JPWO2020026627A1 - 絶縁被膜処理液、絶縁被膜付き方向性電磁鋼板およびその製造方法 - Google Patents
絶縁被膜処理液、絶縁被膜付き方向性電磁鋼板およびその製造方法 Download PDFInfo
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- JPWO2020026627A1 JPWO2020026627A1 JP2019555706A JP2019555706A JPWO2020026627A1 JP WO2020026627 A1 JPWO2020026627 A1 JP WO2020026627A1 JP 2019555706 A JP2019555706 A JP 2019555706A JP 2019555706 A JP2019555706 A JP 2019555706A JP WO2020026627 A1 JPWO2020026627 A1 JP WO2020026627A1
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- insulating coating
- treatment liquid
- steel sheet
- grain
- oriented electrical
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
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- 239000011163 secondary particle Substances 0.000 description 1
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- 239000006104 solid solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
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- 239000011701 zinc Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C22/73—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 characterised by the process
- C23C22/74—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 characterised by the process for obtaining burned-in conversion coatings
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- 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
-
- 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
- H01F1/16—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 in the form of sheets
- H01F1/18—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 in the form of sheets with insulating coating
Abstract
Description
Mg、Ca、Ba、Sr、Zn、Al、Mnのリン酸塩のうちから選ばれる1種または2種以上のリン酸塩と、コロイド状シリカと、金属元素を含む化合物の粒子と、を含有し、
前記リン酸塩100質量部に対し、前記コロイド状シリカの含有量がSiO2固形分換算で50〜120質量部であり、かつ、前記金属元素を含む化合物の粒子の含有量が金属元素換算で5〜60質量部であり、
チクソトロピーインデックス(TI)が1.00以上10.00以下である、絶縁被膜処理液。
[2]金属元素を含む化合物の粒子が、Ti、Zr、Hf、V、Mg、Zn、Nbの酸化物の粒子、Ti、Zr、Hf、V、Mg、Zn、Nbの窒化物の粒子のうちから選ばれる1種または2種以上である、[1]に記載の絶縁被膜処理液。
[3]金属元素を含む化合物の粒子が、TiO2、ZrO2、HfO2、MgO、ZnO、Nb2O5、V2O5、TiN、ZrNの粒子から選ばれる1種または2種以上である、[1]または[2]に記載の絶縁被膜処理液。
[4]金属元素を含む化合物の粒子の粒径が0.05μm以上1.0μm以下である、[1]〜[3]のいずれかに記載の絶縁被膜処理液。
[5]さらにカチオン系界面活性剤を含有する、[1]〜[4]のいずれかに記載の絶縁被膜処理液。
[6]カチオン系界面活性剤が第4級アンモニウム塩型カチオン系界面活性剤である、[5]に記載の絶縁被膜処理液。
[7]カチオン系界面活性剤の含有量が、Mg、Ca、Ba、Sr、Zn、Al、Mnのリン酸塩のうちから選ばれる1種または2種以上のリン酸塩100質量部に対し、0.20〜2.0質量部である、[5]または[6]に記載の絶縁被膜処理液。
[8][1]〜[7]のいずれかに記載の絶縁被膜処理液を焼付けしてなる絶縁被膜を表面に備える、絶縁被膜付き方向性電磁鋼板。
[9][1]〜[7]のいずれかに記載の絶縁被膜処理液を、方向性電磁鋼板の表面に塗布した後、焼付けする、絶縁被膜付き方向性電磁鋼板の製造方法。
[10]絶縁被膜処理液を方向性電磁鋼板の表面に塗布する際、前記方向性電磁鋼板を搬送しながら、前記絶縁被膜処理液をロールコーターを用いて前記方向性電磁鋼板の表面に塗布する、[9]に記載の絶縁被膜付き方向性電磁鋼板の製造方法。
Cは、ゴス方位結晶粒の発生に有用な成分であり、かかる作用を有効に発揮させるためには、C含有量は0.001%以上とすることが好ましい。一方、C含有量が0.10%を超えると脱炭焼鈍によっても脱炭不良を起こす場合がある。したがって、C含有量は0.001〜0.10%の範囲が好ましい。
Siは、電気抵抗を高めて鉄損を低下させるとともに、鉄のBCC組織を安定化させて高温の熱処理を可能とするために必要な成分であり、Si含有量は1.0%以上とすることが好ましい。一方、Si含有量が5.0%を超えると冷間圧延が困難となる。したがって、Si含有量は1.0〜5.0%の範囲が好ましい。Si含有量は、2.0〜5.0%の範囲がより好ましい。
Mnは、鋼の熱間脆性の改善に有効に寄与するだけでなく、SやSeが混在している場合には、MnSやMnSe等の析出物を形成し結晶粒成長の抑制剤としての機能を発揮するため、Mn含有量は0.01%以上とすることが好ましい。一方、Mn含有量が1.0%を超えるとMnSe等の析出物の粒径が粗大化してインヒビターとしての効果が失われる場合がある。したがって、Mn含有量は0.01〜1.0%の範囲が好ましい。
Alは、鋼中でAlNを形成して分散第二相としてインヒビターの作用をする有用成分であるので、sol.Alとして0.003%以上含有することが好ましい。一方、Al含有量がsol.Alとして0.050%を超えて含有するとAlNが粗大に析出してインヒビターとしての作用が失われる場合がある。したがって、Al含有量はsol.Alとして0.003〜0.050%の範囲が好ましい。
NもAlと同様にAlNを形成するために必要な成分であるため、N含有量は0.001%以上とすることが好ましい。一方、N含有量が0.020%を超えるとスラブ加熱時にふくれ等を生じる場合がある。したがって、N含有量は0.001〜0.020%の範囲が好ましい。
S、Seは、MnやCuと結合してMnSe、MnS、Cu2−xSe、Cu2−xSを形成し鋼中の分散第二相としてインヒビターの作用を発揮する有用成分であるため、S、Seの1種または2種の合計の含有量は0.001%以上とすることが好ましい。一方、S、Seの1種または2種の合計の含有量が0.05%を超える場合はスラブ加熱時の固溶が不完全となるだけでなく、製品表面の欠陥の原因ともなる場合がある。したがって、S、Seの含有量は、S又はSeの1種を含有する場合、SとSeの2種を含有する場合のいずれも合計で0.001〜0.05%の範囲が好ましい。
これらの粒子を用いることで、被膜張力、耐食性をより高めやすくなる。
TI=η(L)/η(H) ・・・(1)
また、上記速度変動としては、例えば、絶縁被膜処理液を方向性電磁鋼板の表面に塗布する製造ラインにおいて前記鋼板の搬送速度の最高速度と最低速度の差が50mpm以上となる製造条件が挙げられる。
板厚:0.20mmの仕上焼鈍済みの方向性電磁鋼板を準備した。この方向性電磁鋼板の磁束密度B8は1.920Tであった。この方向性電磁鋼板を、リン酸酸洗後、表1に記載の種々のクロムフリー絶縁被膜処理液を焼付け後の両面合計で8.0g/m2となるように塗布した。この際、前記絶縁被膜処理液を、ロールコーターを用いて方向性電磁鋼板を120mpmと240mpmの二水準の搬送速度で搬送して塗布した。その後、820℃、30秒、N2:100vol%雰囲気の条件で焼付け処理を行い、絶縁被膜付き方向性電磁鋼板を製造した。
金属元素を含む化合物の粒子としては、TiO2、ZrO2、HfO2、Nb2O5、V2O5、MgO、ZnOを使用した。いずれも粒径は0.1〜0.8μmの範囲であった。絶縁被膜処理液中の金属元素を含む化合物の粒径は、島津製作所製レーザ回折式粒度分布測定装置SALD−3100にて測定した。粒径は、平均粒径を示し、体積基準で50%粒子径つまり、メディアン径を示す。また、金属元素を含む化合物の粒子の含有量は金属元素で固形分換算したものを示した。
分散剤として用いた界面活性剤としては、花王株式会社製コータミン24P(第4級アンモニウム塩型カチオン系界面活性剤)を用い、その含有量を溶媒を含まない量で示した。
絶縁被膜処理液の比重は純水を用いて、1.180に調整した。
被膜処理液の粘度は東機産業製のB型粘度計にてNo.1ローターを用いて、液温20℃、回転数6rpmの時の粘度η(L)と、回転数60rpmの時の粘度η(H)を測定した。そして、下記(1)式から、チクソトロピーインデックス(TI)を算出した。
TI=η(L)/η(H) ・・・(1)
絶縁被膜処理液を、ロールコーターを用いて方向性電磁鋼板を120mpmと240mpmの二水準の搬送速度で搬送して塗布、焼付けした後の表面の状態を目視で観察し、以下のように評価した。以下の評価で○を合格とした。
両条件(120mpm、240mpm)でリビング欠陥無:○
どちらか一方の条件でリビング欠陥有:△120 または △240(△120は120mpmの条件でリビング欠陥が発生したことを意味し、△240は240mpmの条件でリビング欠陥が発生したことを意味する)
両方の条件でリビング欠陥有:×
鉄損(W17/50)は、JIS C 2550に規定された方法で、絶縁被膜付き方向性電磁鋼板から作成した幅30mm×長さ280mmの試験片を用いて測定を行った。鉄損(W17/50)0.88W/kg以下を合格とした。
鋼板への付与張力(被膜張力)は、圧延方向の張力とし、絶縁被膜付き方向性電磁鋼板から作成した圧延直角方向長さ30mm×圧延方向長さ280mmの試験片の一方の面を粘着テープでマスキングしてから、もう一方の面の絶縁被膜をアルカリ、酸などを用いて除去し、次いで前記試験片の片端30mmを固定して試験片250mmの部分を測定長さとして反り量を測定し、以下の式から求めた。なお、鋼板ヤング率は132GPaとした。付与張力10.0MPa以上を合格とした。
鋼板への付与張力(MPa)=鋼板ヤング率(GPa)×板厚(mm)×反り量(mm)÷(そり測定長さ(mm))2×103
耐吸湿性は、絶縁被膜付き方向性電磁鋼板から作製した50mm×50mmの試験片3枚を、100℃の蒸留水中で5分間浸漬煮沸することにより絶縁被膜表面からリンを溶出させ、その溶出量[μg/150cm2]をICP発光分析で定量分析して測定し評価した。リン溶出量100[μg/150cm2]以下を合格とした。
板厚:0.27mmの仕上焼鈍済みの方向性電磁鋼板を準備した。この方向性電磁鋼板の磁束密度B8は1.928Tであった。この方向性電磁鋼板を、リン酸酸洗後、表2に記載の種々のクロムフリー絶縁被膜処理液を焼付け後の両面合計で12.0g/m2となるように塗布した。この際、前記絶縁被膜処理液を、ロールコーターを用いて方向性電磁鋼板を100mpmと300mpmの二水準の搬送速度で搬送して塗布した。その後、900℃、30秒、N2:90vol%−H2:10vol%雰囲気の条件で焼付け処理を行い、絶縁被膜付き方向性電磁鋼板を製造した。
金属元素を含む化合物の粒子としては、日産株式会社製ZrO2ゾルナノユースZR30AHを使用し、その添加量はリン酸塩100質量部に対し金属元素(Zr)で固形分換算し20質量部とした。粒径は0.1μmであった(実施例1と同様に測定)。
分散剤として用いた界面活性剤としては、サンノプコ株式会社製SNディスパーサント4215(第4級アンモニウム塩型カチオン系界面活性剤)、花王株式会社製アセタミン24(アルキルアミン型カチオン系界面活性剤)を用い、それぞれの添加量を溶媒を含まない量で示した。
絶縁被膜処理液の比重は純水を用いて、1.250に調整した。
絶縁被膜処理液を、ロールコーターを用いて方向性電磁鋼板を100mpmと300mpmの二水準の搬送速度で搬送して塗布、焼付けした後の表面の状態を目視で観察し、以下のように評価した。以下の評価で○を合格とした。
両条件(100mpm、300mpm)でリビング欠陥無:○
どちらか一方の条件でリビング欠陥有:△100 または △300(△100は100mpmの条件でリビング欠陥が発生したことを意味し、△300は300mpmの条件でリビング欠陥が発生したことを意味する)
両方の条件でリビング欠陥有:×
板厚:0.23mmの仕上焼鈍済みの方向性電磁鋼板を準備した。この方向性電磁鋼板の磁束密度B8は1.923Tであった。この方向性電磁鋼板を、リン酸酸洗後、表3に記載の種々のクロムフリー絶縁被膜処理液を焼付け後の両面合計で10.0g/m2となるように塗布した。この際、前記絶縁被膜処理液を、ロールコーターを用いて方向性電磁鋼板を150mpmと380mpmの二水準の搬送速度で搬送して塗布した。その後、950℃、10秒、N2:85vol%−H2:15vol%雰囲気の条件で焼付け処理を行い、絶縁被膜付き方向性電磁鋼板を製造した。
金属元素を含む化合物の粒子としては、TiO2、ZrN、HfO2、MgOを用いた。添加量は金属元素で固形分換算したものを示した。これらの絶縁被膜処理液中の粒径は、実施例1と同様にして測定した。
絶縁被膜処理液の粘度特性を制御するため、表3に記載の無機酸を同表に記載された量添加した。添加量は無機酸以外の溶媒等を含まない量で示した。
絶縁被膜処理液の比重は純水を用いて、1.100に調整した。
絶縁被膜処理液を、ロールコーターを用いて方向性電磁鋼板を150mpmと380mpmの二水準の搬送速度で搬送して塗布、焼付けした後の表面の状態を目視で観察し、以下のように評価した。以下の評価で○を合格とした。
両条件(150mpm、380mpm)でリビング欠陥無:○
どちらか一方の条件でリビング欠陥有:△150 または △380(△150は150mpmの条件でリビング欠陥が発生したことを意味し、△380は380mpmの条件でリビング欠陥が発生したことを意味する)
両方の条件でリビング欠陥有:×
Claims (10)
- 方向性電磁鋼板の表面に、クロムフリー絶縁被膜を形成するための絶縁被膜処理液であって、
Mg、Ca、Ba、Sr、Zn、Al、Mnのリン酸塩のうちから選ばれる1種または2種以上のリン酸塩と、コロイド状シリカと、金属元素を含む化合物の粒子と、を含有し、
前記リン酸塩100質量部に対し、前記コロイド状シリカの含有量がSiO2固形分換算で50〜120質量部であり、かつ、前記金属元素を含む化合物の粒子の含有量が金属元素換算で5〜60質量部であり、
チクソトロピーインデックス(TI)が1.00以上10.00以下である、絶縁被膜処理液。 - 金属元素を含む化合物の粒子が、Ti、Zr、Hf、V、Mg、Zn、Nbの酸化物の粒子、Ti、Zr、Hf、V、Mg、Zn、Nbの窒化物の粒子のうちから選ばれる1種または2種以上である、請求項1に記載の絶縁被膜処理液。
- 金属元素を含む化合物の粒子が、TiO2、ZrO2、HfO2、MgO、ZnO、Nb2O5、V2O5、TiN、ZrNの粒子から選ばれる1種または2種以上である、請求項1または2に記載の絶縁被膜処理液。
- 金属元素を含む化合物の粒子の粒径が0.05μm以上1.0μm以下である、請求項1〜3のいずれかに記載の絶縁被膜処理液。
- さらにカチオン系界面活性剤を含有する、請求項1〜4のいずれかに記載の絶縁被膜処理液。
- カチオン系界面活性剤が第4級アンモニウム塩型カチオン系界面活性剤である、請求項5に記載の絶縁被膜処理液。
- カチオン系界面活性剤の含有量が、Mg、Ca、Ba、Sr、Zn、Al、Mnのリン酸塩のうちから選ばれる1種または2種以上のリン酸塩100質量部に対し、0.20〜2.0質量部である、請求項5または6に記載の絶縁被膜処理液。
- 請求項1〜7のいずれかに記載の絶縁被膜処理液を焼付けしてなる絶縁被膜を表面に備える、絶縁被膜付き方向性電磁鋼板。
- 請求項1〜7のいずれかに記載の絶縁被膜処理液を、方向性電磁鋼板の表面に塗布した後、焼付けする、絶縁被膜付き方向性電磁鋼板の製造方法。
- 絶縁被膜処理液を方向性電磁鋼板の表面に塗布する際、前記方向性電磁鋼板を搬送しながら、前記絶縁被膜処理液をロールコーターを用いて前記方向性電磁鋼板の表面に塗布する、請求項9に記載の絶縁被膜付き方向性電磁鋼板の製造方法。
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