JP7060160B2 - 絶縁被膜付き電磁鋼板 - Google Patents
絶縁被膜付き電磁鋼板 Download PDFInfo
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- JP7060160B2 JP7060160B2 JP2021510999A JP2021510999A JP7060160B2 JP 7060160 B2 JP7060160 B2 JP 7060160B2 JP 2021510999 A JP2021510999 A JP 2021510999A JP 2021510999 A JP2021510999 A JP 2021510999A JP 7060160 B2 JP7060160 B2 JP 7060160B2
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
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Description
[1]Siに結合するアルコキシ基以外の置換基が、水素、アルキル基、及びフェニル基から選ばれた少なくとも1種の非反応性置換基のみからなるトリアルコキシシラン及び/又はジアルコキシシラン(A)と、
重合性不飽和基を構造中に含有しないシランカップリング剤(B)と、
平均粒子径が0.08~0.9μmで、かつ、アスペクト比が10~100である板状シリカ(C)と、
重合性不飽和基含有化合物(D)と、
水と、
を以下の条件(1)~(3)を満足するように含有する表面処理剤を電磁鋼板の少なくとも片面に塗布、乾燥してなる絶縁被膜を有する絶縁被膜付き電磁鋼板。
(1)前記トリアルコキシシラン及び/又はジアルコキシシラン(A)と前記シランカップリング剤(B)との質量比(A/B)が0.05~1.00である。
(2)前記板状シリカ(C)の含有量が、前記表面処理剤における(A)~(D)の総質量に対し2~30質量%である。
(3)前記重合性不飽和基含有化合物(D)の含有量が、前記表面処理剤における(A)~(D)の総質量に対し2~18質量%である。
重合性不飽和基を構造中に含有しないシランカップリング剤(B)と、
平均粒子径が0.08~0.9μmで、かつ、アスペクト比が10~100である板状シリカ(C)と、
重合性不飽和基含有化合物(D)と、
潤滑剤(E)と、
水と、
を以下の条件(1)~(4)を満足するように含有する表面処理剤を電磁鋼板の少なくとも片面に塗布、乾燥してなる絶縁被膜を有する絶縁被膜付き電磁鋼板。
(1)前記トリアルコキシシラン及び/又はジアルコキシシラン(A)と前記シランカップリング剤(B)との質量比(A/B)が0.05~1.00である。
(2)前記板状シリカ(C)の含有量が、前記表面処理剤における(A)~(E)の総質量に対し2~30質量%である。
(3)前記重合性不飽和基含有化合物(D)の含有量が、前記表面処理剤における(A)~(E)の総質量に対し2~18質量%である。
(4)前記潤滑剤(E)の含有量が、前記表面処理剤における(A)~(E)の総質量に対し0.5~20質量%である。
本実施形態において、素材である電磁鋼板としては、特に制限はなく、従来から公知のものいずれもが適合する。すなわち、磁束密度の高いいわゆる軟鉄板(電気鉄板)やSPCCなどの一般冷延鋼板、また比抵抗を上げるためにSiやAlを含有させた無方向性電磁鋼板などいずれもが有利に適合する。
本実施形態で用いる表面処理剤(電磁鋼板用表面処理剤)は、Siに結合するアルコキシ基以外の置換基が、水素、アルキル基、及びフェニル基から選ばれた少なくとも1種の非反応性置換基のみからなるトリアルコキシシラン及び/又はジアルコキシシラン(A)と、重合性不飽和基を構造中に含有しないシランカップリング剤(B)と、平均粒子径が0.08~0.9μmで、かつ、アスペクト比が10~100である板状シリカ(C)と、重合性不飽和基含有化合物(D)と、水とを含有し、任意で潤滑剤(E)を含有する。
本実施形態で用いる表面処理剤は、トリアルコキシシラン及び/又はジアルコキシシラン(A)を含む。
本実施形態で用いる表面処理剤は、重合性不飽和基を構造中に含有しないシランカップリング剤(B)を含む。シランカップリング剤(B)の種類は、重合性不飽和基を構造中に含有しない限り特に限定されず、一般式XSi(R4)n(OR)3-n(ここで、nは0、1又は2)で示され、それらの1種以上を同時に用いることができる。Xは、活性水素含有アミノ基、エポキシ基、及びメルカプト基から選ばれる少なくとも1種の反応性官能基を有する分子鎖である。R4はアルキル基であり、好ましくは炭素数1~4の直鎖又は分岐のアルキル基であり、更に好ましくは炭素数1~2の直鎖又は分岐のアルキル基である。ORは任意の加水分解性基であり、Rは例えばアルキル基であり、好ましくは炭素数1~4の直鎖又は分岐のアルキル基であり、更に好ましくは炭素数1~2の直鎖又は分岐のアルキル基である。また、Rは例えばアシル基(-COR5)であり、R5は好ましくは炭素数1~4の直鎖又は分岐のアルキル基であり、更に好ましくは炭素数1~2の直鎖又は分岐のアルキル基である。シランカップリング剤(B)として、例えば、N-(アミノエチル)3-アミノプロピルトリメトキシシラン、3-アミノプロピルトリメトキシシラン、3-グリシドキシプロピルトリメトキシシラン、3-グリシドキシプロピルメチルジメトキシシラン、2-(3,4エポキシシクロヘキシル)エチルトリエトキシシラン、3-メルカプトプロピルトリメトキシシラン、及びこれらの加水分解物などが使用できる。なかでも、電磁鋼板の耐食性がより優れるという観点から、アミノ基又はエポキシ基を有するシランカップリング剤が好ましい。
本実施形態において、トリアルコキシシラン及び/又はジアルコキシシラン(A)とシランカップリング剤(B)との質量比(A/B)は、0.05~1.00の範囲とする。質量比が1.00を超える場合、シランカップリング剤(B)の量が十分でなく、絶縁被膜の強靭性を十分に得ることができない。その結果、耐テンションパッド性の劣化やハンドリングでの傷や被膜剥離などが発生し易い。本開示では、トリアルコキシシラン及び/又はジアルコキシシラン(A)よりもシランカップリング剤(B)を多く含有させることにより、耐テンションパッド性を顕著に向上させることができる。この観点から、質量比(A/B)は1.00以下とし、好ましくは0.50以下とする。一方で、質量比(A/B)が低すぎると、TIG溶接性が低下する。この観点から、質量比(A/B)は0.05以上とし、好ましくは0.10以上とする。
本実施形態で用いる表面処理剤は、板状シリカ(C)を含む。この板状シリカは、葉状シリカや鱗片状シリカとも呼ばれるもので、SiO2の薄層が多数積層された層状珪酸構造を有している。そして、かかる板状シリカとしては、非結晶性又は微結晶性を有するものが好ましい。板状シリカは、薄層の一次粒子が積層した凝集粒子を作製し、この凝集粒子を粉砕することによって得ることができる。かような板状シリカは層状の形態をとるため、一般的なシリカ粒子、例えばコロイダルシリカなどと比較して腐食物質透過抑制性に優れ、さらに水酸基が多いために密着性に優れ、かつ軟質であることから滑り性に優れる。また、板状シリカを含む表面処理剤を塗布した場合、塗布量が少なくなりがちな鋼板表面凸部においても表面処理剤が残り、鋼板表面の凹凸に従った均一な表面処理剤の塗布が可能となるため、耐食性に劣ることがない。
本実施形態で用いる表面処理剤は、重合性不飽和基含有化合物(D)を含むことが重要である。重合性不飽和基含有化合物(D)として、例えば、ビニル基、ビニレン基、及びビニリデン基から選ばれる少なくとも1種の重合性不飽和基を有する化合物が挙げられる。重合性不飽和基含有化合物(D)は、モノマーであっても、ポリマー(オリゴマーを含む)であってもよい。
<装置及び操作条件>
分離カラム:東ソー株式会社製TSKgelSuperAWM-H(2本を直列に接続して使用)
検出器:示差屈折計
カラム温度:40℃
移動相:関東化学株式会社製N,N-ジメチルホルムアミド(10mmоl/L LiBr)
標準試料:標準ポリスチレンキット(東ソー株式会社製PStQuick B)
試料濃度:0.1質量%
試料注入量:30μL(マイクロリットル)
流速:0.5mL/min
本実施形態で用いる表面処理剤は、打抜き性及び耐テンションパッド性を向上させるため、任意で潤滑剤(E)を含有することができる。潤滑剤(E)としては、ポリエチレンワックス、酸化ポリエチレンワックス、酸化ポリプロピレンワックス、カルナバワックス、パラフィンワックス、モンタンワックス、ライスワックス、テフロン(登録商標)ワックス、2硫化炭素、グラファイトなどが挙げられる。また、潤滑剤(E)としては、ノニオン性アクリル樹脂を用いてもよい。ノニオン性アクリル樹脂としては、例えばアクリル酸、メタクリル酸、アクリル酸エステル、メタクリル酸エステル、スチレンなどのビニル系モノマーをポリエチレンオキサイド又はポリプロピレンオキサイドを構造上にもつノニオン系界面活性剤(乳化剤)の存在下、水中で乳化重合した水系エマルション等、ノニオン性乳化剤で乳化されたアクリル樹脂が挙げられる。これらの潤滑剤の中から、1種又は2種以上を用いることができる。
本実施形態では、電磁鋼板の少なくとも片面に表面処理剤を塗布し、加熱乾燥することにより、絶縁被膜を形成する。表面処理剤を電磁鋼板に塗布する方法としては、ロールコート法、バーコート法、浸漬法、スプレー塗布法などが挙げられ、処理される電磁鋼板の形状などによって適宜最適な方法が選択される。より具体的には、例えば、電磁鋼板がシート状であればロールコート法、バーコート法又はスプレー塗布法を選択できる。スプレー塗布法は、表面処理剤を電磁鋼板にスプレーしてロール絞りや気体を高圧で吹きかけて塗布量を調整する方法である。電磁鋼板が成型品とされている場合であれば、表面処理剤に浸漬して引き上げ、場合によっては圧縮エアーで余分な表面処理剤を吹き飛ばして塗布量を調整する方法などが選択される。
板厚:0.5mmの電磁鋼板[A230(JIS C 2552(2000))]を供試材として使用した。
試験板の作製方法としては、まず上記の供試材の表面を、日本パーカライジング(株)製パルクリーンN364Sを用いて処理し、表面上の油分や汚れを取り除いた。次に、水道水で水洗して供試材表面が水で100%濡れることを確認した後、更に純水(脱イオン水)を流しかけ、100℃雰囲気のオーブンで水分を乾燥したものを試験板として使用した。
各成分を表1に示す組成(質量比)にて水中で混合し、表面処理剤を得た。なお、表面処理剤に対する成分(A)~(E)の総質量の濃度は6.3g/Lとした。以下に、表1で使用した化合物について説明する。
A1:メチルトリメトキシシラン
A2:ジメチルジメトキシシラン
B1:3-グリシドキシプロピルトリメトキシシラン
B2:3-アミノプロピルトリメトキシシラン
B3:N-(アミノエチル)3-アミノプロピルトリメトキシシラン
C1:平均粒子径0.2μm、アスペクト比20
C2:平均粒子径0.5μm、アスペクト比50
C3:平均粒子径0.1μm、アスペクト比10
D1:アクリレート変性ウレタン樹脂(重量平均分子量:7500)
D2:ビニルトリメトキシシラン
D3:3-メタクリロキシプロピルトリメトキシシラン
D4:フマル酸
D5:(メタ)アクリロイル基変性ウレタン樹脂(重量平均分子量:7500)
D6:アクリロイル基変性ウレタン樹脂(重量平均分子量:500000)
E1:ポリエチレンワックス(ケミパール900)
連続焼鈍ラインにおいて所定の材質を得るための焼鈍を行った後、鋼板が冷却された段階でロールコーター塗装にて表面処理剤を塗布し、オーブンにて最高到達板温が200℃となるようにして乾燥させ、被膜付着量0.5g/m2の絶縁被膜を両面に形成した。ロールコーター条件としては、3ロールでフルリバース方式とした。なお、最高到達板温は試験板表面の最高到達温度を示す。
[接着特性]
接着強度評価用試験片のサイズは、25mm×100mmとし、DIN EN 1465(2009-07)に準じてせん断引張試験片を作製し、せん断引張試験を実施した。具体的には、接着剤を介して2枚の試験片の絶縁被膜同士を接着させて、接着面と平行な方向に引張荷重をかけて、接着面が破壊される時の最大荷重を接着面積で割ることで、引張せん断強度を求めた。接着剤としては、アセック(株)製の嫌気性アクリル系接着剤AS5334を使用し、アクチベータとしては、アセック(株)製のAS8000を使用した。以下の判定基準で引張せん断強度を評価した。結果を表1に示す。なお、◎又は○であれば合格とした。
(判定基準)
◎:8MPa以上
○:5MPa以上8MPa未満
×:5MPa未満
50mm×50mmに打ち抜いた供試材2枚を重ね合わせ、200gのオモリを乗せて50℃、相対湿度80%の恒温恒湿槽で2週間放置した。重ね合わせた2面の平均の錆発生面積率を目視にて測定した。結果を表1に示す。なお、◎又は○であれば合格とした。
(判定基準)
◎:0%
○:0%超え5%未満
×:5%以上
面積が10mm×10mmのテンションパッドを用い、太平理化工業(株)製ラビングテスターにて、19.6N(2.0kgf)の荷重をかけ絶縁被膜表面を100往復擦った。擦った部分とその近傍の付着量測定を行い、100往復後の絶縁被膜残存率を算出した。付着量は、Siの蛍光X線強度を測定し、付着量既知の標準板により得られた検量線から求めた。結果を表1に示す。なお、◎又は○であれば合格とした。
(判定基準)
◎:90%以上
○:70%以上90%未満
×:70%未満
100往復を200往復に変更した以外は、上記と同様の方法及び判定基準にて、耐テンションパッド性を評価した。結果を表1に示す。なお、◎又は○であれば合格とした。
Claims (2)
- Siに結合するアルコキシ基以外の置換基が、水素、アルキル基、及びフェニル基から選ばれた少なくとも1種の非反応性置換基のみからなるトリアルコキシシラン及び/又はジアルコキシシラン(A)と、
重合性不飽和基を構造中に含有しないシランカップリング剤(B)と、
平均粒子径が0.08~0.9μmで、かつ、アスペクト比が10~100である板状シリカ(C)と、
ビニル基、ビニレン基、及びビニリデン基から選ばれる少なくとも1種の重合性不飽和基を有する重合性不飽和基含有化合物(D)と、
水と、
を以下の条件(1)~(3)を満足するように含有する表面処理剤を電磁鋼板の少なくとも片面に塗布、乾燥してなる絶縁被膜を有する絶縁被膜付き電磁鋼板。
(1)前記トリアルコキシシラン及び/又はジアルコキシシラン(A)と前記シランカップリング剤(B)との質量比(A/B)が0.05~1.00である。
(2)前記板状シリカ(C)の含有量が、前記表面処理剤における(A)~(D)の総質量に対し2~30質量%である。
(3)前記重合性不飽和基含有化合物(D)の含有量が、前記表面処理剤における(A)~(D)の総質量に対し2~18質量%である。 - Siに結合するアルコキシ基以外の置換基が、水素、アルキル基、及びフェニル基から選ばれた少なくとも1種の非反応性置換基のみからなるトリアルコキシシラン及び/又はジアルコキシシラン(A)と、
重合性不飽和基を構造中に含有しないシランカップリング剤(B)と、
平均粒子径が0.08~0.9μmで、かつ、アスペクト比が10~100である板状シリカ(C)と、
ビニル基、ビニレン基、及びビニリデン基から選ばれる少なくとも1種の重合性不飽和基を有する重合性不飽和基含有化合物(D)と、
潤滑剤(E)と、
水と、
を以下の条件(1)~(4)を満足するように含有する表面処理剤を電磁鋼板の少なくとも片面に塗布、乾燥してなる絶縁被膜を有する絶縁被膜付き電磁鋼板。
(1)前記トリアルコキシシラン及び/又はジアルコキシシラン(A)と前記シランカップリング剤(B)との質量比(A/B)が0.05~1.00である。
(2)前記板状シリカ(C)の含有量が、前記表面処理剤における(A)~(E)の総質量に対し2~30質量%である。
(3)前記重合性不飽和基含有化合物(D)の含有量が、前記表面処理剤における(A)~(E)の総質量に対し2~18質量%である。
(4)前記潤滑剤(E)の含有量が、前記表面処理剤における(A)~(E)の総質量に対し0.5~20質量%である。
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