Example】

〔実施例1〕表2に示す成分組成を有する板厚0.1m
mの高珪素鋼板において、5torr〜1×(1/10
5)torrの範囲の異なる真空度の雰囲気において、
1200℃×15分の熱処理(最終焼鈍)を行った。こ
の時の実験室気温は27℃、湿度80%であった。この
ようにして得られた試料を図2に示す三点曲げ試験に供
し、割れずに押し込めるストローク距離を測定した。さ
らに、各試料の残材をオージェ電子分光装置に持込み、
8×(1/1010)torrの真空中で破壊させ、その
破面を観察して結晶粒界での組成分析を行った。この組
成分析に基づき、試料の中から粒界酸素濃度が3〜5a
t%、粒界炭素濃度が略0.3at%、平均結晶粒径が
略0.2mmのものを選び、これらの試料について三点
曲げ量に及ぼす粒界硫黄濃度の影響を調べた。その結果
を図7に示す。これによれば、結晶粒界における硫黄濃
度が減少すると三点曲げ量が明らかに向上しており、結
晶粒界の硫黄濃度が低いほうが加工性が良好であること
が判る。
[Example 1] Plate thickness of 0.1 m having the composition shown in Table 2
m high silicon steel sheet, 5 torr to 1 × (1/10
5 ) In an atmosphere of vacuum degree with different torr range,
Heat treatment (final annealing) was performed at 1200 ° C. for 15 minutes. At this time, the laboratory temperature was 27 ° C. and the humidity was 80%. The sample thus obtained was subjected to the three-point bending test shown in FIG. 2, and the stroke distance at which the sample could be pushed in without cracking was measured. In addition, bring the remaining material of each sample into the Auger electron spectrometer,
It was broken in a vacuum of 8 × (1/10 10 ) torr, and the broken surface was observed to analyze the composition at the grain boundaries. Based on this compositional analysis, the oxygen concentration in the grain boundary was 3 to 5
t%, grain boundary carbon concentration of about 0.3 at% and average crystal grain size of about 0.2 mm were selected, and the influence of the grain boundary sulfur concentration on the three-point bending amount was examined for these samples. The result is shown in FIG. 7. According to this, when the sulfur concentration in the crystal grain boundary is decreased, the three-point bending amount is obviously improved, and it is understood that the workability is better when the sulfur concentration in the crystal grain boundary is lower.

【0025】〔実施例2〕表3に示す成分組成を有する
種々の板厚の高珪素鋼板について、1×(1/104
torrの真空度の雰囲気において、800〜1300
℃の範囲の異なる焼鈍温度で15分間の最終焼鈍を行
い、種々の板厚、平均結晶粒径を有する試料を作製し
た。このようにして得られた試料について三点曲げ試験
を実施し、さらに各試料の残材をオージェ電子分光装置
に持込み、結晶粒界の酸素濃度、炭素濃度、硫黄濃度を
測定した。オージェ電子分光測定の結果では、いずれの
試料も粒界酸素濃度が8±2at%、粒界炭素濃度が
0.8〜2at%、粒界硫黄濃度が0.05〜0.10
at%の範囲であった。各試料の平均結晶粒径および三
点曲げ試験の結果を表4に示す。これによれば、平均結
晶粒径が2.0mmを超えると曲げ特性が著しく劣化す
ることが判る。また、板厚が0.5mmを超えるものは
平均結晶粒径が2.0mm以下であっても曲げ特性に劣
っている。
Example 2 With respect to high silicon steel sheets having various thicknesses and having the composition shown in Table 3, 1 × (1/10 4 )
800 to 1300 in an atmosphere with a vacuum degree of torr
Final annealing was performed for 15 minutes at different annealing temperatures in the range of ° C to prepare samples having various plate thicknesses and average crystal grain sizes. A three-point bending test was performed on the samples thus obtained, and the residual material of each sample was brought into an Auger electron spectroscope to measure the oxygen concentration, carbon concentration, and sulfur concentration of grain boundaries. As a result of Auger electron spectroscopy measurement, the grain boundary oxygen concentration was 8 ± 2 at%, the grain boundary carbon concentration was 0.8 to 2 at%, and the grain boundary sulfur concentration was 0.05 to 0.10.
It was in the range of at%. Table 4 shows the average crystal grain size of each sample and the result of the three-point bending test. According to this, it can be seen that the bending property is significantly deteriorated when the average crystal grain size exceeds 2.0 mm. Further, those having a plate thickness of more than 0.5 mm are inferior in bending property even if the average crystal grain size is 2.0 mm or less.

【0026】〔実施例3〕表5に示す化学成分を有する
板厚0.3mmの珪素鋼板を作製し、1200℃におい
て浸珪処理−拡散処理(Si拡散浸透処理)を行った。
上記浸珪処理は、キャリアガスとして高純度窒素ガス
(露点−70℃)を混合した四塩化珪素(SiCl4
雰囲気ガスと、キャリアガスとして通常窒素ガス(露点
−30℃)を混合した四塩化珪素(SiCl4)雰囲気
ガスの2種類の雰囲気ガスを使用して行った。これらの
試料について三点曲げ試験を行い、また、その残材から
オージェ電子分光測定により結晶粒界の酸素濃度、炭素
濃度、硫黄濃度を測定した。この組成分析に基づき、試
料の中から粒界酸素濃度が略10at%、粒界炭素濃度
が略0.7at%、平均結晶粒径が略0.80mmのも
のを選び、これらの試料について粒界硫黄濃度と三点曲
げ量との相関を調べた。その結果を図8に示す。これに
よれば、Si拡散浸透処理により得られた高珪素鋼板に
ついても、結晶粒界の硫黄濃度の規制が鋼板の加工性の
向上に有効であることが判る。
Example 3 A silicon steel sheet having a chemical composition shown in Table 5 and a thickness of 0.3 mm was prepared and subjected to a siliconizing treatment-diffusion treatment (Si diffusion infiltration treatment) at 1200 ° C.
The siliconizing treatment is performed using silicon tetrachloride (SiCl 4 ) mixed with high-purity nitrogen gas (dew point −70 ° C.) as a carrier gas.
Two atmosphere gases were used: an atmosphere gas and a silicon tetrachloride (SiCl 4 ) atmosphere gas in which nitrogen gas (dew point −30 ° C.) was mixed as a carrier gas. A three-point bending test was performed on these samples, and the oxygen concentration, carbon concentration, and sulfur concentration at the grain boundaries were measured from the remaining material by Auger electron spectroscopy. Based on this compositional analysis, those having a grain boundary oxygen concentration of about 10 at%, a grain boundary carbon concentration of about 0.7 at%, and an average crystal grain size of about 0.80 mm were selected from the samples. The correlation between sulfur concentration and three-point bending amount was investigated. The result is shown in FIG. According to this, it can be seen that, even in the high-silicon steel sheet obtained by the Si diffusion and infiltration treatment, the regulation of the sulfur concentration in the crystal grain boundaries is effective in improving the workability of the steel sheet.

【0027】〔実施例4〕表6に示す成分組成を有する
板厚0.35mmの鋼板を圧延法にて作製し、露点を−
10℃から−70℃、H2S濃度を0から0.1vol
%で変化させた窒素雰囲気中で1200℃×15分の熱
処理を行った。これらの試料について図2に示した三点
曲げ試験を行い、また、その残材からオージェ電子分光
測定により、結晶粒界の酸素濃度および硫黄濃度を測定
し、三点曲げ量に及ぼす粒界酸素濃度、粒界硫黄濃度の
影響を調べた。その結果を図5に示す。これによれば、
粒界酸素濃度が30at%以下では粒界硫黄濃度と三点
曲げ性の相関は認められるが、粒界酸素濃度が30at
%を超えると、粒界硫黄濃度を0.2at%以下に低減
させても三点曲げ性にほとんど変化は見られないことが
判る。
Example 4 A steel plate having a composition of the components shown in Table 6 and a plate thickness of 0.35 mm was prepared by a rolling method, and the dew point was-.
10 ℃ to -70 ℃, H 2 S concentration 0 to 0.1 vol
The heat treatment was performed at 1200 ° C. for 15 minutes in the nitrogen atmosphere changed in%. The three-point bending test shown in Fig. 2 was performed on these samples, and the oxygen concentration and the sulfur concentration of the crystal grain boundaries were measured from the residual material by Auger electron spectroscopy to determine the effect of the grain boundary oxygen on the three-point bending amount. The effect of concentration and intergranular sulfur concentration was investigated. The result is shown in FIG. According to this
When the grain boundary oxygen concentration is 30 at% or less, the correlation between the grain boundary sulfur concentration and the three-point bendability is recognized, but the grain boundary oxygen concentration is 30 at%.
It is found that when the content exceeds 0.1%, there is almost no change in the three-point bendability even when the grain boundary sulfur concentration is reduced to 0.2 at% or less.

【0028】[0028]

【表1】 [Table 1]

【0029】[0029]

【表2】 [Table 2]

【0030】[0030]

【表3】 [Table 3]

【0031】[0031]

【表4】 [Table 4]

【0032】[0032]

【表5】 [Table 5]

【0033】[0033]

【表6】 [Table 6]

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

【図1】本発明者らが行った試験において得られた高珪
素鋼板について、最終焼鈍雰囲気の真空度と鋼板の三点
曲げ特性との関係を示すグラフ
FIG. 1 is a graph showing the relationship between the degree of vacuum in the final annealing atmosphere and the three-point bending property of a steel sheet obtained from a test conducted by the inventors of the present invention.

【図2】鋼板の加工性を評価する三点曲げ試験方法を示
す説明図
FIG. 2 is an explanatory diagram showing a three-point bending test method for evaluating workability of a steel sheet.

【図3】粒界酸素濃度が3〜5at%の高珪素鋼板につ
いて、粒界硫黄濃度と三点曲げ特性との関係を示すグラ
FIG. 3 is a graph showing the relationship between the grain boundary sulfur concentration and the three-point bending property for a high silicon steel sheet having a grain boundary oxygen concentration of 3 to 5 at%.

【図4】粒界酸素濃度が略同じ高珪素鋼板について、粒
界硫黄濃度と鋼板の引張り伸びとの関係を示すグラフ
FIG. 4 is a graph showing the relationship between the grain boundary sulfur concentration and the tensile elongation of the steel sheets for high silicon steel sheets having substantially the same grain boundary oxygen concentration.

【図5】粒界硫黄濃度および粒界酸素濃度と鋼板の三点
曲げ特性との関係を示すグラフ
FIG. 5 is a graph showing the relationship between the grain boundary sulfur concentration and the grain boundary oxygen concentration and the three-point bending property of the steel sheet.

【図6】粒界酸素濃度が略5at%、粒界炭素濃度が略
1at%、粒界硫黄濃度が略0.05at%の高珪素鋼
板について、板面からみた平均結晶粒径と三点曲げ特性
との関係を示すグラフ
FIG. 6 is an average crystal grain size as seen from the plate surface and three-point bending for a high silicon steel sheet having a grain boundary oxygen concentration of about 5 at%, a grain boundary carbon concentration of about 1 at%, and a grain boundary sulfur concentration of about 0.05 at%. Graph showing the relationship with characteristics

【図7】実施例1の高珪素鋼板について、粒界硫黄濃度
と鋼板の三点曲げ特性との関係を示すグラフ
FIG. 7 is a graph showing the relationship between the grain boundary sulfur concentration and the three-point bending property of the high silicon steel sheet of Example 1

【図8】実施例3の高珪素鋼板について、粒界硫黄濃度
と鋼板の三点曲げ特性との関係を示すグラフ
FIG. 8 is a graph showing the relationship between the grain boundary sulfur concentration and the three-point bending property of the steel sheet for the high silicon steel sheet of Example 3

───────────────────────────────────────────────────── フロントページの続き (72)発明者 笠井 勝司 東京都千代田区丸の内一丁目1番2号 日 本鋼管株式会社内 (72)発明者 岡田 和久 東京都千代田区丸の内一丁目1番2号 日 本鋼管株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Katsushi Kasai 1-2-1, Marunouchi, Chiyoda-ku, Tokyo Nihon Kokan Co., Ltd. (72) Kazuhisa Okada 1-2-1 Marunouchi, Chiyoda-ku, Tokyo Date Main Steel Pipe Co., Ltd.

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】 Si:4〜10wt%を含有し、結晶粒
界におけるO濃度(結晶粒界に偏析する元素中のO濃
度)が30at%以下、結晶粒界におけるS濃度(結晶
粒界に偏析する元素中のS濃度)が0.2at%以下で
ある加工性の優れた高珪素電磁鋼板。
1. An Si concentration of 4 to 10 wt%, an O concentration at a crystal grain boundary (O concentration in an element segregated at the crystal grain boundary) is 30 at% or less, and an S concentration at the crystal grain boundary (at the crystal grain boundary). A high silicon magnetic steel sheet having excellent workability, in which the S concentration in the segregating element) is 0.2 at% or less.
【請求項2】 C:0.01wt%以下、Si:4〜1
0wt%、Mn:0.5wt%以下、P:0.01wt
%以下、S:0.01wt%以下、Sol.Al:0.
2wt%以下、N:0.01wt%以下、O:0.02
wt%以下、残部Feおよび不可避不純物からなり、結
晶粒界におけるO濃度(結晶粒界に偏析する元素中のO
濃度)が30at%以下、結晶粒界におけるS濃度(結
晶粒界に偏析する元素中のS濃度)が0.2at%以下
である加工性の優れた高珪素電磁鋼板。
2. C: 0.01 wt% or less, Si: 4-1
0 wt%, Mn: 0.5 wt% or less, P: 0.01 wt
% Or less, S: 0.01 wt% or less, Sol. Al: 0.
2 wt% or less, N: 0.01 wt% or less, O: 0.02
wt% or less, the balance being Fe and unavoidable impurities, and the O concentration in the crystal grain boundaries (O in the elements segregated at the crystal grain boundaries
A high-silicon electrical steel sheet having excellent workability, in which the concentration) is 30 at% or less, and the S concentration in the crystal grain boundary (S concentration in the element segregated in the crystal grain boundary) is 0.2 at% or less.
【請求項3】 Si+Al:4〜10wt%を含有し、
結晶粒界におけるO濃度(結晶粒界に偏析する元素中の
O濃度)が30at%以下、結晶粒界におけるS濃度
(結晶粒界に偏析する元素中のS濃度)が0.2at%
以下である加工性の優れた高珪素電磁鋼板。
3. Si + Al: containing 4 to 10 wt%,
O concentration in the crystal grain boundary (O concentration in the element segregated in the crystal grain boundary) is 30 at% or less, S concentration in the crystal grain boundary (S concentration in the element segregated in the crystal grain boundary) is 0.2 at%
The following are high-silicon electrical steel sheets with excellent workability.
【請求項4】 C:0.01wt%以下、Si+Al:
4〜10wt%、Mn:0.5wt%以下、P:0.0
1wt%以下、S:0.01wt%以下、N:0.01
wt%以下、O:0.02wt%以下、残部Feおよび
不可避不純物からなり、結晶粒界におけるO濃度(結晶
粒界に偏析する元素中のO濃度)が30at%以下、結
晶粒界におけるS濃度(結晶粒界に偏析する元素中のS
濃度)が0.2at%以下である加工性の優れた高珪素
電磁鋼板。
4. C: 0.01 wt% or less, Si + Al:
4 to 10 wt%, Mn: 0.5 wt% or less, P: 0.0
1 wt% or less, S: 0.01 wt% or less, N: 0.01
wt% or less, O: 0.02 wt% or less, balance Fe and unavoidable impurities, O concentration in crystal grain boundaries (O concentration in elements segregated in crystal grain boundaries) is 30 at% or less, S concentration in crystal grain boundaries (S in elements segregated at the grain boundaries
A high silicon electrical steel sheet having a workability of 0.2 at% or less.
【請求項5】 板厚が0.5mm以下、板面から見た平
均結晶粒径が2.0mm以下である請求項1、請求項
2、請求項3または請求項4に記載の加工性の優れた高
珪素電磁鋼板。
5. The workability according to claim 1, claim 2, claim 3 or claim 4, wherein the plate thickness is 0.5 mm or less and the average crystal grain size when viewed from the plate surface is 2.0 mm or less. Excellent high silicon electrical steel sheet.
JP5028562A 1992-12-08 1993-01-25 High silicon magnetic steel sheet with excellent workability Expired - Fee Related JP2956406B2 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP5028562A JP2956406B2 (en) 1993-01-25 1993-01-25 High silicon magnetic steel sheet with excellent workability
DE69312233T DE69312233T2 (en) 1992-12-08 1993-12-07 Electrical sheet
EP93119720A EP0601549B1 (en) 1992-12-08 1993-12-07 Electrical steel sheet
KR1019930026779A KR960006447B1 (en) 1992-12-08 1993-12-07 High silicon steel sheet excellent in workability
CN93120804A CN1035889C (en) 1992-12-08 1993-12-08 Electrical steel sheet

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Application Number Priority Date Filing Date Title
JP5028562A JP2956406B2 (en) 1993-01-25 1993-01-25 High silicon magnetic steel sheet with excellent workability

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