JPH05195239A - Pretreatment for uniform formation of insulating film on magnetic steel sheet - Google Patents
Pretreatment for uniform formation of insulating film on magnetic steel sheetInfo
- Publication number
- JPH05195239A JPH05195239A JP564492A JP564492A JPH05195239A JP H05195239 A JPH05195239 A JP H05195239A JP 564492 A JP564492 A JP 564492A JP 564492 A JP564492 A JP 564492A JP H05195239 A JPH05195239 A JP H05195239A
- Authority
- JP
- Japan
- Prior art keywords
- steel sheet
- annealing
- subscale
- pretreatment
- pickling
- 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
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14775—Fe-Si based alloys in the form of sheets
- H01F1/14783—Fe-Si based alloys in the form of sheets with insulating coating
Landscapes
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical Treatment Of Metals (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は電磁鋼板の製造方法に
関連し、とくに欠陥のない平滑かつ均一性に優れるフォ
ステライト絶縁被膜を安定的に形成させるための予備処
理方法を提案しようとするものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an electromagnetic steel sheet, and is intended to propose a pretreatment method for stably forming a forsterite insulating coating film which is smooth and has excellent uniformity without defects. Is.
【０００２】方向性電磁鋼板は変圧器などの積鉄心ある
いは巻鉄心として用いられるため、各層間の電気絶縁性
が保たれるように鋼板表面に電気絶縁被膜が被覆され
る。この絶縁被膜は、電気絶縁性、表面平滑性、占積率
など多くの要件のほかに、地鉄との密着性、外観的な均
一性を併せて満足することが要求される。Since the grain-oriented electrical steel sheet is used as a laminated iron core or a wound iron core of a transformer or the like, the surface of the steel sheet is coated with an electric insulating coating so that the electric insulation between layers can be maintained. In addition to many requirements such as electric insulation, surface smoothness, and space factor, this insulating coating is required to satisfy the adhesion to the base steel and the appearance uniformity.
【０００３】絶縁被膜の形成方法としては、一般に所望
の最終板厚に冷間圧延された含けい素鋼冷延板をサブス
ケール生成事前処理として脱脂洗浄後、湿水素雰囲気中
で700 〜900 ℃の温度範囲、数分間の連続脱炭焼鈍（１
次再結晶も兼ねる）を行うことにより、脱炭と同時に鋼
中のSiを酸化してSiO2を含む酸化膜（サブスケール）を
鋼板表面に生じさせ、このサブスケール上にMgO を主成
分とする焼鈍分離剤を塗布してコイル状に巻取り、これ
を水素気流中で1100〜1250℃の温度範囲の２次再結晶及
び純化焼鈍を行うことにより、上記SiO2とMgO とを反応
させて鋼板上に主としてフォルステライト（Mg2SiO4)か
らなるガラス状の薄い絶縁被膜（以下単に絶縁被膜とい
う）を形成させる。この方法によって工業的に得られる
絶縁被膜は必ずしも鋼板表面上に均一に形成されるとは
限らず、ときには地鉄との密着性の弱い部分や斑点状に
地鉄が裸出するような被膜欠陥をともなう場合がある。
これらの欠陥は電気絶縁性の低下をもたらし、変圧器用
鉄心にあっては渦電流が発生し所期の性能を発揮できな
くなる。As a method for forming an insulating coating, generally, a cold-rolled silicon-containing steel cold-rolled sheet having a desired final thickness is subjected to degreasing and washing as a subscale production pretreatment, and then in a wet hydrogen atmosphere at 700 to 900 ° C. Continuous decarburization annealing (1
By performing the second recrystallization as well), at the same time as decarburization, Si in the steel is oxidized to form an oxide film (subscale) containing SiO 2 on the surface of the steel sheet, and MgO is the main component on this subscale. The above-mentioned SiO 2 and MgO are reacted with each other by applying an annealing separating agent to be wound into a coil and performing secondary recrystallization and purification annealing in a temperature range of 1100 to 1250 ° C. in a hydrogen stream. A glass-like thin insulating film (hereinafter simply referred to as an insulating film) composed mainly of forsterite (Mg 2 SiO 4 ) is formed on a steel plate. Insulating coatings obtained industrially by this method are not always uniformly formed on the surface of the steel sheet, and sometimes coating defects such as bare spots of bare iron or spots with weak adhesion to the iron May be accompanied by.
These defects bring about a decrease in electrical insulation, and eddy currents are generated in the transformer core, so that desired performance cannot be achieved.
【０００４】したがって、方向性電磁鋼板の製造にあた
って、良好な特性を有する絶縁被膜を形成させることが
重要になる。Therefore, in the production of grain-oriented electrical steel sheet, it is important to form an insulating coating having good characteristics.
【０００５】[0005]
【従来の技術】前記したような欠陥を改善し、特性の良
好な絶縁被膜を形成させるためには、脱炭焼鈍において
欠陥のない均一なサブスケールを生成させること、また
そのためには冷間圧延後脱炭焼鈍前鋼板の表面状況すな
わち脱脂洗浄等のサブスケール生成事前処理が重要であ
ることが知られていてこれまでにも多くの提案がなされ
ている。2. Description of the Related Art In order to improve the above-mentioned defects and form an insulating film having good characteristics, it is necessary to form a uniform subscale without defects in decarburizing annealing, and for that purpose, cold rolling is required. It is known that the surface condition of the steel sheet before post-decarburization annealing, that is, the pre-scale generation pretreatment such as degreasing cleaning is important, and many proposals have been made so far.
【０００６】例えば、特公昭５３−２２５２９号公報に
方向性珪素鋼板の絶縁被膜形成方法が開示されている
が、この方法は脱炭焼鈍前に鋼板の表面層が３ｇ／m2以
上除去されるように酸洗するものであり、脱炭焼鈍前の
鋼板表面の有害な付着物除去に効果があり、それなりに
絶縁被膜の欠陥の改善に有効であるが、地鉄表面を３ｇ
／m2以上と多く溶失させるため、歩止り低下による経済
的損失が大きいこと（特に板厚が薄くなるとより顕著に
なる）、強酸洗を行うため鋼板表面の凹凸が大きくな
り、これが占積率に対し悪影響をおよぼすことなどの不
利があった。For example, Japanese Patent Publication No. 53-22529 discloses a method for forming an insulating coating on a grain-oriented silicon steel sheet. In this method, the surface layer of the steel sheet is removed by 3 g / m 2 or more before decarburization annealing. It is effective in removing harmful deposits on the surface of the steel sheet before decarburizing and annealing, and it is effective in improving the defects of the insulating coating.
/ M 2 or more, it causes a large economic loss due to a decrease in yield (particularly more noticeable when the plate thickness is thin). There were disadvantages such as having a negative effect on the rate.
【０００７】また、特公昭５８−４６５４７号公報に方
向性珪素鋼板の絶縁被膜形成方法として、脱炭焼鈍後の
鋼板表面に絶縁被膜の形成に有利に作用するサブスケー
ルを得るために、脱炭焼鈍前鋼板表面にSi化合物を付着
させる手段が開示されている。しかしながら、電磁鋼板
の製造工程における熱延板のスケール除去不良や、中間
焼鈍時鋼板表面に形成されるスケールすなわちSiO2やFe
2SiO4(ファイヤライト) などの膜が、冷間圧延時に粉砕
され一部は圧延中に脱落するものの他は表面に不均一に
残った状態の鋼板に、上記手段を適用することになるた
め、得られた絶縁被膜の平滑性、均一性に問題が生じ、
加えて、鋼板表面に残ったスケールが、脱脂工程で鋼板
表面に付着する脱脂液中のNa, Na化合物の付着量を増加
させる要因となりこのNa, Na化合物が絶縁被膜の欠陥発
生原因になるという問題があった。Further, as a method for forming an insulating coating on a grain-oriented silicon steel sheet in Japanese Patent Publication No. 58-46547, decarburization is performed in order to obtain a subscale that advantageously acts on the surface of the steel sheet after decarburization annealing. A means for depositing a Si compound on the surface of the steel sheet before annealing is disclosed. However, scale removal failure of hot-rolled sheet in the manufacturing process of electromagnetic steel sheet and scale formed on the steel sheet surface during intermediate annealing, that is, SiO 2 and Fe
2 film such as SiO 4 (fayalite) is, the steel sheet of the state portion are ground during cold rolling that remains uneven in addition the surface of which fall off during rolling, since the applying the above means , There is a problem in the smoothness and uniformity of the obtained insulating coating,
In addition, the scale remaining on the steel plate surface becomes a factor that increases the amount of Na and Na compounds in the degreasing liquid that adheres to the steel plate surface during the degreasing process, and this Na and Na compound causes defects in the insulating coating. There was a problem.
【０００８】さらに、特公昭６０−１４１０４号公報に
方向性けい素鋼板のフォルステライト絶縁被膜の形成方
法として、鋼板表面のブラッシングを強化する手段が、
特開昭６１−２８１８１６号公報に一方向性けい素鋼板
の製造方法として、鋼板表面を超音波洗浄する手段がそ
れぞれ開示されている。これらは共に脱炭焼鈍前の鋼板
表面の清浄度を向上させるものであるが、付着物の除去
効果はあるものの、これらの手段によっても前工程の変
動を完全に吸収しきれずに鋼板上のスケールを十分に除
去することが困難な場合があり、上記したようなスケー
ルの残存に加えて有害なNa, Na化合物の付着量が増加す
ることによる問題があった。Further, as a method for forming a forsterite insulating coating on grain-oriented silicon steel sheet, Japanese Patent Publication No. 60-14104 discloses a means for strengthening brushing on the steel sheet surface.
Japanese Unexamined Patent Publication No. 61-281816 discloses a method of ultrasonically cleaning the surface of a steel sheet as a method for producing a unidirectional silicon steel sheet. Both of these improve the cleanliness of the steel sheet surface before decarburization annealing, but although they have the effect of removing deposits, these measures do not completely absorb the fluctuations in the previous process, and the scale on the steel sheet cannot be completely absorbed. In some cases, it may be difficult to remove satisfactorily, and in addition to the above scale remaining, there is a problem due to an increase in the amount of harmful Na and Na compounds attached.
【０００９】[0009]
【発明が解決しようとする課題】この発明は、前記した
問題点を有利に解決しようとするものであり、欠陥のな
い均一かつ平滑な絶縁被膜を形成させるために、含けい
素鋼冷延板のサブスケール生成事前処理を適正化し脱炭
焼鈍により欠陥のない平滑なサブスケールが得られる電
磁鋼板絶縁被膜の均一形成用予備処理方法を提案するこ
とを目的とする。SUMMARY OF THE INVENTION The present invention is intended to advantageously solve the above-mentioned problems, and in order to form a uniform and smooth insulating coating free from defects, a cold rolled silicon steel sheet. It is an object of the present invention to propose a pretreatment method for uniform formation of electrical steel sheet insulating coatings by optimizing the subscale generation pretreatment of (1) and obtaining a smooth subscale without defects by decarburization annealing.
【００１０】[0010]
【課題を解決するための手段】この発明は、最終板厚に
冷間圧延した含けい素鋼板のサブスケール生成事前処理
として、脱脂後酸洗を施して鋼板上のスケールを除去
し、さらにSi化合物を鋼板表面に付着させるものであ
り、かくすることにより脱炭焼鈍で良好なサブスケール
が生成し、最終焼鈍で欠陥のない優れた特性を有する絶
縁被膜が得られることを見出したことによるものであ
る。As a pre-scale generation pretreatment of a silicon-containing silicon steel sheet cold-rolled to a final thickness, the present invention removes the scale on the steel sheet by performing pickling after degreasing and further removing Si. It is for adhering the compound to the surface of the steel sheet, and by doing so, it was found that a good subscale is generated by decarburizing annealing and an insulating coating having excellent properties without defects is obtained by final annealing. Is.
【００１１】すなわち、この発明の要旨は、含けい素鋼
冷延板にサブスケール生成事前処理を施してから脱炭・
１次再結晶焼鈍を行うに当り、該サブスケール事前処理
が、含けい素鋼冷延板を脱脂後、残留スケールを除去す
る酸洗を行い、つづいてSi化合物の付着処理を施すこと
から成る電磁鋼板絶縁被膜の均一形成用予備処理方法で
あり、さらにサブスケール生成事前処理と脱炭焼鈍とを
連続して行うものである。That is, the gist of the present invention is to decarburize a silicon-containing cold-rolled steel sheet after subjecting it to a subscale generation pretreatment.
In carrying out the primary recrystallization annealing, the subscale pretreatment consists of degreasing the silicon steel cold-rolled sheet, followed by pickling to remove residual scale, and then applying a Si compound adhesion treatment. This is a pretreatment method for uniform formation of an electrical steel sheet insulating coating, and further performs subscale generation pretreatment and decarburization annealing successively.
【００１２】ここに、鋼板表面に付着させるSi化合物と
は、オルトけい酸（H4SiO4）、メタけい酸（H2SiO3) 、
コロイダルシリカの如き水溶状超微粒SiO2及びけい酸ア
ルカリ水溶液中で電解処理したときに鋼板に電着するSi
O2またはこれにH2O が結合した化合物等をいう。The Si compound attached to the surface of the steel sheet is orthosilicic acid (H 4 SiO 4 ), metasilicic acid (H 2 SiO 3 ),
Si electrodepositing the steel plate when electrolytic treatment with colloidal silica such as water-like ultra fine SiO 2 and silicates alkaline aqueous solution of
O 2 or a compound in which H 2 O is bound to O 2 or the like.
【００１３】[0013]
【作用】この発明をさらに詳しく以下に述べる。この発
明は、最終板厚に冷間圧延した鋼板の脱炭焼鈍前のサブ
スケール生成事前処理として、まず、脱脂して鋼板上に
付着している圧延油などを除去してつぎの酸洗を容易に
し、酸洗によりスケールを除去したのちサブスケールの
形成に有利に作用するSi化合物を鋼板表面に付着させる
ものであり、このような処理を行うことにより脱炭焼鈍
で欠陥のない均一なサブスケールが得られ、さらにその
後の焼鈍分離剤の塗布につづく最終焼鈍により欠陥のな
い均一かつ平滑な絶縁被膜を得るものである。The present invention will be described in more detail below. This invention is a subscale generation pretreatment before decarburization annealing of a steel plate cold-rolled to the final plate thickness, first, degreasing and removing rolling oil and the like adhering to the steel plate, and then the next pickling. It facilitates and removes the scale by pickling, and then deposits a Si compound that has an advantageous effect on the formation of the subscale on the surface of the steel sheet. A scale is obtained, and further a final annealing subsequent to the application of the annealing separator is followed to obtain a defect-free uniform and smooth insulating coating.
【００１４】この発明において、酸洗前に脱脂を行うの
は、圧延油など油分の付着した鋼板をそのまま酸洗する
と均一に酸洗することが困難なためであり、また酸洗後
Si化合物を付着させるのは、Si化合物が単に脱炭焼鈍で
のサブスケールの生成に有利に作用すること以外に、Si
化合物を付着させることにより、その前工程の酸洗で強
酸洗を行わなくても欠陥のない均一なサブスケールを得
ることができ、ひいては良好な絶縁被膜が得られること
によるものである。In the present invention, degreasing is performed before pickling because it is difficult to pickle a steel sheet having oil content such as rolling oil as it is, and after pickling.
The deposition of Si compound is because the Si compound does not only favor the subscale formation during decarburization annealing,
This is because by adhering the compound, it is possible to obtain a uniform subscale without defects even if strong pickling is not carried out in the pickling in the previous step, and thus a good insulating film can be obtained.
【００１５】このように酸洗後Si化合物を付着させるこ
とにより、前記した特公昭５３−２２５２９号公報の場
合のような強酸洗を必要としなくなり弱酸洗ですむこと
から、酸洗によって前記したような歩止りの低下、占積
率に影響する鋼板表面の凹凸の発生を抑制することがで
きる。By thus adhering the Si compound after pickling, the strong pickling as in the case of Japanese Patent Publication No. 53-22529 is no longer necessary, and only weak pickling is required. It is possible to suppress the occurrence of irregularity on the surface of the steel sheet, which may cause a decrease in the yield and to affect the space factor.
【００１６】また、脱脂及びSi化合物を付着させる際
に、絶縁被膜の形成に有害なNa及びNa化合物が、酸化膜
の割れ目に残留したり、酸洗不良により鋼板上に残った
酸化物などの汚物と一緒になって残留したりするが、上
記のように脱脂後酸洗することによりスケールが除去さ
れるためその付着量が減少し、その後のサブスケール生
成及び絶縁被膜の形成に有利に作用する。In addition, when degreasing and adhering Si compounds, Na and Na compounds harmful to the formation of the insulating film remain in the cracks of the oxide film, oxides left on the steel plate due to poor pickling, etc. Although it remains together with the dirt, the scale is removed by degreasing and pickling as described above, so the amount of adhesion is reduced and it has an advantageous effect on the subsequent formation of subscale and formation of an insulating film. To do.
【００１７】さらに、脱脂、酸洗により清浄化した鋼板
表面に所定量のSi化合物を付着させることにより、焼鈍
時にFeO の生成が抑制されること、たまFeO の生成しな
い領域の脱炭焼鈍雰囲気であっても好適なサブスケール
の組成であるSiO2、Fe2SiO4 の形の酸化物の形成を促進
させ均一なサブスケールが得られる。Further, by depositing a predetermined amount of Si compound on the surface of the steel sheet cleaned by degreasing and pickling, the production of FeO is suppressed during annealing, and in the decarburization annealing atmosphere in the area where FeO is not produced occasionally. Even if it is, a uniform subscale can be obtained by promoting the formation of oxides in the form of SiO 2 and Fe 2 SiO 4 , which are suitable subscale compositions.
【００１８】そしてこれらの予備処理により最終焼鈍に
より欠陥がなく均一かつ平滑な絶縁被膜が得られ、前記
した脱脂のみでSi化合物を付着させた場合の問題点は解
消される。By these pretreatments, a uniform and smooth insulating film having no defects can be obtained by the final annealing, and the above problems when the Si compound is adhered only by degreasing are solved.
【００１９】つぎにこの発明の実施態様を図面により説
明する。図１は、この発明を適用する場合の脱脂−酸洗
−Si化合物付着処理（電着）ラインの１例を示す模式図
である。図１においては、１はペイオフリール、２はス
トリップ、３はアルカリ浸漬槽、４，５，８，９，12,
13はスクラバー、６，10, 14は湯洗槽、７は酸洗槽、11
は電解槽（Si化合物付着）、15はドライヤー、16はテン
ションリールである。Next, an embodiment of the present invention will be described with reference to the drawings. FIG. 1 is a schematic diagram showing an example of a degreasing-pickling-Si compound adhesion treatment (electrodeposition) line when the present invention is applied. In FIG. 1, 1 is a payoff reel, 2 is a strip, 3 is an alkali immersion tank, 4, 5, 8, 9, 12,
13 is a scrubber, 6, 10 and 14 are hot water washing tanks, 7 is a pickling tank, 11
Is an electrolytic cell (Si compound is attached), 15 is a dryer, and 16 is a tension reel.
【００２０】なお、この発明では上記ラインを連続焼鈍
ラインに組み込み、湯洗槽14を経たストリップ２を直接
連続焼鈍ラインに送り連続的に脱炭焼鈍することもよ
い。In the present invention, the above line may be incorporated into a continuous annealing line, and the strip 2 that has passed through the hot water bath 14 may be directly sent to the continuous annealing line for continuous decarburization annealing.
【００２１】上記において、アルカリ浸漬槽３のアルカ
リ溶液は圧延油などのストリップ２の表面に付着してい
る油分を除去できるものであればよいが、けい酸ナトリ
ウム類を用いることが好適である。なお、脱脂方法はこ
の例の浸漬脱脂のほか、スプレー脱脂、電解脱脂などを
用いてもよい。In the above, the alkaline solution in the alkaline dipping tank 3 may be any one capable of removing the oil component such as rolling oil adhering to the surface of the strip 2, but sodium silicates are preferably used. As the degreasing method, spray degreasing, electrolytic degreasing, or the like may be used in addition to the immersion degreasing of this example.
【００２２】酸洗槽７の酸洗液は塩酸、硫酸、リン酸な
どいずれでもよく、その酸洗条件は、除去する酸化物の
量により液の濃度、温度及び酸洗時間を調整するが、過
酸洗は歩止りを低下させるとともに表面粗度を大きくし
製品での占積率を低下させるという問題が生じる。した
がって、通常の使用範囲としては塩酸を用いる場合、濃
度３〜10％、温度40〜70℃酸洗時間３〜60秒間程度の弱
酸洗でよく、前工程で脱脂され、後工程でSi化合物が塗
布されるため、この程度の弱酸洗で最終的に欠陥のない
均一かつ平滑な絶縁被膜を得ることができる。The pickling solution in the pickling tank 7 may be any of hydrochloric acid, sulfuric acid, phosphoric acid, etc. The pickling conditions are such that the concentration, temperature and pickling time of the solution are adjusted depending on the amount of oxide to be removed. The overpickling causes a problem that the yield is lowered and the surface roughness is increased to lower the space factor in the product. Therefore, when hydrochloric acid is used as a normal range of use, weak acid pickling with a concentration of 3 to 10% and a temperature of 40 to 70 ° C and a pickling time of about 3 to 60 seconds is sufficient, and degreasing is performed in the previous step and Si compounds are removed in the subsequent step. Since it is applied, a uniform and smooth insulating film without defects can be finally obtained by such a weak pickling.
【００２３】なお、塩酸酸洗の場合の液の濃度及び温度
をパラメーターとする酸洗時間と鋼板の溶失減量の関係
を図３に示すが、液の濃度60％、温度60℃、酸洗時間20
秒の条件でも溶失減量は0.6 g/m2程度てあり、酸洗によ
る歩止り低下はわずかである。FIG. 3 shows the relationship between the pickling time and the loss of the steel sheet in the case of hydrochloric acid pickling with the concentration and temperature of the solution as parameters. The concentration of the solution is 60%, the temperature is 60 ° C., and the pickling is Time 20
Even under the condition of seconds, the loss on dissolution was about 0.6 g / m 2 , and the decrease in yield due to pickling was slight.
【００２４】電解槽11に用いる電解液は、オルトけい酸
ナトリウム(Na4SiO4) 、メタけい酸ナトリウム(Na2Si
O3) あるいは種々のけい酸ナトリウムの液体混合物であ
る水ガラスなどが適している。これらの電解液を用いて
電解脱脂することにより、鋼板表面にけい酸、けい酸塩
あるいはこれらと鉄の水酸化物の化合物すなわちSi化合
物をストリップ２表面に電着させる。またこの電解によ
り有害なNa及びその化合物の付着を抑制することができ
る。The electrolytic solution used in the electrolytic cell 11 is sodium orthosilicate (Na 4 SiO 4 ) or sodium metasilicate (Na 2 Si).
O 3 ) or water glass, which is a liquid mixture of various sodium silicates, is suitable. By electrolytic degreasing using these electrolytic solutions, silicic acid, silicate or a compound of these and a hydroxide of iron, that is, a Si compound, is electrodeposited on the surface of the strip 2. Further, this electrolysis can suppress the harmful adhesion of Na and its compounds.
【００２５】なお、Si化合物のストリップ２表面への付
着処理は、浸漬法によってもよいが、上記した電解法
が、電流量により付着量の制御が容易であること、酸洗
によりスケールが除去されていることと相まって絶縁被
膜の形成に有害なNa及びその化合物の付着を抑制できる
ことなどから有利に適合する。The adhesion treatment of the Si compound on the surface of the strip 2 may be carried out by the dipping method. However, in the above-mentioned electrolysis method, the adhesion amount can be easily controlled by the amount of electric current, and the scale is removed by pickling. In addition to this, the adhesion of Na and its compounds, which are harmful to the formation of the insulating coating, can be suppressed, which is advantageous.
【００２６】以上のような脱脂−酸洗−Si化合物付着の
サブスケール事前処理を行うことにより、つぎの脱炭焼
鈍でストリップ表面に欠陥のない薄く均一なサブスケー
ルを生成させることができ、その後の焼鈍分離剤の塗
布、最終焼鈍により欠陥のない均一かつ平滑な絶縁被膜
を形成させることができる。By performing the degreasing-pickling-Si compound deposition subscale pretreatment as described above, it is possible to produce a thin and uniform subscale with no defects on the strip surface by the subsequent decarburization annealing. By applying the annealing separating agent and the final annealing, it is possible to form a uniform and smooth insulating coating without defects.
【００２７】さらに、上記ラインを連続焼鈍ラインに組
込み連続してこれらの処理を行うことにより、連続焼鈍
前に一度コイルに巻取ることによって発生するコイル両
端部の不均一部の発生が解消され、より均一で安定した
品質の製品が得られる。Furthermore, by incorporating the above-mentioned line into a continuous annealing line and continuously performing these treatments, the occurrence of non-uniform portions at both ends of the coil caused by winding once around the coil before continuous annealing is eliminated, A more uniform and stable quality product is obtained.
【００２８】[0028]
【実施例】適合例 Si：3.30wt％と抑制剤としてSe, Sbを含有する0.3 mmの
最終板厚に冷間圧延された方向性電磁鋼板用冷延コイル
を、前掲図１に示したラインを用いて、濃度：３％、温
度：８０℃のけい酸ナトリウム中で浸漬時間：７秒間の
脱脂を行ったのち、ブラッシング、湯洗し、濃度：５
％、温度：60℃の塩酸溶液中で浸漬時間：７秒間の酸洗
を行い、さらにブラッシング、湯洗したのち、濃度：３
％、温度：８０℃のけい酸ナトリウム中で電流密度：１
０C/dm2 の電解処理を行って付着量：２mg/m2のSi化合
物を付着させ、ブラッシング、水洗した。Examples Suitable example Si: 3.30 wt% and Se, Sb as inhibitors, cold-rolled coil for grain-oriented electrical steel sheet cold-rolled to a final plate thickness of 0.3 mm, the line shown in FIG. 1 above. After degreasing in sodium silicate at a concentration of 3% and a temperature of 80 ° C. for 7 seconds, brushing and washing with hot water, concentration: 5
%, Temperature: 60 ° C. Immersion in hydrochloric acid solution for 7 seconds, pickling, brushing and washing with hot water, concentration: 3
%, Temperature: 80 ° C. in sodium silicate Current density: 1
An electrolytic treatment of 0 C / dm 2 was performed to deposit a Si compound with a deposition amount of 2 mg / m 2 , and the resultant was brushed and washed with water.
【００２９】この最終の水洗に用いる水には、Na：１pp
m 以下の純水を用い、その温度は80℃とした。ついで、
露点：60℃、H2：50％、残部N2ガスよりなる湿水素雰囲
気中で、830℃、３分間の連続脱炭焼鈍を施し、さらにM
gO を主成分とする焼鈍分離剤を塗布したのちコイル状
に巻取り、850 ℃に保持して２次再結晶を完了させたの
ち、H2雰囲気中で1200℃、10時間の純化焼鈍を施した。The water used for this final washing includes Na: 1 pp
Pure water of m or less was used, and the temperature was 80 ° C. Then,
Dew point: 60 ° C, H 2 : 50%, balance N 2 gas in a wet hydrogen atmosphere, continuous decarburization annealing at 830 ° C for 3 minutes, and then M
After applying an annealing separating agent containing gO as the main component, it was wound into a coil and kept at 850 ° C to complete the secondary recrystallization, and then purified annealing was performed at 1200 ° C for 10 hours in an H 2 atmosphere. did.
【００３０】比較例 前掲図１の６の湯洗槽、７の酸洗槽、８，９のスクラバ
ー、10の湯洗槽を用いないで、その他の条件は適合例と
同様の条件で処理した。 Comparative Example Without using the hot water washing tank 6 in FIG. 1, the pickling tank 7 in FIG. 1, the scrubber 8 and 9, and the hot water washing tank 10 in other conditions, the other conditions were the same as those in the conforming example. ..
【００３１】これらの適合例、比較例とも複数のコイル
を用いて処理したもので、各冷延板の酸素目付量と、こ
れに対応する最終焼鈍後の絶縁膜の欠陥発生率の関係を
調査した。これらの調査結果を図２にまとめて示す。Both the conforming example and the comparative example were processed using a plurality of coils, and the relationship between the oxygen basis weight of each cold-rolled sheet and the corresponding defect occurrence rate of the insulating film after the final annealing was investigated. did. The results of these investigations are summarized in FIG.
【００３２】ここに、絶縁被膜の欠陥発生率は最終焼鈍
後の板面を全面にわたって表面観察を行い、鋼帯の長さ
１００ｍを１区画とし、被膜欠陥が検出された区画数の
全区画数に対する割合として算出したものである。Here, the defect occurrence rate of the insulating film was observed by observing the entire surface of the plate after the final annealing, and the length of the steel strip was 100 m as one partition, and the total number of partitions in which the film defect was detected was the total number of partitions. It is calculated as a ratio to.
【００３３】図２から明らかなように、適合例は冷延板
の酸素目付量が多くなっても絶縁被膜の欠陥発生率は少
なく安定しているのに対し、比較例は酸素目付量の増加
とともに絶縁被膜の欠陥発生率も増加している。As is clear from FIG. 2, the conformity example is stable with a small defect occurrence rate of the insulating film even when the oxygen basis weight of the cold-rolled sheet increases, whereas the comparative example increases the oxygen basis weight. At the same time, the defect occurrence rate of the insulating coating is increasing.
【００３４】すなわち、比較例では冷間圧延までの前工
程の変動があった場合これを吸収しきれずに絶縁被膜の
欠陥発生率が変動することを示しているのに対し、この
発明の適合例は前工程の変動があってもこれに影響され
ることなく、欠陥の少ない絶縁被膜を得ることができる
ことを示している。That is, in the comparative example, when there is a change in the previous process up to cold rolling, it cannot be completely absorbed, and the defect occurrence rate of the insulating film changes, whereas a suitable example of the present invention. Indicates that an insulating coating with few defects can be obtained without being affected by fluctuations in the previous process.
【００３５】[0035]
【発明の効果】この発明は、冷延板を脱脂後酸洗するこ
とにより、鋼板表面上に残留する酸化膜の除去を容易に
し、加えてSi化合物を鋼板上に均一に付着させ脱炭焼鈍
により欠陥のない均一なサブスケールを生成させ、その
結果最終焼鈍において欠陥のない均一かつ平滑な絶縁被
膜を歩止りの低下をともなうことなく形成させるもので
あって、電磁鋼板絶縁被膜の均一形成用予備処理方法と
して有利に適用できる。INDUSTRIAL APPLICABILITY The present invention facilitates the removal of an oxide film remaining on the surface of a steel sheet by degreasing and then pickling the cold-rolled sheet, and additionally deposits a Si compound evenly on the steel sheet for decarburization annealing. To produce a uniform subscale without defects, and as a result, to form a uniform and smooth insulating film without defects in the final annealing without lowering the yield. It can be advantageously applied as a pretreatment method.
【図１】この発明を適用する場合の脱脂−酸洗−Si化合
物付着処理（電解）ラインの１例を示す模式図である。FIG. 1 is a schematic view showing an example of a degreasing-pickling-Si compound adhesion treatment (electrolysis) line when the present invention is applied.
【図２】冷延板の酸素目付量と絶縁被膜の欠陥発生率の
関係を示すグラフである。FIG. 2 is a graph showing the relationship between the oxygen basis weight of a cold rolled sheet and the defect occurrence rate of an insulating coating.
【図３】塩酸酸洗による酸洗時間と溶失減量の関係を示
すグラフである。FIG. 3 is a graph showing the relationship between the acid pickling time by hydrochloric acid pickling and the amount of dissolution loss.
１ ペイオフリール ２ ストリップ ３ アルカリ浸漬槽 ４，５，８，９，12, 13 スクラバー ６，10, 14 湯洗槽 ７ 酸洗槽 11 電解槽 15 ドライヤー 16 テンションリール 1 Payoff reel 2 Strip 3 Alkali immersion tank 4, 5, 8, 9, 12, 13 Scrubber 6,10, 14 Hot water cleaning tank 7 Pickling tank 11 Electrolytic tank 15 Dryer 16 Tension reel
Claims (2)
前処理を施してから脱炭・１次再結晶焼鈍を行うに当
り、 該サブスケール事前処理が、含けい素鋼冷延板を脱脂
後、残留スケールを除去する酸洗を行い、つづいてSi化
合物の付着処理を施すことから成る電磁鋼板絶縁被膜の
均一形成用予備処理方法。1. When carrying out decarburization / primary recrystallization annealing after subjecting a silicon steel cold-rolled sheet to a subscale generation pretreatment, the subscale pretreatment is performed on the silicon steel cold rolled sheet. A pretreatment method for uniform formation of an electrical steel sheet insulating coating, which comprises degreasing, pickling to remove residual scale, and subsequent adhesion treatment of Si compounds.
処理と脱炭・１次再結晶焼鈍とを連続して行うことを特
徴とする電磁鋼板絶縁被膜の均一形成用予備処理方法。2. A pretreatment method for uniform formation of an electrical steel sheet insulating coating, which comprises continuously performing the subscale generation pretreatment according to claim 1 and decarburization / primary recrystallization annealing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4005644A JP2731312B2 (en) | 1992-01-16 | 1992-01-16 | Pretreatment method for uniform formation of electrical steel sheet insulation coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4005644A JP2731312B2 (en) | 1992-01-16 | 1992-01-16 | Pretreatment method for uniform formation of electrical steel sheet insulation coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05195239A true JPH05195239A (en) | 1993-08-03 |
| JP2731312B2 JP2731312B2 (en) | 1998-03-25 |
Family
ID=11616844
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4005644A Expired - Fee Related JP2731312B2 (en) | 1992-01-16 | 1992-01-16 | Pretreatment method for uniform formation of electrical steel sheet insulation coating |
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| Country | Link |
|---|---|
| JP (1) | JP2731312B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009533855A (en) * | 2006-04-12 | 2009-09-17 | シーメンス アクチエンゲゼルシヤフト | Lamination method of electromagnetic steel strip for transformer core |
| JP2017133080A (en) * | 2016-01-29 | 2017-08-03 | Ｊｆｅスチール株式会社 | Oriented electromagnetic steel sheet and manufacturing method therefor |
| JP6191810B1 (en) * | 2017-03-24 | 2017-09-06 | 新日鐵住金株式会社 | Steel plate manufacturing method |
| US10062483B2 (en) | 2011-12-28 | 2018-08-28 | Jfe Steel Corporation | Grain-oriented electrical steel sheet and method for improving iron loss properties thereof |
| JP2019094571A (en) * | 2019-02-14 | 2019-06-20 | Ｊｆｅスチール株式会社 | Oriented electromagnetic steel sheet and manufacturing method thereof |
| US20220106661A1 (en) * | 2019-01-16 | 2022-04-07 | Nippon Steel Corporation | Method for producing grain oriented electrical steel sheet |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02243771A (en) * | 1989-03-17 | 1990-09-27 | Kawasaki Steel Corp | Production of grain-oriented silicon steel sheet having uniform forsterite coating film |
-
1992
- 1992-01-16 JP JP4005644A patent/JP2731312B2/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02243771A (en) * | 1989-03-17 | 1990-09-27 | Kawasaki Steel Corp | Production of grain-oriented silicon steel sheet having uniform forsterite coating film |
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| JP2009533855A (en) * | 2006-04-12 | 2009-09-17 | シーメンス アクチエンゲゼルシヤフト | Lamination method of electromagnetic steel strip for transformer core |
| US10062483B2 (en) | 2011-12-28 | 2018-08-28 | Jfe Steel Corporation | Grain-oriented electrical steel sheet and method for improving iron loss properties thereof |
| JP2017133080A (en) * | 2016-01-29 | 2017-08-03 | Ｊｆｅスチール株式会社 | Oriented electromagnetic steel sheet and manufacturing method therefor |
| JP6191810B1 (en) * | 2017-03-24 | 2017-09-06 | 新日鐵住金株式会社 | Steel plate manufacturing method |
| WO2018173287A1 (en) * | 2017-03-24 | 2018-09-27 | 新日鐵住金株式会社 | Method for manufacturing steel sheet |
| CN110121573A (en) * | 2017-03-24 | 2019-08-13 | 日本制铁株式会社 | The manufacturing method of steel plate |
| US11401567B2 (en) | 2017-03-24 | 2022-08-02 | Nippon Steel Corporation | Manufacturing method of steel sheet |
| US20220106661A1 (en) * | 2019-01-16 | 2022-04-07 | Nippon Steel Corporation | Method for producing grain oriented electrical steel sheet |
| JP2019094571A (en) * | 2019-02-14 | 2019-06-20 | Ｊｆｅスチール株式会社 | Oriented electromagnetic steel sheet and manufacturing method thereof |
| WO2022186357A1 (en) * | 2021-03-03 | 2022-09-09 | Ｊｆｅスチール株式会社 | Method for determining finish annealing conditions for oriented electromagnetic steel sheet, and method for manufacturing oriented electromagnetic steel sheet using said determination method |
| JP7168134B1 (en) * | 2021-03-03 | 2022-11-09 | Ｊｆｅスチール株式会社 | METHOD FOR DETERMINING FINISH ANNEALING CONDITIONS FOR GRAIN-EDUCED ELECTRICAL STEEL AND METHOD FOR MANUFACTURING GRAY-ORIENTED ELECTRICAL STEEL USING THE DETERMINATION METHOD |
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