JP3272210B2 - Method for forming insulating film on unidirectional silicon steel sheet - Google Patents
Method for forming insulating film on unidirectional silicon steel sheetInfo
- Publication number
- JP3272210B2 JP3272210B2 JP23501495A JP23501495A JP3272210B2 JP 3272210 B2 JP3272210 B2 JP 3272210B2 JP 23501495 A JP23501495 A JP 23501495A JP 23501495 A JP23501495 A JP 23501495A JP 3272210 B2 JP3272210 B2 JP 3272210B2
- Authority
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- Japan
- Prior art keywords
- steel sheet
- insulating film
- film
- silicon steel
- tension
- 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.)
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- Chemical Treatment Of Metals (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【発明の属する技術分野】本発明はフォルステライト
（Ｍｇ2 ＳｉＯ4 ）等の無機鉱物質皮膜の生成を意図的
に防止して製造した仕上げ焼鈍済みの一方向性珪素鋼板
や、フォルステライト等の無機鉱物質皮膜を酸洗等の手
段で除去したり、さらには鏡面ないしはそれに近い状態
に調製した仕上げ焼鈍済みの一方向性珪素鋼板に対し、
良好な鉄損を得ることができるよう張力付与型の絶縁性
皮膜を形成する方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a finish-annealed unidirectional silicon steel sheet manufactured by intentionally preventing the formation of an inorganic mineral film such as forsterite (Mg 2 SiO 4 ), and forsterite. The inorganic mineral film is removed by means such as pickling or the like, and the finish-annealed unidirectional silicon steel sheet prepared to a mirror surface or a state close to it is
The present invention relates to a method for forming a tension-imparting insulating film so that good iron loss can be obtained.
【０００２】[0002]
【従来の技術】一方向性珪素鋼板は磁気鉄芯材料として
多用されており、特にエネルギーロスを少なくするため
に鉄損の少ない材料が求められている。この鉄損の低減
には鋼板に張力を付与することが有効であることから、
鋼板に比べ熱膨張係数の小さい材質からなる皮膜を高温
で形成することによって鋼板に張力を付与し、鉄損低減
が図られてきた。仕上げ焼鈍工程で鋼板表面の酸化物と
焼鈍分離剤とが反応して生成するフォルステライト系皮
膜は、鋼板に張力を与えることができ、皮膜密着性も優
れている。2. Description of the Related Art A grain-oriented silicon steel sheet is widely used as a magnetic iron core material. In particular, a material having a small iron loss is required to reduce energy loss. Since it is effective to apply tension to the steel sheet to reduce this iron loss,
By forming a film made of a material having a smaller coefficient of thermal expansion than a steel sheet at a high temperature, tension has been applied to the steel sheet to reduce iron loss. The forsterite-based coating formed by the reaction between the oxide on the steel sheet surface and the annealing separator in the finish annealing step can give tension to the steel sheet and has excellent coating adhesion.
【０００３】さらに、特開昭４８−３９３３８号公報で
開示されたコロイド状シリカとリン酸塩を主体とするコ
ーティング液を焼き付けることによって絶縁皮膜を形成
する方法は、鋼板に対する張力付与の効果が大きく、鉄
損低減に有効である。したがって、仕上げ焼鈍工程で生
じたフォルステライト系皮膜を残した上で、リン酸塩を
主体とする絶縁皮膜を形成することが一般的な一方向性
珪素鋼板の製造方法となっている。Furthermore, the method of forming an insulating film by baking a coating solution mainly composed of colloidal silica and phosphate disclosed in Japanese Patent Application Laid-Open No. 48-39338 has a large effect of imparting tension to a steel sheet. It is effective for reducing iron loss. Therefore, it is a general method of manufacturing a unidirectional silicon steel sheet to form a phosphate-based insulating film while leaving the forsterite-based film generated in the finish annealing step.
【０００４】一方、近年、フォルステライト系皮膜と地
鉄の乱れた界面構造が、鉄損に対する皮膜張力効果をあ
る程度減少させていることが明らかになってきた。そこ
で、例えば、特開昭４９−９６９２０号公報に開示され
ている如く、仕上げ焼鈍工程で生ずるフォルステライト
系皮膜を除去したり、さらに鏡面化仕上げを行った後、
改めて張力皮膜を形成させることにより、さらなる鉄損
低減を試みる技術が開発された。On the other hand, in recent years, it has become clear that the disordered interface structure between the forsterite-based coating and the ground iron reduces the effect of the coating tension on iron loss to some extent. Therefore, for example, as disclosed in Japanese Patent Application Laid-Open No. 49-96920, after removing a forsterite-based film generated in a finish annealing step or further performing a mirror finish,
A technique was developed to try to further reduce iron loss by forming a tension film again.
【０００５】しかしながら、上記絶縁皮膜はフォルステ
ライトを主体とする皮膜の上に形成した場合は、かなり
の皮膜密着性が得られるものの、フォルステライト系皮
膜を除去したり、あるいは仕上げ焼鈍工程で意図的にフ
ォルステライト形成を行わなかったものに対しては皮膜
密着性が十分ではない。However, when the above-mentioned insulating film is formed on a film mainly composed of forsterite, a considerable film adhesion can be obtained, but the forsterite-based film is removed or intentionally applied in a finish annealing step. On the other hand, if the forsterite was not formed, the film adhesion was not sufficient.
【０００６】フォルステライト系皮膜の除去を行った場
合は、コーティング液を塗布して形成させる張力付与型
絶縁皮膜のみで所要の皮膜張力を確保する必要があり、
必然的に厚膜化しなければならず、より一層の密着性が
必要である。[0006] When the forsterite-based film is removed, it is necessary to secure a required film tension only with a tension-imparting insulating film formed by applying a coating liquid.
Inevitably, the film thickness must be increased, and further adhesion is required.
【０００７】したがって、従来の皮膜形成法では鏡面化
の効果を十分に引き出すほどの皮膜張力を達成すること
は困難であり、十分な鉄損低減が図られていなかった。
そこで、特開平５−２８７５４６号公報において、鋼板
表面にフォルステライト系皮膜のない一方向性珪素鋼板
に対し、リン酸塩とコロイド状シリカを主成分とするコ
ーティング液の塗布、焼き付けを行う際の雰囲気に水素
を含有させ、張力付与型の絶縁皮膜を形成させる方法が
開示された。[0007] Therefore, it is difficult to achieve a film tension sufficient to bring out the effect of mirror finishing by the conventional film forming method, and a sufficient reduction in iron loss has not been achieved.
Therefore, Japanese Patent Application Laid-Open No. 5-287546 discloses a method for applying and baking a coating liquid containing phosphate and colloidal silica as a main component to a unidirectional silicon steel sheet having no forsterite coating on the steel sheet surface. A method has been disclosed in which hydrogen is contained in an atmosphere to form a tension-imparting insulating film.
【０００８】[0008]
【発明が解決しようとする課題】しかしながら、特開平
５−２８７５４６号公報において開示された技術につい
ては次に述べるような問題点があった。該公報には絶縁
皮膜の焼き付けを行う雰囲気中に水素を含有させること
によって、皮膜密着性が確保できることが述べられてい
る。この方法によって皮膜密着性はそれなりに改善され
る。しかしながら、焼き付け雰囲気中の水素分圧を制御
しただけでは安定した鉄損低減効果が得られないという
問題点があった。However, the technique disclosed in Japanese Patent Application Laid-Open No. 5-287546 has the following problems. The publication states that the film adhesion can be ensured by incorporating hydrogen into the atmosphere in which the insulating film is baked. This method improves the film adhesion to some extent. However, there is a problem that a stable iron loss reduction effect cannot be obtained only by controlling the hydrogen partial pressure in the baking atmosphere.
【０００９】[0009]
【課題を解決するための手段】本発明は上述の問題点を
解決し、無機鉱物質皮膜のない仕上げ焼鈍済みの一方向
性珪素鋼板に対し、良好な鉄損を得ることができるよう
に張力付与型の絶縁性皮膜を形成させる方法である。DISCLOSURE OF THE INVENTION The present invention solves the above-mentioned problems, and provides a tension-strength so that a good iron loss can be obtained for a finish-annealed unidirectional silicon steel sheet having no inorganic mineral substance film. This is a method of forming an application type insulating film.
【００１０】本発明の要旨は次の通りである。 （１）鋼板表面に無機鉱物質皮膜のない仕上げ焼鈍済み
一方向性珪素鋼板にコーティング液を塗布し、焼き付け
ることによって非晶質主体の張力付与型絶縁皮膜を形成
する方法において、コーティング液の焼き付けを行う雰
囲気のＰ H2 O／Ｐ H2 （Ｐ H2 O ，Ｐ H2 はそれぞれ
雰囲気中の水蒸気分圧と水素分圧）を１０-2以上として
鋼板と張力付与型絶縁皮膜との間に生ずる界面荒れを防
止することを特徴とする一方向性珪素鋼板の絶縁皮膜形
成方法。 （２）張力付与型の絶縁皮膜を形成させるコーティング
液がリン酸塩とコロイド状シリカを主体とすることを特
徴とする（１）に記載の一方向性珪素鋼板の絶縁皮膜形
成方法。The gist of the present invention is as follows. (1) A method of applying a coating liquid to a finish-annealed unidirectional silicon steel sheet having no inorganic mineral substance film on the surface of the steel sheet and baking the coated liquid to form an amorphous-based tension-imparting insulating film, and baking the coating liquid. P H 2 O / P H 2 atmosphere to perform between the (P H 2 O, P H 2 are each steam partial pressure and hydrogen partial pressure in the atmosphere) steel sheet and the tension-imparting insulating coating as 10 -2 A method for forming an insulating film on a grain-oriented silicon steel sheet, characterized by preventing roughening of an interface generated in the steel sheet. (2) The method for forming an insulating film on a unidirectional silicon steel sheet according to (1), wherein the coating liquid for forming the tension imparting type insulating film is mainly composed of phosphate and colloidal silica.
【００１１】以下、発明の詳細について説明する。発明
者らは鉄損値に対し、雰囲気中の水素分圧（Ｐ H2 ）だ
けでなく水蒸気分圧（Ｐ H2 O)も影響するのではないか
と予想した。そこで、次のような手順で検討を行い、鉄
損値に対する焼き付け雰囲気（Ｐ H2 O ／Ｐ H2 ）の影
響を調べた。まず、仕上げ焼鈍済みの一方向性珪素鋼板
の表面に生成しているフォルステライト系皮膜を酸洗に
よって除去し、さらに化学研磨を施すことによって表面
を鏡面化した。The details of the present invention will be described below. The inventors expected that not only the hydrogen partial pressure (P H 2 ) in the atmosphere but also the water vapor partial pressure (P H 2 O) would affect the iron loss value. Therefore, the following procedure was used to examine the effect of the baking atmosphere (P H 2 O / P H 2 ) on the iron loss value. First, the forsterite-based film formed on the surface of the finish-annealed unidirectional silicon steel sheet was removed by pickling, and the surface was mirror-finished by chemical polishing.
【００１２】次に、この鋼板に対し、リン酸アルミニウ
ムとコロイド状シリカを主成分とするコーティング液を
塗布し、８５０℃で１２０秒間焼き付けし、非晶質の張
力付与型絶縁皮膜を形成させた。この焼き付けの際、雰
囲気中のＰ H2 O とＰ H2 の両方を調整した。最後に、
皮膜付き試料の鉄損値を測定した。Next, a coating solution containing aluminum phosphate and colloidal silica as main components was applied to the steel sheet and baked at 850 ° C. for 120 seconds to form an amorphous tension-imparting insulating film. . During this baking was adjusted both P H 2 O and P H 2 in the atmosphere. Finally,
The iron loss value of the sample with the film was measured.
【００１３】結果をまとめたものが図１である。図１か
ら低い鉄損値を得るためには焼き付け雰囲気のＰ H2 O
／Ｐ H2 を１０-2以上にした時、低い（優れた）鉄損値
を得ることができることがわかる。FIG. 1 summarizes the results. P H 2 O of the baking atmosphere to obtain a low iron loss value from 1
When / P H 2 is 10 −2 or more, a low (excellent) iron loss value can be obtained.
【００１４】なお、鉄損値の測定はレーザー照射法によ
る磁区制御処理を施し、かつ磁束密度（一般にＢ8 で代
表される）が１．９３テスラ前後の試料について行っ
た。一般に、一方向性珪素鋼板の鉄損値は試料の磁区の
大きさと磁束密度の影響を受ける。そのため、磁区制御
を施し磁区の大きさが等しく、かつ磁束密度についても
ほぼ同じ値の試料について鉄損値を測定し比較した。こ
れによって鉄損値に対する焼き付け雰囲気のＰ H2 O ／
Ｐ H2 の影響のみを抽出できる。[0014] The measurement of the iron loss is subjected to a magnetic domain control treatment by laser irradiation, and (represented generally at B 8) the magnetic flux density was performed on 1.93 Tesla before and after the sample. Generally, the iron loss value of a unidirectional silicon steel sheet is affected by the size of the magnetic domain and the magnetic flux density of the sample. Therefore, magnetic domain control was performed, and iron loss values were measured and compared for samples having the same magnetic domain size and substantially the same magnetic flux density. As a result, the baking atmosphere PH 2 O /
Only the effect of P H 2 can be extracted.
【００１５】[0015]
【発明の実施の形態】本発明における張力付与型の絶縁
皮膜はその大部分が非晶質である。発明者らは皮膜の非
晶質状態に対して焼き付け雰囲気のＰ H2 O ／Ｐ H2 が
次のように作用するのではないかと推測している。Ｐ H
2 O ／Ｐ H2 が１０-2以上の雰囲気で焼き付けた場合、
皮膜は非晶質状態のまま一様に鋼板を被覆している。BEST MODE FOR CARRYING OUT THE INVENTION Most of the tension imparting type insulating film of the present invention is amorphous. The inventors presume that PH 2 O / P H 2 in the baking atmosphere acts on the amorphous state of the film as follows. PH
When baked in an atmosphere where 2 O / P H 2 is 10 -2 or more,
The coating uniformly covers the steel sheet in an amorphous state.
【００１６】ところが、Ｐ H2 O ／Ｐ H2 が１０-2未満
の雰囲気で焼き付けた場合、皮膜の一部が結晶化し微小
なクラックが入る。一旦、皮膜に微小なクラックが入る
とこのクラックを介して鋼板表面が雰囲気の影響を受
け、その結果ある種の界面荒れが発生し、良好な鉄損値
が得られないものと推測している。However, when the film is baked in an atmosphere where P H 2 O / P H 2 is less than 10 −2 , a part of the film is crystallized and minute cracks are formed. It is speculated that once a minute crack enters the film, the surface of the steel sheet is affected by the atmosphere through the crack, and as a result, some kind of interface roughness occurs, and a good iron loss value cannot be obtained. .
【００１７】[0017]
【実施例】Ｓｉを３．２５％含有する最終板厚０．２３
mmに冷間圧延された珪素鋼板に対し、脱炭焼鈍を行っ
た。この時、鋼板表面にはＳｉＯ2 を含む酸化層が形成
される。ついで、この鋼板に対し、ＭｇＯを主体とする
焼鈍分離剤を塗布し、最終仕上げ焼鈍を行った。このよ
うにして焼鈍した一方向性珪素鋼板表面にはフォルステ
ライトを主体とする皮膜が存在している。[Example] Final plate thickness 0.23 containing 3.25% of Si
A decarburizing annealing was performed on the silicon steel sheet cold-rolled to the mm. At this time, an oxide layer containing SiO 2 is formed on the surface of the steel sheet. Next, an annealing separator mainly composed of MgO was applied to the steel sheet, and final finishing annealing was performed. A coating mainly composed of forsterite exists on the surface of the annealed silicon steel sheet thus annealed.
【００１８】このフォルステライト系皮膜付きの鋼板を
硫酸とフッ化アンモニウムの水溶液に浸漬することによ
りフォルステライト系皮膜を除去し、さらにフッ酸と過
酸化水素の混合水溶液中で化学研磨し表面を鏡面状態に
仕上げた。The steel plate with the forsterite-based coating is immersed in an aqueous solution of sulfuric acid and ammonium fluoride to remove the forsterite-based coating, and further chemically polished in a mixed aqueous solution of hydrofluoric acid and hydrogen peroxide to obtain a mirror-finished surface. Finished in condition.
【００１９】次に、この鋼板表面に濃度２０％のコロイ
ド状シリカの懸濁液１００ml、濃度５０％のリン酸アル
ミニウム溶液１００ml、無水クロム酸５ｇからなるコー
ティング液を溝付きロールによって片面当たり９ｇ／ｍ
2 塗布し、水素５％、窒素９５％、露点−２０℃でＰ H
2 O ／Ｐ H2 が２．５×１０-2の雰囲気と水素７５％、
窒素２５％、露点−２０℃でＰ H2 O ／Ｐ H2 が０．２
×１０-2の雰囲気で８５０℃、１２０秒間焼き付け、リ
ン酸アルミニウムを主体とする皮膜を形成させた。最後
にレーザー照射法による磁区制御を施し、鉄損を測定し
た。Next, a coating solution consisting of 100 ml of a suspension of colloidal silica having a concentration of 20%, 100 ml of a solution of aluminum phosphate having a concentration of 50%, and 5 g of chromic anhydride was applied to the surface of the steel sheet by a grooved roll at a rate of 9 g / side. m
2 applied, hydrogen 5%, nitrogen 95%, dew point -20 ℃ PH
2 O / P H 2 atmosphere of 2.5 × 10 -2 and 75% hydrogen,
25% nitrogen, dew point -20 ° C, PH 2 O / P H 2 0.2
The film was baked at 850 ° C. for 120 seconds in an atmosphere of × 10 -2 to form a film mainly composed of aluminum phosphate. Finally, the magnetic domain was controlled by a laser irradiation method, and the iron loss was measured.
【００２０】結果を表１に示す。焼き付け雰囲気のＰ H
2 O ／Ｐ H2 が０．２×１０-2である比較例に比べ、焼
き付け雰囲気のＰ H2 O ／Ｐ H2 が２．５×１０-2であ
る本発明の方が鉄損値が低く優れている。本発明の一例
について説明したが、勿論本発明はかかる実施例に限定
されない。The results are shown in Table 1. Burning atmosphere PH
Compared with the comparative example in which 2 O / P H 2 is 0.2 × 10 −2 , the iron loss value of the present invention, in which the firing atmosphere PH 2 O / P H 2 is 2.5 × 10 −2 , is better But lower and better. Although an example of the present invention has been described, the present invention is, of course, not limited to such an embodiment.
【００２１】[0021]
【表１】 [Table 1]
【００２２】[0022]
【発明の効果】本発明によって界面荒れを起こさず、非
晶質の張力付与型絶縁皮膜を形成できるので、低い（優
れた）鉄損値を得ることができる。According to the present invention, an amorphous tension-imparting insulating film can be formed without causing interface roughness, so that a low (excellent) iron loss value can be obtained.
【図１】鉄損値に及ぼす張力付与型絶縁皮膜を焼き付け
る時の雰囲気のＰ H2 O ／Ｐ H2 の影響を示す図表であ
る。FIG. 1 is a chart showing the effect of P H 2 O / P H 2 in the atmosphere when baking a tension imparting type insulating film on an iron loss value.
フロントページの続き (72)発明者 牛神 義行 富津市新富20−１ 新日本製鐵株式会社 技術開発本部内 (56)参考文献 特開 平５−311353（ＪＰ，Ａ) 特開 平５−287546（ＪＰ，Ａ) 特開 平６−184762（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C23C 22/00 - 22/86 C21D 9/46 501 Continuation of the front page (72) Inventor Yoshiyuki Ushigami 20-1 Shintomi, Futtsu Nippon Steel Corporation Technology Development Division (56) References JP-A-5-311353 (JP, A) JP-A-5-287546 (JP, A) JP-A-6-184762 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C23C 22/00-22/86 C21D 9/46 501
Claims (2)
焼鈍済み一方向性珪素鋼板にコーティング液を塗布し、
焼き付けることによって非晶質主体の張力付与型絶縁皮
膜を形成する方法において、コーティング液の焼き付け
を行う雰囲気のＰ H2 O ／Ｐ H2 （Ｐ H2 O ，Ｐ H2 は
それぞれ雰囲気中の水蒸気分圧と水素分圧）を１０-2以
上として鋼板と張力付与型絶縁皮膜との間に生ずる界面
荒れを防止することを特徴とする一方向性珪素鋼板の絶
縁皮膜形成方法。1. A coating liquid is applied to a finish-annealed unidirectional silicon steel sheet having no inorganic mineral substance film on the steel sheet surface,
In a method of forming an amorphous-based tension-imparting insulating film by baking, PH 2 O / PH 2 (PH 2 O, PH 2 in the atmosphere in which the coating solution is baked is water vapor in the atmosphere, respectively). A method for forming an insulating film on a unidirectional silicon steel sheet, wherein the interface between the steel sheet and the tension-imparting insulating film is prevented from being roughened by setting the partial pressure and the hydrogen partial pressure to 10 -2 or more.
ティング液がリン酸塩とコロイド状シリカを主体とする
ことを特徴とする請求項１に記載の一方向性珪素鋼板の
絶縁皮膜形成方法。2. The method for forming an insulating film on a unidirectional silicon steel sheet according to claim 1, wherein the coating liquid for forming the tension imparting type insulating film is mainly composed of phosphate and colloidal silica.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23501495A JP3272210B2 (en) | 1995-09-13 | 1995-09-13 | Method for forming insulating film on unidirectional silicon steel sheet |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23501495A JP3272210B2 (en) | 1995-09-13 | 1995-09-13 | Method for forming insulating film on unidirectional silicon steel sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0978253A JPH0978253A (en) | 1997-03-25 |
| JP3272210B2 true JP3272210B2 (en) | 2002-04-08 |
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ID=16979800
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23501495A Ceased JP3272210B2 (en) | 1995-09-13 | 1995-09-13 | Method for forming insulating film on unidirectional silicon steel sheet |
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| JP4288054B2 (en) | 2002-01-08 | 2009-07-01 | 新日本製鐵株式会社 | Method for producing grain-oriented silicon steel sheet |
| WO2019155858A1 (en) * | 2018-02-06 | 2019-08-15 | Ｊｆｅスチール株式会社 | Electromagnetic steel sheet with insulating coating and production method therefor |
| JP7188458B2 (en) * | 2019-01-16 | 2022-12-13 | 日本製鉄株式会社 | Grain-oriented electrical steel sheet and manufacturing method thereof |
| JP7260798B2 (en) * | 2019-01-16 | 2023-04-19 | 日本製鉄株式会社 | Manufacturing method of grain-oriented electrical steel sheet |
| WO2021084793A1 (en) | 2019-10-31 | 2021-05-06 | Ｊｆｅスチール株式会社 | Electromagnetic steel sheet with insulation coating film |
| WO2023204267A1 (en) * | 2022-04-21 | 2023-10-26 | 日本製鉄株式会社 | Grain-oriented electromagnetic steel sheet and production method therefor |
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| JP2698501B2 (en) * | 1992-04-07 | 1998-01-19 | 新日本製鐵株式会社 | Method for forming insulating film on unidirectional silicon steel sheet |
| JP2698003B2 (en) * | 1992-08-25 | 1998-01-19 | 新日本製鐵株式会社 | Method for forming insulating film on unidirectional silicon steel sheet |
| JP2667082B2 (en) * | 1992-05-08 | 1997-10-22 | 新日本製鐵株式会社 | Ultra-low iron loss grain-oriented electrical steel sheet without glass coating and method for producing the same |
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| Publication number | Publication date |
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| JPH0978253A (en) | 1997-03-25 |
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