JP5194641B2 - 方向性電磁鋼板用絶縁被膜処理液および絶縁被膜付方向性電磁鋼板の製造方法 - Google Patents
方向性電磁鋼板用絶縁被膜処理液および絶縁被膜付方向性電磁鋼板の製造方法 Download PDFInfo
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- JP5194641B2 JP5194641B2 JP2007217570A JP2007217570A JP5194641B2 JP 5194641 B2 JP5194641 B2 JP 5194641B2 JP 2007217570 A JP2007217570 A JP 2007217570A JP 2007217570 A JP2007217570 A JP 2007217570A JP 5194641 B2 JP5194641 B2 JP 5194641B2
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Description
これらの方法によって形成される絶縁被膜は、方向性電磁鋼板に引張応力を与え、磁歪特性を改善する効果を有する。しかし、これらの絶縁被膜処理液は、絶縁被膜の耐吸湿性を良好に維持するための成分として、無水クロム酸、クロム酸塩または重クロム酸塩などのクロム化合物を含み、これらに由来する6価クロムを含有する。絶縁被膜処理液中に含まれる6価クロムは、焼付けにより3価クロムに還元されて無害化されるが、廃液処理作業において取り扱いが難しいなどの問題があった。
その結果、Mg、Sr、Zn、BaおよびCaといった2価金属の過マンガン酸塩を添加することにより、所望の特性を有する絶縁被膜を得られることを見出した。
本発明は、上記の知見に立脚するものである。
(1)Mg、Ca、Ba、Sr、Zn、AlおよびMnのリン酸塩のうちから選ばれる1種または2種以上を含有し、この選択した該リン酸塩中のPO4を基準として、該PO4:1molに対し、コロイド状シリカをSiO2換算で0.5〜10mol、並びにMg、Sr、Zn、BaおよびCaの過マンガン酸塩のうちから選ばれる1種または2種以上を、該過マンガン酸塩中の金属元素換算で0.02〜2.5mol含有させることを特徴とする方向性電磁鋼板用絶縁被膜処理液。
上記絶縁被膜処理液として、Mg、Ca、Ba、Sr、Zn、AlおよびMnのリン酸塩のうちから選ばれる1種または2種以上を含有し、この選択した該リン酸塩中のPO4を基準として、該PO4:1molに対し、コロイド状シリカをSiO2換算で0.5〜10mol、並びにMg、Sr、Zn、BaおよびCaの過マンガン酸塩のうちから選ばれる1種または2種以上を、該過マンガン酸塩中の金属元素換算で0.02〜2.5mol含有した絶縁被膜処理液を用い、焼付け処理を350℃以上1100℃以下の温度で行うことを特徴とする絶縁被膜付方向性電磁鋼板の製造方法。
まず、絶縁被膜処理液として、リン酸マグネシウム[Mg(H2PO4)2]の34mass%水溶液:450ml(PO4:1mol)に対して、SiO2:30mass%のコロイド状シリカ450ml(SiO2:2mol)および過マンガン酸マグネシウム・六水和物[Mg(MnO4)2・6H2O]をMg換算で0.01〜5molの範囲で含有させた絶縁被膜処理液を用意した。
これらの絶縁被膜処理液を、フォルステライト被膜を有する二次再結晶焼鈍後の板厚:0.22mmの方向性電磁鋼板に塗布し、800℃、60秒の焼付け処理を施し、片面あたり厚さ:2μmの絶縁被膜を形成させた。
かくして得られた方向性電磁鋼板について、次に示す方法により、被膜張力、耐吸湿性、防錆性および占積率を評価した。
(1)被膜張力
上記の絶縁被膜付方向性電磁鋼板から、長さ方向を圧延方向として、幅:30mm×長さ:280mmの試験片をせん断により採取し、片面の絶縁被膜を除去してから、鋼板の長さ方向の片端30mmを固定して長さ方向を水平に、幅方向を鉛直方向として、試験片端部の反りの大きさを測定し、次の式から被膜張力を算出した。
σ(MPa)=1.2152×105(MPa)×板厚(mm)×反り(mm)/250(mm)/250(mm)
(2)耐吸湿性
耐吸湿性は、上記の絶縁被膜付方向性電磁鋼板から、50mm×50mmの試験片3枚を採取し、これらを100℃の蒸留水中で5分間浸漬煮沸して被膜表面のP溶出量を定量分析し、平均値で評価した。
(3)防錆性
防錆性は、温度50℃、露点50℃の空気中に上記の絶縁被膜付鋼板を50時間保持後、鋼板表面を目視観察し、錆の発生がないものを(○)、錆が発生したものを(×)とした。
(4)占積率
占積率は、JIS C 2550に準拠する方法で評価した。
図1に、P溶出量すなわち耐吸湿性に及ぼす過マンガン酸マグネシウム・六水和物の添加量の影響を、また図2には、被膜張力に及ぼす過マンガン酸マグネシウム・六水和物の添加量の影響を示す。図中の過マンガン酸マグネシウム・六水和物の添加量は、Mg換算でのmol数である。過マンガン酸マグネシウム・六水和物の添加量が、PO4:1molに対して、0.02mol以上になると、耐吸湿性が著しく向上し、また被膜張力の改善も認められた。一方、添加量が2.5molを超えた場合には、耐吸湿性は問題なかったものの、被膜張力の低下が認められた。
なお、防錆性および占積率については、過マンガン酸マグネシウム・六水和物の添加量が、Mg換算で0.02〜2.5molの範囲で良好であった。
本発明の絶縁被膜処理液は、Mg、Ca、Ba、Sr、Zn、AlおよびMnのリン酸塩のうちから選ばれる1種または2種以上と、コロイド状シリカ並びにMg、Sr、Zn、BaおよびCaの過マンガン酸塩から選ばれる1種または2種以上から構成される。
まず、リン酸塩であるが、Mg、Ca、Ba、Sr、Zn、AlおよびMnのリン酸塩のうちから1種または2種以上選んで含有させることが必要である。これは、これら以外のリン酸塩では、クロム酸塩類を添加しない場合には、耐吸湿性の良好な被膜が得られないからである。特に、Mg、Ca、Ba、Sr、Zn、AlおよびMnの第一リン酸塩であるMg(H2PO4)2、Ca(H2PO4)2、Ba(H2PO4)2、Sr(H2PO4)2、Zn(H2PO4)2、Al(H2PO4)3、Mn(H2PO4)2およびこれらの水和物は、水に容易に溶解するため、本発明に好適に用いることができる。
なお、本発明の過マンガン酸塩とは、(MnO4)−とMg、Sr、Zn、BaまたはCaの化合物(金属塩)であり、これらの水和物であってもよい。
コロイド状シリカとリン酸塩は、焼付け処理時にガラス質を形成するが、このガラス質に取り込まれなかったリン酸塩中のフリーのPO4が、過マンガン酸塩中の2価金属Mg、Sr、Zn、Ba、およびCaや過マンガン酸塩中のMnと結合し、例えば、Mgの過マンガン酸塩の場合、絶縁被膜中で水に対して不溶であるMg3(PO4)2を生成し、耐吸湿性が向上する。
また、硫酸塩など他の水溶性の塩と比較して過マンガン酸塩は、焼付け処理において、形成途上の被膜中に均一に分散する。そのため、フリーのPO4とMg、Sr、Zn、Ba、CaまたはMnは、容易に結合して水に対して不溶である物質を形成することも、耐吸湿性向上に寄与している。一方、KやNaなどの1価金属の過マンガン酸塩を用いた場合には、被膜張力が低下するとともに、防錆性が劣化するという問題が生じたが、2価金属の過マンガン酸塩を用いることにより、これらの問題が解決された。すなわち、そのメカニズムは必ずしも明らかではないが、KやNaといった1価金属を用いた場合、前記ガラス質中での原子間の結合をこれらの金属が切断する作用を生じ、結果として被膜張力の低下や防錆性の劣化をもたらしたものと考えられる。
方向性電磁鋼板が巻鉄心型の変圧器に用いられる場合、鋼板が巻かれ、鉄心の形に成形された後、800℃×3時間程度の歪取焼鈍が施される。その際、隣接する被膜同士で融着することがある。このような融着は、鉄心の層間絶縁抵抗を低下させることになり、ひいては磁気特性を劣化させる原因となるので、絶縁被膜には、耐融着性を付与させることが望ましいからである。
また、方向性電磁鋼板が積鉄心型の変圧器に用いられる場合、鋼板の積み作業を円滑に行うためには、鋼板同士の滑り性を良好にすることが望ましいからである。
所定の成分組成を有する方向性電磁鋼板用鋼スラブを熱間圧延し、必要に応じて熱延板焼鈍を施し、1回または中間焼鈍を挟む2回以上冷間圧延により最終板厚とし、その後、一次再結晶焼鈍と二次再結晶焼鈍を施した後、上述した本発明の絶縁被膜処理液を鋼板表面に塗布し、350〜1100℃の温度で焼付け処理する。
本発明において、スラブの成分組成は、特に制限されることはなく、従来公知のいずれもが適合する。ちなみに、スラブの主要成分であるC:0.10mass%以下、Si:2.0〜5.0mass%およびMn:0.01〜1.0mass%の他に、インヒビターとしてMnSを用いる場合は、S:200ppm 程度、AlNを用いる場合は、sol.Al:200ppm程度、およびMnSeとSbを用いる場合は、Mn、SeおよびSbを添加することができる。
冷間圧延に続く一次再結晶焼鈍は、一次再結晶のために施すが、脱炭を兼ねて行ってもよく、その処理条件は、800〜950℃の温度で10〜600秒間、連続焼鈍を行うことが望ましい。なお、一次再結晶焼鈍中、あるいは一次再結晶焼鈍後に、アンモニアガスなどを用いて窒化処理を施すこともできる。
なお、絶縁被膜処理液は、塗布性の向上のために、水を加えて希釈し密度を調整しても良い。また、塗布する際には、ロールコーターなど、公知の方法を使用することができる。
焼付け温度は、750℃以上であることが望ましい。これは、750℃以上で焼付けることによって、被膜張力が発生するからである。一方、1100℃を超えると被膜張力と防錆性が劣化するため、1100℃以下とする必要がある。ただし、方向性電磁鋼板が変圧器の鉄心に使用される場合、焼付け温度は、350℃以上であれば良い。これは、鉄心の製造に際しては、800℃の温度で3時間程度の歪取焼鈍が施されることが多いが、この場合、被膜張力は、この歪取焼鈍時に発現するからである。
・上記の絶縁被膜処理液中に過マンガン酸塩を含有させなかったもの。
・上記の絶縁被膜処理液中の過マンガン酸塩の代わりに、硫酸マグネシウム・七水和物をMg換算で1mol含有させたもの。
・リン酸マグネシウムMg(H2PO4)2水溶液500ml(PO4:1mol)に対して、コロイド状シリカ700ml(SiO2を3mol)および過マンガン酸ナトリウムをNa換算で0.5mol含有させたもの。
・リン酸マグネシウムMg(H2PO4)2水溶液500ml(PO4:1mol)に対して、コロイド状シリカ700ml(SiO2を3mol)および過マンガン酸カリウムをK換算で0.5mol含有させたもの。
(1)被膜張力
上記の絶縁被膜付方向性電磁鋼板から、長さ方向を圧延方向として、幅:30mm×長さ:280mmの試験片をせん断により採取し、片面の絶縁被膜を除去してから、鋼板の長さ方向の片端30mmを固定して長さ方向を水平に、幅方向を鉛直方向として、試験片端部の反りの大きさを測定し、次の式から被膜張力を算出した。
σ(MPa)=1.2152×105(MPa)×板厚(mm)×反り(mm)/250(mm)/250(mm)
(2)耐吸湿性
耐吸湿性は、上記の絶縁被膜付方向性電磁鋼板から、50mm×50mmの試験片3枚を採取し、これらを100℃の蒸留水中で5分間浸漬煮沸して被膜表面のP溶出量を定量分析し、平均値で評価した。
(3)防錆性
防錆性は、温度50℃、露点50℃の空気中に、上記の絶縁被膜付方向性電磁鋼板を50時間保持後、鋼板表面を目視観察し、錆が発生した部分の面積率で評価した。
(4)占積率
占積率は、JIS C 2550に準拠する方法で評価した。
以上の測定結果を表1に示す。
この焼付け処理後の方向性電磁鋼板について、実施例1と同様の方法で、被膜張力、耐吸湿性、防錆性および占積率を評価した。
結果を表2に示す。
この焼付け処理後の方向性電磁鋼板について、実施例1と同様の方法で、被膜張力、耐吸湿性、防錆性および占積率を評価した。なお、被膜張力については、歪取焼鈍の影響を調査するため、800℃×3時間の歪取焼鈍後にも評価を行った。
結果を表3に示す。
Claims (2)
- Mg、Ca、Ba、Sr、Zn、AlおよびMnのリン酸塩のうちから選ばれる1種または2種以上を含有し、この選択した該リン酸塩中のPO4を基準として、該PO4:1molに対し、コロイド状シリカをSiO2換算で0.5〜10mol、並びにMg、Sr、Zn、BaおよびCaの過マンガン酸塩のうちから選ばれる1種または2種以上を、該過マンガン酸塩中の金属元素換算で0.02〜2.5mol含有させることを特徴とする方向性電磁鋼板用絶縁被膜処理液。
- 方向性電磁鋼板用スラブを、熱間圧延後、必要に応じて熱延板焼鈍を施したのち、1回または中間焼鈍を挟む2回以上の冷間圧延により最終板厚に仕上げ、ついで一次再結晶焼鈍後、必要に応じてMgOを主体とする焼鈍分離剤を塗布してから二次再結晶焼鈍を施し、さらに絶縁被膜処理液を塗布したのち、焼付け処理を行う一連の工程により、方向性電磁鋼板を製造するに際し、
上記絶縁被膜処理液として、Mg、Ca、Ba、Sr、Zn、AlおよびMnのリン酸塩のうちから選ばれる1種または2種以上を含有し、この選択した該リン酸塩中のPO4を基準として、該PO4:1molに対し、コロイド状シリカをSiO2換算で0.5〜10mol、並びにMg、Sr、Zn、BaおよびCaの過マンガン酸塩のうちから選ばれる1種または2種以上を、該過マンガン酸塩中の金属元素換算で0.02〜2.5mol含有した絶縁被膜処理液を用い、焼付け処理を350℃以上1100℃以下の温度で行うことを特徴とする絶縁被膜付方向性電磁鋼板の製造方法。
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