JPH08337823A - Production of grain oriented silicon steel sheet excellent in blankability and magnetic property - Google Patents
Production of grain oriented silicon steel sheet excellent in blankability and magnetic propertyInfo
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- JPH08337823A JPH08337823A JP7141652A JP14165295A JPH08337823A JP H08337823 A JPH08337823 A JP H08337823A JP 7141652 A JP7141652 A JP 7141652A JP 14165295 A JP14165295 A JP 14165295A JP H08337823 A JPH08337823 A JP H08337823A
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- Prior art keywords
- annealing
- steel sheet
- coating
- film
- finish annealing
- Prior art date
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、変圧器その他の電気
機器の鉄心などに用いられる方向性けい素鋼板の製造方
法に関し、特に磁気特性に併せて打ち抜き性を向上しよ
うとするものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a grain-oriented silicon steel sheet used for an iron core of a transformer or other electric equipment, and particularly to improve punchability in accordance with magnetic characteristics.
【０００２】[0002]
【従来の技術】方向性電磁鋼板は、含けい素鋼スラブに
熱間圧延、次いで冷間圧延を施し、その後脱炭焼鈍を施
し鋼板表面に酸化層を形成し、その後MgO を主成分とす
る焼鈍分離剤を塗布してから仕上げ焼鈍を行って、２次
再結晶粒を発達させるとともに鋼板表面にフォルステラ
イト質被膜を形成する、一連の工程にて製造されるのが
一般的である。かくして得られた方向性電磁鋼板は、打
ち抜きや剪断により所定形状に加工した単板の多数枚を
積層して変圧器その他の電気機器の鉄心として提供され
る。2. Description of the Related Art Grain-oriented electrical steel sheets are made of slabs of silicon steel that are hot-rolled, then cold-rolled, decarburized and annealed to form an oxide layer on the surface of the steel sheet, and then MgO is the main component. It is generally manufactured by a series of steps in which after applying an annealing separator, finish annealing is performed to develop secondary recrystallized grains and form a forsterite coating on the surface of a steel sheet. The grain-oriented electrical steel sheet thus obtained is provided as an iron core of a transformer or other electric equipment by laminating a large number of single sheets processed into a predetermined shape by punching or shearing.
【０００３】この打ち抜きや剪断の加工工程において
は、鋼板表面を覆うフォルステライト質被膜が硬質であ
ることから、その加工後の鋼板に反りが発生したり、あ
るいは打ち抜き金型が早期に磨耗することが問題になる
ため、いわゆる打ち抜き性を向上することも方向性電磁
鋼板の重要な課題となっている。In the punching and shearing process, since the forsterite coating covering the surface of the steel sheet is hard, the steel sheet after the working is warped or the punching die is worn early. However, improving so-called punchability is also an important issue for grain-oriented electrical steel sheets.
【０００４】従来、この課題に対して、グラス被膜（下
地被膜）のない方向性磁気鋼板を提供する方法が種々提
案されている。例えば、特開昭59-96278号および同60-3
9123号各公報には、主成分がAl2O3 の焼鈍分離剤を用い
てフォルステライト被膜の形成を阻止する方法が開示さ
れている。また、特開昭64-79381号公報には、焼鈍分離
剤主成分としてCaまたはSrメタ珪酸塩及びCaのアルミン
酸塩から選ばれた非水和性粉末の１種または２種以上を
合計で15〜60wt％を含み、残部は少なくとも40wt％のAl
2O3 粉末からなる混合物を主成分とする、焼鈍分離剤を
用いる方法が開示されている。さらに、特開昭64-62476
号公報には、MgO を主成分としアルカリもしくはアルカ
リ土類塩化物を２〜40部添加した焼鈍分離剤を用いて、
仕上げ焼鈍でマグネシアと鋼板表面の酸化膜中のSiO2と
の反応を抑制して、グラス被膜を生成させない方法が開
示されている。To solve this problem, various methods have been proposed in the past for providing a grain-oriented magnetic steel sheet without a glass coating (undercoat). For example, JP-A-59-96278 and JP-A-60-3
Japanese Patent No. 9123 discloses a method of preventing the formation of a forsterite film by using an annealing separator having a main component of Al 2 O 3 . Further, Japanese Patent Laid-Open No. 64-79381 discloses a total of one or more non-hydratable powders selected from Ca or Sr metasilicate and Ca aluminate as a main component of an annealing separator. 15-60% by weight, balance of at least 40% by weight Al
A method of using an annealing separator having a mixture of 2 O 3 powder as a main component is disclosed. Furthermore, JP-A-64-62476
In the gazette, an annealing separator containing MgO as a main component and 2 to 40 parts of an alkali or alkaline earth chloride is added,
A method is disclosed in which the reaction between magnesia and SiO 2 in the oxide film on the surface of the steel sheet is suppressed by finish annealing and a glass film is not formed.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、上記の
方法はいずれも、仕上げ焼鈍中にフォルステライト質の
グラス被膜の形成を極力抑制する技術であり、グラス被
膜による効果が得られずに２次再結晶が不安定になるか
ら、磁気特性の劣化が不可避であった。However, each of the above methods is a technique for suppressing the formation of a forsterite glass coating film during finish annealing as much as possible, and the effect of the glass coating film is not obtained, so that the secondary recycling is not performed. Since the crystal becomes unstable, the deterioration of magnetic properties was inevitable.
【０００６】なぜなら、方向性電磁鋼板用の素材は、
（１１０）＜００１＞方位の集積度を高めるために、例
えばMnSe, MnS, AlNなどのインヒビター成分を含有して
いるのが一般的であり、仕上げ焼鈍中に鋼板表面の酸化
が過度に進行した場合、表層インヒビターの分解消失が
起こりやすく、２次再結晶不良を生じる。また、鋼板の
窒化が進行して地鉄表層近傍で窒化物が過度に析出して
も、２次再結晶不良を招くのである。[0006] Because, the material for the grain-oriented electrical steel sheet is
In order to increase the degree of integration of the (110) <001> orientation, it is common to contain an inhibitor component such as MnSe, MnS, AlN, etc., and excessive oxidation of the steel sheet surface occurred during finish annealing. In this case, decomposition and disappearance of the surface layer inhibitor is likely to occur, resulting in secondary recrystallization failure. Further, even if nitriding of the steel sheet progresses and nitride is excessively precipitated in the vicinity of the surface layer of the base steel, secondary recrystallization failure is caused.
【０００７】そこで、この発明は、２次再結晶不良をま
ねくことなしに、被膜のない方向性電磁鋼製品を得る方
法について提案することによって、打ち抜き性および磁
気特性がともに優れた方向性電磁鋼板を提供しようとす
るものである。Therefore, the present invention proposes a method for obtaining a grain-oriented electrical steel product without a coating without causing a secondary recrystallization defect, thereby providing a grain-oriented electrical steel sheet excellent in both punching properties and magnetic properties. Is to provide.
【０００８】[0008]
【課題を解決するための手段】すなわち、この発明は、
含けい素鋼素材に熱間圧延、そして冷間圧延を施して最
終板厚に仕上げ、次いで湿水素中にて脱炭焼鈍を施して
鋼板表面に酸化層を形成したのち、焼鈍分離剤を塗布し
てから仕上げ焼鈍を行う一連の工程にて方向性電磁鋼板
を製造するに当たり、該仕上げ焼鈍中に線膨張係数が含
けい素鋼素材の0.5 倍以下のセラミック質被膜を形成
し、引き続く仕上げ焼鈍後期の降温時に被膜と素材との
間に生じる熱応力により被膜を剥離させることを特徴と
する打ち抜き性および磁気特性の優れた方向性電磁鋼板
の製造方法である。That is, the present invention provides:
Hot-rolling and cold-rolling the silicon-containing steel material to finish to the final thickness, then decarburizing annealing in wet hydrogen to form an oxide layer on the steel sheet surface, and then applying an annealing separator. In the process of producing grain-oriented electrical steel sheets in a series of steps after which finish annealing is performed, a ceramic coating with a coefficient of linear expansion of 0.5 times or less of that of silicon steel material is formed during the finish annealing, and the subsequent finish annealing is performed. A method for producing a grain-oriented electrical steel sheet having excellent punching properties and magnetic properties, characterized in that the coating film is peeled off by a thermal stress generated between the coating film and the raw material when the temperature is lowered in the latter half.
【０００９】ここで、上記セラミック質被膜には、低熱
膨張性のMg−Al−Si−Ｏ系シリケート化合物からなるも
の、とりわけ４MgO ・５Al2O3 ・２SiO2、２MgO ・２Al
2O3・５SiO2または MgO・Al2O3 ・２SiO2が有利に適合
する。また、上記の被膜を形成するには、MgO ：10〜20
wt％およびAl2O3 ：20〜50wt％を含み残部がSiO2の組成
になる焼鈍分離剤を用いることが好ましい。[0009] Here, the above-mentioned ceramic membrane coating, made of a low thermal expansion of the Mg-Al-Si-O-based silicate compounds, especially 4MgO · 5Al 2 O 3 · 2SiO 2, 2MgO · 2Al
2 O 3 · 5SiO 2 or MgO · Al 2 O 3 · 2SiO 2 is advantageously suited. Further, in order to form the above film, MgO: 10 to 20
It is preferable to use an annealing separator containing wt% and Al 2 O 3 : 20 to 50 wt% and the balance being SiO 2 .
【００１０】次に、この発明を完成するに到った実験結
果について述べる。表１に示す化学成分になる鋼塊に熱
間圧延を施し、引き続き１回の中間焼鈍を含む冷間圧延
にて、板厚0.22mmの冷延板を作製した。この冷延板にＨ
2 ：50％および露点：62℃の湿水素雰囲気中で 840℃×
２分間の脱炭焼鈍を施し、図１に示す組成の焼鈍分離剤
（図中記号のＡ〜Ｚおよびａ〜ｇ）を塗布してから、 8
50℃×15時間の１次保定を含む、1200℃×10時間の仕上
げ焼鈍を施した。この仕上げ焼鈍は、室温〜 850℃まで
を窒素雰囲気とし、その後 850℃から1100℃を水素−窒
素混合雰囲気、そして1100℃〜鈍化焼鈍温度域 (1200
℃) を水素雰囲気として行った。Next, the results of experiments that have led to the completion of the present invention will be described. A steel ingot having the chemical composition shown in Table 1 was hot-rolled, and then cold-rolled including one intermediate annealing to produce a cold-rolled sheet having a sheet thickness of 0.22 mm. H on this cold rolled sheet
2 : 840 ° C in a wet hydrogen atmosphere with 50% and dew point: 62 ° C
After decarburizing annealing for 2 minutes and applying the annealing separating agent (A to Z and a to g in the figure) having the composition shown in FIG. 1, 8
Finish annealing was performed at 1200 ° C for 10 hours, including primary retention at 50 ° C for 15 hours. In this finish annealing, the room temperature to 850 ° C is set in a nitrogen atmosphere, then 850 ° C to 1100 ° C in a hydrogen-nitrogen mixed atmosphere, and 1100 ° C to the annealing temperature range (1200
(° C.) under a hydrogen atmosphere.
【００１１】[0011]
【表１】 [Table 1]
【００１２】かくして得られた鋼板の表面状態を調査し
たところ、被膜がなく金属光沢を有する鋼板が多数認め
られた。そこで、これら鋼板に被膜のない理由を解明す
るため、仕上げ焼鈍工程を詳しく観察した結果、これら
鋼板では、仕上げ焼鈍中に被膜が形成されるが、この被
膜は仕上げ焼鈍後期の降温時に剥離し、金属光沢面が現
れたことを新たに見出した。さらに、被膜が仕上げ焼鈍
後期の降温時に剥離する現象を詳細に調査したところ、
地鉄および被膜の線膨張係数の差と相関のあることを知
見した。When the surface condition of the steel sheet thus obtained was investigated, a large number of steel sheets without a coating and having metallic luster were recognized. Therefore, in order to elucidate the reason why there is no coating on these steel sheets, as a result of observing the finish annealing step in detail, in these steel sheets, a coating is formed during finish annealing, but this coating peels off during cooling during the latter stage of finish annealing, It was newly found that a metallic glossy surface appeared. Furthermore, a detailed investigation of the phenomenon that the film peels off during lowering of the temperature in the latter stage of finish annealing,
It was found that there was a correlation with the difference in the coefficient of linear expansion between the base steel and the coating.
【００１３】すなわち、上記の実験で使用した焼鈍分離
剤にて仕上げ焼鈍中に生成した被膜および地鉄の線膨張
係数の比と、仕上げ焼鈍後の鋼板片面の酸素目付け量と
の関係を図２に示す。ここで鋼板片面の酸素目付け量
は、仕上げ焼鈍後の被膜の剥離性を示す指標として用い
た。すなわち、酸素目付け量が少ないほど、被膜の剥離
性は良好である。同図から、酸素目付け量が極めて少な
くなって、被膜がほとんどあるいは全く残存しない条件
は、被膜の線膨張係数が地鉄のそれの0.5 倍以下の範囲
であることがわかる。That is, the relationship between the ratio of the linear expansion coefficient of the coating and the base iron formed during the finish annealing with the annealing separator used in the above experiment and the oxygen basis weight of one side of the steel sheet after the finish annealing is shown in FIG. Shown in. Here, the oxygen basis weight of one side of the steel sheet was used as an index showing the peelability of the coating film after finish annealing. That is, the smaller the oxygen basis weight, the better the peelability of the coating. From the figure, it is understood that the linear expansion coefficient of the coating is within 0.5 times that of the base iron under the condition that the coating amount of oxygen is extremely small and the coating hardly remains at all.
【００１４】さらに、上記と同様の条件にて得られた鋼
板に対して、表面状態および磁気特性に関する、より詳
しい調査を行った。その結果を、表面状態については図
３に、また得られた鋼板の磁束密度Ｂ8 値については図
４に、それぞれ示す。Further, the steel sheets obtained under the same conditions as above were subjected to a more detailed investigation on the surface condition and magnetic properties. The results are shown in FIG. 3 for the surface condition and in FIG. 4 for the magnetic flux density B 8 value of the obtained steel sheet.
【００１５】図３に示すように、完全な金属光沢がみと
められた、すなわち被膜が完全に剥離していた鋼板は、
MgO ：20wt％以下、SiO2：30wt％以下およびAl2O3 ：10
〜60wt％の範囲の組成の焼鈍分離剤を塗布したものであ
り、それ以外の組成の焼鈍分離剤を塗布した鋼板は完全
に被膜が形成されるか、もしくは被膜の剥離が不十分で
不完全な金属光沢を示した。なお、完全な金属光沢を有
する表面とは、片面当たりの酸素目付け量が 0.1ｇ／ｍ
2 以下で仕上げ焼鈍後に２次粒が認識できるものを指
す。As shown in FIG. 3, the steel sheet having a complete metallic luster, that is, the coating film completely peeled off,
MgO: 20 wt% or less, SiO 2 : 30 wt% or less, and Al 2 O 3 : 10
A steel sheet coated with an annealing separator with a composition in the range of up to 60 wt% and coated with an annealing separator with a composition other than that either forms a complete film, or the film peeling is incomplete and incomplete. It exhibited a metallic luster. A surface with a perfect metallic luster means that the oxygen basis weight per surface is 0.1 g / m 2.
A value of 2 or less indicates that secondary particles can be recognized after finish annealing.
【００１６】一方、磁束密度は、図４に示す結果から、
MgO：30wt％以下、SiO2：50〜80wt％および Al2O3：20
〜50wt％の組成の焼鈍分離剤を塗布したもので、Ｂ8 値
が1.95Ｔ以上と良好な結果が得られることがわかる。従
って、被膜がなくかつ磁束密度に優れた鋼板を得るに
は、図２に示したように、線膨張係数が地鉄のそれの0.
5 倍以下の被膜を仕上げ焼鈍中に形成することが肝要で
あり、特にMgO ：10〜20wt％およびAl2O3 ：20〜50wt％
を含み、残部がSiO2の組成になる焼鈍分離剤を用いるこ
とが好ましい。On the other hand, the magnetic flux density is calculated from the results shown in FIG.
MgO: 30 wt% or less, SiO 2 : 50-80 wt% and Al 2 O 3 : 20
It can be seen that, when an annealing separator having a composition of up to 50 wt% is applied, a good result with a B 8 value of 1.95 T or more is obtained. Therefore, in order to obtain a steel sheet with no coating and excellent magnetic flux density, as shown in Fig. 2, the coefficient of linear expansion is 0.
It is important to form a film of 5 times or less during finish annealing, especially MgO: 10 to 20 wt% and Al 2 O 3 : 20 to 50 wt%.
It is preferable to use an annealing separator containing the above and having the composition of SiO 2 as the balance.
【００１７】また、図１に示した組成の焼鈍分離剤を塗
布してから、1200℃で５時間保持する仕上げ焼鈍を行っ
て得られた被膜の組成について調査した。この仕上げ焼
鈍は、900 ℃〜1100℃の温度域を水素雰囲気で、それ以
外は窒素雰囲気で行った。かくして得られた鋼板の表面
に生成した主な酸化物を、Ｘ線回折により同定した結果
について図５に示す。Further, the composition of the coating film obtained by applying the annealing separator having the composition shown in FIG. 1 and then performing the final annealing held at 1200 ° C. for 5 hours was investigated. This finish annealing was performed in a hydrogen atmosphere in a temperature range of 900 ° C to 1100 ° C, and in a nitrogen atmosphere in other cases. The main oxide formed on the surface of the steel sheet thus obtained was identified by X-ray diffraction, and the results are shown in FIG.
【００１８】図５に示す被膜組成物の分析結果と図３お
よび４に示した結果とを重ね合わせると、被膜の剥離性
および磁気特性に優れる被膜はコーディライトやサフィ
リンを主相とするものであり、またコーディライトやサ
フィリンを主相とする被膜は、コーディライトおよびサ
フィリンの化学量論組成よりもSiO2リッチ側で形成され
ることがわかる。すなわち、MgO ：30wt％以下かつSi
O2：30wt％以上の条件でコーディライトやサフィリンが
形成され、MgO リッチでは、エンスタタイトまたはフォ
ルステライトが形成され、Al2O3 リッチではスピネルが
主相となる。When the analysis results of the coating composition shown in FIG. 5 and the results shown in FIGS. 3 and 4 are overlapped, the coating having excellent peelability and magnetic properties is mainly composed of cordierite or sapphirine. It can be seen that the film containing cordierite or sapphirine as the main phase is formed on the SiO 2 rich side of the stoichiometric composition of cordierite or sapphirine. That is, MgO: 30 wt% or less and Si
O 2: at 30 wt% or more conditions cordierite and sapphirine are formed in the MgO-rich, enstatite or forsterite is formed, a spinel is the main phase in the Al 2 O 3 rich.
【００１９】[0019]
【作用】仕上げ焼鈍中には、脱炭焼鈍後の表面酸化層と
焼鈍分離剤成分との固相反応によりセラミックス質被膜
が形成される。そして、焼鈍分離剤の主成分が MgOであ
ると、フォルステライト質のグラス被膜が生成される。
このフォルステライト質被膜の線膨張係数は、方向性電
磁鋼板用素材の約 0.8〜0.9 倍であり、フォルステライ
ト質の線膨張係数は地鉄のそれと比較的近い値を示し、
地鉄および被膜間に働く応力（熱応力）は小さいため、
被膜は地鉄との密着性に優れる特徴を有する。During the finish annealing, a ceramic coating is formed by the solid-phase reaction between the surface oxide layer after decarburization annealing and the annealing separating agent component. When the main component of the annealing separator is MgO, a forsterite glass film is formed.
The linear expansion coefficient of this forsterite coating is about 0.8 to 0.9 times that of the material for grain-oriented electrical steel, and the linear expansion coefficient of forsterite shows a value relatively close to that of base iron.
Since the stress (thermal stress) acting between the base iron and the coating is small,
The coating has a feature of excellent adhesion to the base steel.
【００２０】地鉄および被膜間に働く応力は、被膜形成
温度、被膜厚み、被膜の線膨張係数および弾性率などに
支配されるが、中でも被膜の線膨張係数の影響が大き
い。すなわち、地鉄の線膨張係数に比べて被膜の線膨張
係数を十分に小さくすると、地鉄および被膜間に働く応
力は増大し、被膜の剥離が容易になる。そこで、この発
明では、線膨張係数が地鉄のそれの0.5 倍以下の被膜を
仕上げ焼鈍中に形成し、該被膜を仕上げ焼鈍後期の降温
時に剥離させることによって、磁気特性を劣化すること
なしに被膜のない打ち抜き性に優れた方向性電磁鋼板の
製造を実現した。The stress acting between the base iron and the coating is governed by the coating forming temperature, the coating thickness, the linear expansion coefficient and the elastic modulus of the coating, and among others, the linear expansion coefficient of the coating has a great influence. That is, when the linear expansion coefficient of the coating is made sufficiently smaller than the linear expansion coefficient of the base iron, the stress acting between the base iron and the coating increases, and the coating peels off easily. Therefore, in the present invention, a film having a coefficient of linear expansion of 0.5 times or less that of that of base iron is formed during finish annealing, and the film is exfoliated at the time of lowering the temperature in the latter stage of finish annealing without deteriorating magnetic properties. We have achieved the production of grain-oriented electrical steel sheets with no coating and excellent punchability.
【００２１】特に、低熱膨張性のMg−Al−Si−Ｏ系シリ
ケート化合物、とりわけ４MgO ・５Al2O3 ・２SiO2、２
MgO ・２Al2O3 ・５SiO2またはMgO ・Al2O3 ・２SiO2な
どのMg−Al−Si−Ｏ系の低線膨張性シリケート化合物の
１種または２種以上の複合酸化物相で構成された被膜
が、有利に適合する。In particular, low thermal expansion Mg-Al-Si-O type silicate compounds, especially 4MgO.5Al 2 O 3 .2SiO 2 , 2
Composed of one or two or more composite oxide phase MgO · 2Al 2 O 3 · 5SiO 2 or MgO · Al 2 O 3 · 2SiO 2 Mg-Al-Si-O -based low thermal expansion silicate compounds, such as The applied coating is advantageously compatible.
【００２２】また、焼鈍分離剤には、 MgO：20wt％以
下、 Al2O3：20〜50wt％およびSiO2：30wt％以上の組成
に成るものを用いることが有利である。すなわち、図３
に示したように、 MgO含有量が20wt％をこえると、線膨
張係数の小さいシリケート化合物が生成する前に、脱炭
焼鈍により生成した酸化層中のSiO2と分離剤中のMgO と
の反応によりエンスタタイトの生成が促進され、被膜の
剥離性が劣化する。It is advantageous to use an annealing separator having a composition of MgO: 20 wt% or less, Al 2 O 3 : 20 to 50 wt% and SiO 2 : 30 wt% or more. That is, FIG.
As indicated, the reaction of the MgO content exceeds 20 wt%, before the small silicate compound coefficients of linear expansion is generated, the SiO 2 oxide layer produced by decarburization annealing and MgO in the separating agent This promotes the generation of enstatite and deteriorates the peelability of the coating.
【００２３】さらに、仕上げ焼鈍後の磁気特性は仕上げ
焼鈍途中での地鉄表面近傍のインヒビターの酸化分解お
よび窒化が過度に進行すると、２次再結晶不良を発生し
やすくなるため、図４に示したように、SiO2含有量を30
wt％以上にして地鉄の酸化及び窒化を抑制することが、
磁束密度を高める上で好ましい。ここで、磁束密度の高
まる理由は定かでないが、SiO2含有量を30wt％以上にす
ると、鋼板表面でのコーディライトやサフィリンの合成
が促進されて地鉄への酸素および窒素の拡散が減少し、
地鉄の酸化及び窒化が抑制されることによると考えられ
る。また、鋼板表面での被膜形成を促進させるために適
度な活性度を有するMgO を用いるが、このMgO 表面は M
g(OH)2化または H2O吸着が起こりやすい。従って、MgO
含有量を低減させると、コイル層間に持ち込まれる水分
量が低下されるため、磁気特性の向上に有効に作用する
と考えられる。Further, the magnetic properties after finish annealing are shown in FIG. 4 because secondary recrystallization failure is likely to occur when oxidative decomposition and nitridation of the inhibitor near the surface of the base iron during the finish annealing proceed excessively. The SiO 2 content of 30
Suppressing the oxidation and nitriding of the base iron by making it more than wt%,
It is preferable for increasing the magnetic flux density. Here, the reason why the magnetic flux density increases is not clear, but if the SiO 2 content is 30 wt% or more, the synthesis of cordierite and sapphirine on the surface of the steel sheet is promoted, and the diffusion of oxygen and nitrogen into the base iron is reduced. ,
It is considered that the oxidation and nitridation of base iron are suppressed. In addition, MgO, which has an appropriate degree of activity, is used to promote the formation of a film on the surface of the steel sheet.
G (OH) 2 conversion or H 2 O adsorption is likely to occur. Therefore, MgO
It is considered that when the content is reduced, the amount of water brought in between the coil layers is reduced, so that the magnetic properties are effectively improved.
【００２４】なお、この発明で対象とする電磁鋼板用素
材の代表組成は、以下の通りである。 Ｃ：0.02〜0.10wt％ Ｃは組織の改善を図るもので、この範囲を外れると良好
な集合組織が形成されない。 Si： 2.0〜4.5 wt％ Si含有量が 2.0wt％未満では、渦電流損失の低減効果が
減少し、一方4.5 wt％をこえると、冷間圧延性が損なわ
れる。これらの成分の他に、インヒビター構成元素を含
有する。すなわち、インヒビターにMnS および／または
MnSeを用いる場合は、Mn：0.03〜0.10wt％、Ｓ＋Se：0.
01〜0.03wt％にする。AlN をインヒビターに用いる場合
は、Al：0.01〜0.04wt％、Ｎ：0.00050 〜0.00120 wt％
とする。この範囲よりも低い含有量ではインヒビターと
して効果が不十分であり、高いと２次再結晶が不安定に
なる。また、これらの他にCu, Sn, Cr, Sb, Ge, Mo, T
e, Bi, Ｐ，Ｖなども適用することができ、さらに各イ
ンヒビターは単独使用、複数使用のいずれも可能であ
る。The representative composition of the electromagnetic steel sheet material targeted by the present invention is as follows. C: 0.02 to 0.10 wt% C aims to improve the structure, and if it is out of this range, a good texture is not formed. Si: 2.0 to 4.5 wt% When the Si content is less than 2.0 wt%, the effect of reducing the eddy current loss decreases, while when it exceeds 4.5 wt%, the cold rolling property is impaired. In addition to these components, it contains an inhibitor constituent element. That is, the inhibitor is MnS and / or
When using MnSe, Mn: 0.03 to 0.10 wt%, S + Se: 0.
01 to 0.03 wt% When AlN is used as an inhibitor, Al: 0.01 to 0.04 wt%, N: 0.00050 to 0.00120 wt%
And If the content is lower than this range, the effect as an inhibitor is insufficient, and if it is higher than the range, secondary recrystallization becomes unstable. In addition to these, Cu, Sn, Cr, Sb, Ge, Mo, T
e, Bi, P, V and the like can also be applied, and each inhibitor can be used alone or in combination.
【００２５】上記の電磁鋼板用素材に、公知の方法で熱
間圧延を行ったあと、１回もしくは中間焼鈍をはさむ複
数回の冷間圧延を施して最終板厚とする。また、必要に
応じて冷間圧延の間に焼鈍を行うことも可能である。次
いで、最終冷延板を脱炭焼鈍し、この発明に従う焼鈍分
離剤を塗布したのち、仕上げ焼鈍を施す。なお、仕上げ
焼鈍後の鋼板に対して、無機、半有機または有機コーテ
ィングを施しても良い。The above electromagnetic steel sheet material is hot-rolled by a known method and then cold-rolled once or a plurality of times with intermediate annealing to obtain a final sheet thickness. Moreover, it is also possible to perform annealing during cold rolling if necessary. Next, the final cold-rolled sheet is decarburized and annealed according to the present invention, and then finish annealing is applied. It should be noted that the steel sheet after finish annealing may be subjected to inorganic, semi-organic or organic coating.
【００２６】実施例１ Ｃ：0.06wt％、Si：3.28wt％、Mn：0.07wt％、Se：0.02
wt％、Sb：0.03wt％を含み、残部実質Feよりなるスラブ
を1400℃に加熱してから熱間圧延によって2.2mm 厚と
し、次に1050℃×２分間の中間焼鈍をはさんだ冷間圧延
によって、最終板厚0.23mmに仕上げた。この冷延板に、
脱炭焼鈍後、焼鈍分離剤として表２に示す組成の焼鈍分
離剤をコーターロールにて塗布、そして乾燥し、仕上げ
焼鈍として850℃×50ｈの保定焼鈍に引き続き乾水素雰
囲気で1150℃×５ｈの純化焼鈍を行った。Example 1 C: 0.06 wt%, Si: 3.28 wt%, Mn: 0.07 wt%, Se: 0.02
wt%, Sb: 0.03wt%, the remaining slab consisting essentially of Fe is heated to 1400 ℃ and hot-rolled to a thickness of 2.2mm, then cold-rolled with intermediate annealing at 1050 ℃ for 2 minutes. The final plate thickness was 0.23 mm. On this cold rolled sheet,
After decarburization annealing, an annealing separator having the composition shown in Table 2 as an annealing separator is applied by a coater roll and dried, and then a final annealing is performed at a constant annealing temperature of 850 ° C x 50h, followed by a dry hydrogen atmosphere at 1150 ° C x 5h. Purification annealing was performed.
【００２７】かくして得られた鋼板の磁気特性および打
ち抜き性について調査した結果を、表２に併せて示す。
なお、打ち抜き性は、ダイス径５ｍｍφのスチールダイ
スにより打抜作業を行った際に、反り高さが５０μｍに
達するまでの打抜回数で評価した。Table 2 also shows the results of an examination of the magnetic properties and punching properties of the thus obtained steel sheet.
The punchability was evaluated by the number of punches until the warp height reached 50 μm when punching was performed with a steel die having a die diameter of 5 mmφ.
【００２８】[0028]
【表２】 [Table 2]
【００２９】実施例２ Ｃ：0.07wt％、Si：3.30wt％、Mn：0.07wt％、Se：0.02
wt％、Sb： 0.025wt％、Al：0.025 wt％、Ｎ：0.0085wt
％、Cu：0.08wt％を含み、残部実質Feよりなるスラブを
1420℃に加熱してから熱間圧延によって2.2mm 厚とし、
1050℃×２分間の中間焼鈍をはさんだ冷間圧延によっ
て、最終板厚0.23mmに仕上げた。この冷延板に、脱炭焼
鈍後、表３に示す焼鈍分離剤を塗布し、仕上げ焼鈍とし
て 850℃×50ｈの保定焼鈍に引き続き乾水素雰囲気で12
00℃×５ｈの純化焼鈍を施した。なお、900 ℃〜1150℃
の間の仕上げ焼鈍は、 N2(25％) ＋H2 (75％) の混合雰
囲気で行った。かくして得られた鋼板の磁気特性および
打ち抜き性について調査した結果を、表３に併せて示
す。Example 2 C: 0.07 wt%, Si: 3.30 wt%, Mn: 0.07 wt%, Se: 0.02
wt%, Sb: 0.025 wt%, Al: 0.025 wt%, N: 0.0085 wt
%, Cu: 0.08wt%, the balance is made of Fe.
After heating to 1420 ℃, hot rolling to 2.2mm thickness,
The final plate thickness was 0.23 mm by cold rolling with intermediate annealing at 1050 ° C for 2 minutes. After decarburizing and annealing, the cold-rolled sheet was coated with the annealing separator shown in Table 3, and the final annealing was carried out in a dry hydrogen atmosphere at a fixed annealing of 850 ° C x 50h.
Purification annealing was performed at 00 ° C for 5 hours. 900 ℃ ~ 1150 ℃
The finish annealing during the period was performed in a mixed atmosphere of N 2 (25%) + H 2 (75%). Table 3 also shows the results of an examination of the magnetic properties and punching properties of the steel sheet thus obtained.
【００３０】[0030]
【表３】 [Table 3]
【００３１】[0031]
【発明の効果】この発明は、仕上げ焼鈍過程での酸化に
よる表層インヒビターの分解消失や鋼板の窒化による地
鉄表層近傍の窒化物析出を仕上焼鈍途中に形成される被
膜により抑制し、しかも形成された被膜を仕上焼鈍降温
時に鋼板から剥離させるようにしたから、磁気特性およ
び打ち抜き性に共に優れた電磁鋼板を製造できる。The present invention suppresses the decomposition and disappearance of the surface layer inhibitor due to the oxidation in the finish annealing process and the precipitation of nitrides in the vicinity of the surface layer of the base iron due to the nitriding of the steel sheet by the film formed during the finish annealing, and moreover, it is formed. Since the above coating is peeled off from the steel sheet during finish annealing and cooling, it is possible to manufacture an electromagnetic steel sheet excellent in both magnetic properties and punchability.
【図面の簡単な説明】[Brief description of drawings]
【図１】焼鈍分離剤の組成を示す図である。FIG. 1 is a diagram showing a composition of an annealing separator.
【図２】鋼板表面の酸素目付量と被膜の線膨張係数との
関係を示す図である。FIG. 2 is a diagram showing a relationship between an oxygen basis weight of a steel sheet surface and a linear expansion coefficient of a coating.
【図３】被膜組成と鋼板表面状態との関係を示す図であ
る。FIG. 3 is a diagram showing a relationship between a coating composition and a steel plate surface state.
【図４】被膜組成と磁束密度との関係を示す図である。FIG. 4 is a diagram showing a relationship between a coating composition and a magnetic flux density.
【図５】被膜の組成を示す図である。FIG. 5 is a diagram showing a composition of a coating film.
Claims (4)
圧延を施して最終板厚に仕上げ、次いで湿水素中にて脱
炭焼鈍を施して鋼板表面に酸化層を形成したのち、焼鈍
分離剤を塗布してから仕上げ焼鈍を行う一連の工程にて
方向性電磁鋼板を製造するに当たり、 該仕上げ焼鈍中に線膨張係数が含けい素鋼素材の0.5 倍
以下のセラミック質被膜を形成し、引き続く仕上げ焼鈍
後期の降温時に被膜と素材との間に生じる熱応力により
被膜を剥離させることを特徴とする打ち抜き性および磁
気特性の優れた方向性電磁鋼板の製造方法。1. A silicon-containing steel material is hot-rolled and cold-rolled to a final thickness, and then decarburized and annealed in wet hydrogen to form an oxide layer on the surface of the steel sheet. In the production of grain-oriented electrical steel sheets in a series of processes in which an annealing separator is applied and then final annealing is performed, a ceramic coating having a linear expansion coefficient of 0.5 times or less that of a silicon steel material is formed during the final annealing. Then, a method for producing a grain-oriented electrical steel sheet having excellent punchability and magnetic properties, characterized in that the coating film is peeled off by a thermal stress generated between the coating film and the raw material at the time of subsequent lowering of temperature during finish annealing.
Al−Si−Ｏ系シリケート化合物からなる請求項１に記載
の製造方法。2. The ceramic coating has a low thermal expansion of Mg--
The production method according to claim 1, comprising an Al-Si-O-based silicate compound.
・２SiO2、２MgO ・２Al2O3 ・５SiO2または MgO・Al2O
3 ・２SiO2である請求項１または２に記載の製造方法。3. The ceramic coating is 4MgO.5Al 2 O 3
· 2SiO 2, 2MgO · 2Al 2 O 3 · 5SiO 2 or MgO · Al 2 O
3. The manufacturing method according to claim 1, which is 3 · 2SiO 2 .
wt％部を含み残部がSiO2の組成になる焼鈍分離剤を用い
る請求項１に記載の製造方法。4. MgO: 10 to 20 wt% and Al 2 O 3 : 20 to 50
The manufacturing method according to claim 1, wherein an annealing separating agent having a composition of wt% and a balance of SiO 2 is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14165295A JP3197791B2 (en) | 1995-06-08 | 1995-06-08 | Method for producing grain-oriented electrical steel sheet with excellent punchability and magnetic properties |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14165295A JP3197791B2 (en) | 1995-06-08 | 1995-06-08 | Method for producing grain-oriented electrical steel sheet with excellent punchability and magnetic properties |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08337823A true JPH08337823A (en) | 1996-12-24 |
| JP3197791B2 JP3197791B2 (en) | 2001-08-13 |
Family
ID=15297033
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14165295A Expired - Fee Related JP3197791B2 (en) | 1995-06-08 | 1995-06-08 | Method for producing grain-oriented electrical steel sheet with excellent punchability and magnetic properties |
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| Country | Link |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100481368B1 (en) * | 2000-09-01 | 2005-04-07 | 주식회사 포스코 | A method for manufacturing low temperature reheated grain-oriented electrical steel sheet having superior punching property |
| JP2018090852A (en) * | 2016-12-01 | 2018-06-14 | Ｊｆｅスチール株式会社 | Production method of directional electromagnetic steel sheet |
| CN109112395A (en) * | 2018-08-10 | 2019-01-01 | 全球能源互联网研究院有限公司 | Ultra-thin band base material of a kind of no bottom orientation and preparation method thereof |
| JP2020509216A (en) * | 2016-12-22 | 2020-03-26 | ポスコＰｏｓｃｏ | Annealing separator composition for grain-oriented electrical steel sheet, grain-oriented electrical steel sheet, and method for producing grain-oriented electrical steel sheet |
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1995
- 1995-06-08 JP JP14165295A patent/JP3197791B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100481368B1 (en) * | 2000-09-01 | 2005-04-07 | 주식회사 포스코 | A method for manufacturing low temperature reheated grain-oriented electrical steel sheet having superior punching property |
| JP2018090852A (en) * | 2016-12-01 | 2018-06-14 | Ｊｆｅスチール株式会社 | Production method of directional electromagnetic steel sheet |
| JP2020509216A (en) * | 2016-12-22 | 2020-03-26 | ポスコＰｏｓｃｏ | Annealing separator composition for grain-oriented electrical steel sheet, grain-oriented electrical steel sheet, and method for producing grain-oriented electrical steel sheet |
| US11773462B2 (en) | 2016-12-22 | 2023-10-03 | Posco Co., Ltd | Annealing separator composition for grain-oriented electrical steel sheet, grain-oriented electrical steel sheet, and method for producing grain-oriented electrical steel sheet |
| CN109112395A (en) * | 2018-08-10 | 2019-01-01 | 全球能源互联网研究院有限公司 | Ultra-thin band base material of a kind of no bottom orientation and preparation method thereof |
| CN109112395B (en) * | 2018-08-10 | 2020-02-07 | 全球能源互联网研究院有限公司 | Non-bottom-layer oriented ultrathin strip base material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| JP3197791B2 (en) | 2001-08-13 |
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