JPWO2021019859A1 - 無方向性電磁鋼板およびその製造方法 - Google Patents
無方向性電磁鋼板およびその製造方法 Download PDFInfo
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- JPWO2021019859A1 JPWO2021019859A1 JP2020546181A JP2020546181A JPWO2021019859A1 JP WO2021019859 A1 JPWO2021019859 A1 JP WO2021019859A1 JP 2020546181 A JP2020546181 A JP 2020546181A JP 2020546181 A JP2020546181 A JP 2020546181A JP WO2021019859 A1 JPWO2021019859 A1 JP WO2021019859A1
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- steel sheet
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- insulating film
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- 229910000565 Non-oriented electrical steel Inorganic materials 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 34
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 102
- 239000010959 steel Substances 0.000 claims abstract description 102
- 239000011248 coating agent Substances 0.000 claims abstract description 48
- 238000000576 coating method Methods 0.000 claims abstract description 48
- 229910000976 Electrical steel Inorganic materials 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 96
- 238000000137 annealing Methods 0.000 claims description 48
- 229910052742 iron Inorganic materials 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 37
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- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- -1 phosphoric acid compound Chemical class 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 17
- 239000010731 rolling oil Substances 0.000 claims description 17
- 238000011282 treatment Methods 0.000 claims description 15
- 239000003995 emulsifying agent Substances 0.000 claims description 13
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 13
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- 230000000694 effects Effects 0.000 description 10
- 229910019142 PO4 Inorganic materials 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 7
- 239000010452 phosphate Substances 0.000 description 7
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- 238000011156 evaluation Methods 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 3
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- 239000005049 silicon tetrachloride Substances 0.000 description 3
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
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- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
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- 230000002950 deficient Effects 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 238000004611 spectroscopical analysis Methods 0.000 description 1
Images
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Abstract
Description
本発明は上記問題に鑑みなされたもので、絶縁被膜を薄くしても、該被膜の密着性に優れる電磁鋼板を、その製造方法と共に提供することを目的とする。
一方、絶縁被膜の表面側のP濃化層は、絶縁被膜を形成する過程で、コーティング液にリン酸化合物などを1質量部以上添加したものを用いれば、該液の乾燥時に絶縁被膜の表面にPが浮上し、濃化層を形成することが出来る。
以上の組み合わせにより、絶縁被膜の表面側および地鉄との界面側の両方にP濃化層を形成することで、絶縁被膜が薄くても被膜密着性に優れた電磁鋼板を得られる。
(1)鋼板の少なくとも片面に絶縁被膜を有する電磁鋼板において、前記絶縁被膜は、表面側および地鉄との界面側の両方に、前記地鉄におけるP濃度より高いP濃度のP濃化層を有する無方向性電磁鋼板。
C:0.010%未満、
Si:1.5%以上10.0%以下、
Al:0.001%以上2.0%以下および
Mn:0.005%以上1.0%以下
を含有し、残部がFeおよび不可避的不純物の成分組成を有する、前記(1)に記載の無方向性電磁鋼板。
P:0.005%以上0.20%以下
を含有する、前記(2)に記載の無方向性電磁鋼板。
Sn:0.002%以上0.10%以下、
Mo:0.005%以上0.10%以下、
Sb:0.005%以上0.30%以下、
Cu:0.01%以上0.50%以下、
Cr:0.01%以上0.50%以下、
Ni:0.010%以上1.0%以下
のうちの1種以上を含有する、前記(2)または(3)に記載の無方向性電磁鋼板。
前記冷間圧延は、リン酸エステル型の乳化剤を1%以上含む圧延油を使用して行い、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。
前記冷間圧延後かつ前記仕上焼鈍前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる工程を有し、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。
前記冷間圧延は、リン酸エステル型の乳化剤を1%以上含む圧延油を使用して行い、
前記冷間圧延後かつ前記仕上焼鈍前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる工程を有し、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。
前記スラブにPを0.005〜0.20質量%含有させ、前記仕上焼鈍の焼鈍温度を1100℃以上とし、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。
前記冷間圧延は、リン酸エステル型の乳化剤を1%以上含む圧延油を使用して行う、
無方向性電磁鋼板の製造方法。
前記冷間圧延後かつ前記仕上焼鈍前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる工程を有する、
無方向性電磁鋼板の製造方法。
前記仕上焼鈍後に浸珪処理を施すか、又は前記仕上焼鈍を浸珪処理を兼ねた仕上焼鈍とする、
前記(8)から(13)のいずれかに記載の無方向性電磁鋼板の製造方法。
絶縁被膜の表面側および地鉄との界面側の両方にPが濃化することにより、被膜が強固となり、かつ地鉄との界面側で濃化したPが、地鉄と絶縁被膜との間のバインダーとして作用する。この効果により、絶縁被膜自身が薄くても、強固で密着性の高い絶縁被膜を有する電磁鋼板が得られる。
Ib>Ia・・・ (1)
Ic>Ia・・・ (2)
絶縁被膜厚は2.0μm以下が好ましい。膜厚が薄いほど占積率が向上するので、さらに好ましくは1.0μm以下である。好ましい膜厚の下限は無いが、形成される絶縁被膜の種類に応じて層間の絶縁が確保可能な薄さに留めればよい。上記絶縁被膜としては、有機成分のみや無機成分のみ、有機・無機複合物などからなるものを用いることができる。具体的には、有機成分としては、アクリル系、アクリルシリコン系、ポリエステル系、エポキシ系、フッ素系の樹脂等が挙げられる。無機成分としては、クロム酸塩系、重クロム酸塩系、ホウ酸塩系、珪酸塩系等が挙げられる。また、有機・無機複合物(半有機)としては、前述した有機成分と無機成分の複合物等が挙げられる。
C:0.010質量%未満
Cは、磁気時効を起こし、磁気特性を劣化させるため、含有量は少ないほど望ましい。しかし、過度のC量の低減は、製造コストの上昇を招く。そこで、C量は、磁気時効が実用上問題とならない0.010質量%未満とすることが好ましい。C量は、より好ましくは0.0050質量%未満である。
Siは、鋼の比抵抗を高め、鉄損特性を改善する元素であり、本発明では、鉄損特性改善効果を得るためには、1.5質量%以上含有させることが好ましい。しかし、Siを10.0質量%を超えて含有させると、飽和磁束密度が顕著に低下し、モータを製造した場合に却って大きなトルクの低下を招くようになる。よって、本発明では、Si量は、1.5質量%以上とすることが好ましく、2.0質量%以上とすることがより好ましく、10.0質量%以下とすることが好ましく、7.0質量%以下とすることがより好ましい。また、Si量は、1.5〜10.0質量%の範囲とすることがより好ましく、2.0〜7.0質量%とすることがさらに好ましい。なお、ここにおけるSi量とは、板厚方向に対するSi含有量の平均値である。
AlはSiと同様に鋼の比抵抗を高めるため、鉄損改善に有効な元素である。一方でAlを過剰に添加すると、飽和磁束密度を低下させるだけでなく、鋼中Nあるいは歪取り焼鈍時の鋼板窒化によるNと結びついてAlNを析出させるため、2.0質量%以下とすることが好ましく、0.50質量%以下とすることがより好ましい。鉄損の改善に有効な比抵抗増を得るためには、Al量を0.001質量%以上とすることが好ましく、0.002質量%以上とすることがより好ましい。更に好ましくは、Al量は、0.002〜0.50質量%である。
Mnは、熱間圧延時の加工性を改善するために、0.005質量%以上で含有させることが好ましく、1.0質量%以下で含有させることが好ましく、0.005〜1.0質量%の範囲で含有させることがより好ましい。Mn量が0.005質量%未満では、上記加工性改善効果が小さく、一方、1.0質量%を超えると、飽和磁束密度が低下するからである。より好ましくは、Mn量は、0.01質量%以上であり、0.30質量%以下であり、0.010〜0.30質量%であることが更に好ましい。
Pは後述するように、スラブ中に添加して熱処理を行うことにより、絶縁被膜中の地鉄との界面側にP濃化層を形成する手段の一つとなる。また、被膜への影響だけでなく、集合組織改善や比抵抗の増加による磁気特性の改善にも有効に作用するので、Pを0.005質量%以上含有させることが好ましく、0.030質量%以上含有させることが好ましい。一方で、P量は、0.20質量%を超えると急激に脆化し、製造性や加工性を損ねることから、0.20質量%以下とすることが好ましく、0.10質量%以下とすることが好ましい。P量は、より好ましくは0.030〜0.10質量%である。
Sn:0.002質量%以上、0.10質量%以下;Mo:0.005質量%以上、0.10質量%以下;Sb:0.005質量%以上、0.30質量%以下;Cu:0.01質量%以上、0.50質量%以下;Cr:0.01質量%以上、0.50質量%以下;Ni:0.010質量%以上、1.0質量%以下
上記成分はいずれも、磁気特性の改善を図るために添加することが有効な元素であるため、上記成分のうち1種以上を各元素の下限値以上にて添加することがさらに望ましい。ただし、添加のし過ぎは、磁気特性の劣化や製造性の悪化につながるので、それぞれに示した上限値までの範囲内で添加することが望ましい。
図1に示した例のように、絶縁被膜の地鉄との界面側において、Pと共にFeが濃化することで、FeとPの化合物が地鉄と絶縁被膜とのバインダーとして作用し、電磁鋼板上により強固に形成された絶縁被膜となる。ここで、Fe濃化の有無はGDSによって評価することができ、Feのピーク強度が得られる分析深さと、Pのピーク強度Ibが得られる分析深さとの差が0.5μm以下である場合に、絶縁被膜の地鉄との界面側がFeの濃化層を有するものとする。
板厚が薄いほど占積率の低下が問題となってくるため、板厚が0.25mm以下よりも薄い場合に本発明の効果が得られやすい。さらに、本発明は、板厚が0.20mm以下のときにより高い効果を発揮する。この効果の観点からは板厚の下限は必要ないが、板厚が0.05mm以下になるとコアの製造にかかわる打抜きなどのコストが大きく増大するため、0.05mm超が望ましい。
ここで、「電磁鋼板の厚み」又は単に「板厚」には、絶縁被膜の厚みも含まれる。
鋼板の板厚方向にSi濃度勾配を有することで、高周波における鉄損の改善が可能である。この濃度勾配を実現するための方法としては、例えば、SiCl4含有雰囲気中で浸珪処理しても良いし、Si濃度の異なる材料を積層して使用したクラッドによる製造方法でも良い。ここで、Siの濃度差は、渦電流損の改善効果を十分に得るため、下限値は1.0質量%とすることが好ましく、1.5質量%とすることがより好ましい。また、Siの濃度差は、ヒステリシス損の劣化を抑制するため、上限値は5.0質量%とすることが好ましく、3.5質量%とすることがより好ましい。更に好ましくは、Siの濃度差は、1.5〜3.5%である。
なお、「鋼板表層」及び「鋼板中心層」は、具体的には、鋼板の両表面(絶縁被膜を除く)からそれぞれ板厚1/3の領域を「鋼板表層」とし、残りの板厚1/3の領域を「鋼板中心層」と定義する。また、鋼板中心層のSi濃度は、該当する領域での平均濃度とし、鋼板表層のSi濃度は、両表面においてそれぞれ該当する領域での平均濃度を、更に平均した値(換言すれば、両表層の平均濃度)とする。そして、上記平均濃度については、EPMAを用いて板厚方向のSi濃度を測定し、その濃度プロファイルから評価することができる。
本発明の電磁鋼板は、常法に従い、電磁鋼板用のスラブに、熱間圧延、冷間圧延、次いで仕上焼鈍を施して仕上焼鈍板とし、該仕上焼鈍板の表面に絶縁被膜を形成する工程により、製造することができる。
絶縁被膜中の地鉄との界面側にPの濃化層を形成するために、上記の製造工程において、下記のいずれかの処理が必要である。
・冷間圧延時に、リン酸エステル型の乳化剤を1%以上含む圧延油を使用する
・前記冷間圧延後かつ前記仕上焼鈍(または浸珪処理)前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる
・スラブにPを0.005質量%以上0.20質量%以下含有させ、仕上焼鈍での焼鈍温度を1100℃以上とする
また、絶縁被膜の表面側にPの濃化層を形成するために、下記の処理が必要である。
・絶縁被膜形成工程において、リン酸化合物を1質量部以上含有する液を塗布する
前記Si濃度差を設けるために、更に、仕上焼鈍後に浸珪処理を行うか、またはコスト低減の理由から、前記仕上焼鈍を浸珪処理を兼ねた仕上焼鈍とすることができる。ここで、浸珪処理を行う場合の雰囲気ガスとしては四塩化珪素と窒素の混合ガスを用いることができる。浸珪処理を行う場合の熱処理温度は1100〜1300℃が望ましく、焼鈍時間は必要な浸珪量に応じ30〜120秒が望ましい。
絶縁被膜中にFe濃化層を形成するために、浸珪処理温度あるいは仕上焼鈍温度を1000℃以上とすることが好ましい。高周波での渦電流損低減の理由から粒径を粗大にすることを避ける必要があるので、好ましくは1300℃以下である。
次いで、仕上焼鈍を20%H2−80%N2乾燥雰囲気で1000℃×10sの条件で施した。なお、表1のNo.21、23および24は1100℃×10sの条件で、No.25は950℃×10sの条件で仕上焼鈍を施した。
Claims (14)
- 鋼板の少なくとも片面に絶縁被膜を有する電磁鋼板において、前記絶縁被膜は、表面側および地鉄との界面側の両方に、前記地鉄におけるP濃度より高いP濃度のP濃化層を有する無方向性電磁鋼板。
- 前記鋼板は、質量%で、
C:0.010%未満、
Si:1.5%以上10.0%以下、
Al:0.001%以上2.0%以下および
Mn:0.005%以上1.0%以下
を含有し、残部がFeおよび不可避的不純物の成分組成を有する、請求項1に記載の無方向性電磁鋼板。 - 前記鋼板は、さらに、質量%で、
P:0.005%以上0.20%以下
を含有する、請求項2に記載の無方向性電磁鋼板。 - 前記成分組成は、さらに、質量%で、
Sn:0.002%以上0.10%以下、
Mo:0.005%以上0.10%以下、
Sb:0.005%以上0.30%以下、
Cu:0.01%以上0.50%以下、
Cr:0.01%以上0.50%以下、
Ni:0.010%以上1.0%以下
のうちの1種以上を含有する、請求項2または3に記載の無方向性電磁鋼板。 - 前記絶縁被膜は、前記地鉄との界面側に、Feの濃化層を有する、請求項1から4のいずれかに記載の無方向性電磁鋼板。
- 前記鋼板の厚みが0.20mm以下である請求項1から5のいずれかに記載の無方向性電磁鋼板。
- 前記鋼板は、Si濃度が前記鋼板の表面側から前記鋼板の中心部側へ向かって低くなる濃度勾配を有し、該濃度勾配における鋼板表層と鋼板中心層とのSi濃度差が1.0〜5.0質量%である、請求項1から6のいずれかに記載の無方向性電磁鋼板。
- 請求項1から7のいずれかに記載の電磁鋼板の製造方法であって、該電磁鋼板用のスラブに、熱間圧延、冷間圧延、次いで仕上焼鈍を施して仕上焼鈍板とし、該仕上焼鈍板の表面に、絶縁被膜を形成する工程において、
前記冷間圧延は、リン酸エステル型の乳化剤を1%以上含む圧延油を使用して行い、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。 - 請求項1から7のいずれかに記載の電磁鋼板の製造方法であって、該電磁鋼板用のスラブに、熱間圧延、冷間圧延、次いで仕上焼鈍を施して仕上焼鈍板とし、該仕上焼鈍板の表面に、絶縁被膜を形成する工程において、
前記冷間圧延後かつ前記仕上焼鈍前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる工程を有し、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。 - 請求項1から7のいずれかに記載の電磁鋼板の製造方法であって、該電磁鋼板用のスラブに、熱間圧延、冷間圧延、次いで仕上焼鈍を施して仕上焼鈍板とし、該仕上焼鈍板の表面に、絶縁被膜を形成する工程において、
前記冷間圧延は、リン酸エステル型の乳化剤を1%以上含む圧延油を使用して行い、
前記冷間圧延後かつ前記仕上焼鈍前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる工程を有し、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。 - 請求項1から7のいずれかに記載の電磁鋼板の製造方法であって、該電磁鋼板用のスラブに、熱間圧延、冷間圧延、次いで仕上焼鈍を施して仕上焼鈍板とし、該仕上焼鈍板の表面に、絶縁被膜を形成する工程において、
前記スラブにPを0.005〜0.20質量%含有させ、前記仕上焼鈍の焼鈍温度を1100℃以上とし、
前記絶縁被膜の形成は、リン酸化合物を1質量部以上含有する液を塗布して行う、
無方向性電磁鋼板の製造方法。 - 請求項11に記載の電磁鋼板の製造方法において、
前記冷間圧延は、リン酸エステル型の乳化剤を1%以上含む圧延油を使用して行う、
無方向性電磁鋼板の製造方法。 - 請求項11または12に記載の電磁鋼板の製造方法において、
前記冷間圧延後かつ前記仕上焼鈍前に、前記冷間圧延を経た鋼板の表面に、リン酸化合物を5質量部以上含む水溶液を塗布乾燥させる工程を有する、
無方向性電磁鋼板の製造方法。 - 前記電磁鋼板用のスラブに、熱間圧延、冷間圧延、次いで仕上焼鈍を施して仕上焼鈍板とし、該仕上焼鈍板の表面に、絶縁被膜を形成する工程において、
前記仕上焼鈍後に浸珪処理を施すか、又は前記仕上焼鈍を浸珪処理を兼ねた仕上焼鈍とする、
請求項8から13のいずれかに記載の無方向性電磁鋼板の製造方法。
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