JP7459939B2 - 方向性電磁鋼板の製造方法 - Google Patents
方向性電磁鋼板の製造方法 Download PDFInfo
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- JP7459939B2 JP7459939B2 JP2022528169A JP2022528169A JP7459939B2 JP 7459939 B2 JP7459939 B2 JP 7459939B2 JP 2022528169 A JP2022528169 A JP 2022528169A JP 2022528169 A JP2022528169 A JP 2022528169A JP 7459939 B2 JP7459939 B2 JP 7459939B2
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- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 title claims description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000000137 annealing Methods 0.000 claims description 48
- 229910000831 Steel Inorganic materials 0.000 claims description 20
- 239000010959 steel Substances 0.000 claims description 20
- 150000002736 metal compounds Chemical class 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 229910052758 niobium Inorganic materials 0.000 claims description 12
- 229910052720 vanadium Inorganic materials 0.000 claims description 10
- 229910052735 hafnium Inorganic materials 0.000 claims description 9
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052715 tantalum Inorganic materials 0.000 claims description 8
- 229910052787 antimony Inorganic materials 0.000 claims description 7
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 229910052718 tin Inorganic materials 0.000 claims description 7
- 238000005261 decarburization Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000005097 cold rolling Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052745 lead Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 20
- 238000000746 purification Methods 0.000 description 19
- 239000003112 inhibitor Substances 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000005259 measurement Methods 0.000 description 10
- 238000001953 recrystallisation Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910006404 SnO 2 Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011817 metal compound particle Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Description
1.質量%で、C:0.01~0.1%、Si:2.0~5.0%およびMn:0.01~1%を含有し、さらにTi、Zr、Hf、V、NbおよびTaのうちのいずれか一種、または二種以上を合計で0.0010~0.0100%含有し、残部がFeおよび不可避的不純物である鋼スラブに、熱間圧延を施し、一回、または中間焼鈍を挟む二回以上の冷間圧延を施した後、脱炭焼鈍を施し、次いで焼鈍分離剤を塗布して、仕上げ焼鈍を施す一連の工程からなる方向性電磁鋼板の製造方法であって、
上記焼鈍分離剤は、MgO:100質量部に対して金属化合物:1~10質量部添加し、上記金属化合物のうち粒子径:1μm以上の粒子の比率を、鋼板表面において0.0010個/μm2以下として塗布することを特徴とする方向性電磁鋼板の製造方法。
質量%で、C:0.03%、N:0.004%、Al:0.007%、Si:3.2%、Mn:0.06%を含有し、さらにインヒビター成分としてNb:0.0070%を含有し、残部がFeおよび不可避的不純物からなる鋼スラブを、1380℃、30分間の条件で加熱し、さらに熱間圧延を施した後、冷間圧延を施し、次いで、1050℃、1分間の条件で中間焼鈍を施し、さらに再度冷間圧延を施して0.23mm厚の冷延板とした。かかる冷延板に、湿水素雰囲気中、840℃、2分間の条件で脱炭焼鈍を施した。
なお、磁気測定はJISC2550の規定に準じ、また、成分分析は発光分光分析を用いて行った。さらに、SnO2を添加しない焼鈍分離剤を用いた場合も上記測定等と同様に測定等を行った。
それぞれの測定等の結果を表1に併記する。
この純化の促進の理由の詳細は明らかではないが、発明者らは、以下のように考えている。
すなわち、二次再結晶焼鈍では、NbはNbNとして析出し、インヒビターによる鋼板組織の粒成長を抑制する力を強化することが知られているが、より高温の純化焼鈍では、これが分解し、NとNbがそれぞれ固溶する。ここで、かかる純化焼鈍時に、SnO2が添加されると、SnO2よりもNb2O5の方が安定であるため、鋼板の表層では、以下の反応が生じることによって、Nbが酸化して純化が進むものと考えられる。
4Nb+5SnO2→2Nb2O5+5Sn
なお、SnO2の分散状態を評価するため、鋼板に焼鈍分離剤を塗布し、焼き付けた後、走査型電子顕微鏡を用いて、その表面を、750μm2程度大きさの視野を10視野程度選択し、倍率:2000倍の条件で、観察した。
同図に示すように、せん断速度が遅い場合、粒子径が1μm以上のSnO2粒子が随所に確認された。一方、せん断速度が速い場合、かような粒子はほとんど確認されなかった。具体的には、10s-1のせん断速度で撹拌した場合、粒子径が1μm以上のSnO2粒子の比率が0.0080個/μm2程度であったのに対し、15s-1のせん断速度で撹拌した場合、その比率は0.0010個/μm2以下になった。
本発明において、SnO2のような金属化合物は鋼板の純化を促進するために重要な成分であるが、含有量が、MgO:100質量部に対して、1質量部に満たないと十分な効果が得られない。その一方で、10質量部を超えると、MgOの比率が低減し、被膜特性、ひいては磁気特性を劣化する。そのため、本発明では1~10質量部の範囲に限定した。
なお、より具体的には、前記金属化合物が、Ti、Cr、Mo、W、Mn、Zn、Sn、Pb、SbおよびBiのうちから選んだ少なくとも一種の酸化物、水酸化物、硝酸塩および硫酸塩のうちのいずれか一種以上である。
なお、これらの化合物は単体で用いても良いし、複数で用いても良い。かかる化合物を用いる場合は、含有量として、MgO:100質量部に対して、0.01~15質量部の範囲が好ましい。0.01質量部より少ないと十分な効果が得られない一方で、15質量部より多いと被膜形成が促進されすぎたり、前述した抑制力が強化されすぎたりして、磁気特性が劣化する。
Cは、集合組織を改善するために重要な元素であるが、含有量が0.01質量%に満たないと十分な効果が得られない一方で、0.1質量%を超えると、脱炭が困難になり、磁気特性を劣化する。そのため、本発明では0.01~0.1質量%の範囲に限定した。
上記好適な成分組成に調整した鋼スラブに、公知の方法に従い、熱間圧延を施し、必要に応じて熱延板焼鈍を施し、一回、または中間焼鈍を挟む二回以上の冷間圧延を施して最終板厚とし、さらに脱炭焼鈍し、次いで、MgO:100質量部に対して、金属化合物を1~10質量部添加した焼鈍分離剤を塗布する。ここで、本発明において、撹拌の方式につき、特に限定するものではないが、例えば、撹拌翼を用いる場合は、その回転速度を変えることによって、またスタティックミキサーを用いる場合は、吐出圧力を変えることによって、せん断速度を調整して撹拌することが好ましい。なお、かかる撹拌の際、15s-1以上のせん断速度で撹拌することが好ましい。これは、鋼板表面から見て、その粒子径が1μm以上である金属化合物の粒子の比率を0.0010個/μm2以下にするためである。なお、上記金属化合物の粒子の比率は、0.0005個/μm2以下が好ましい。一方、その下限は特に限定されず、0個/μm2であって良い。また、上記せん断速度は、20s-1以上であることがより好ましい。一方、その上限は特に限定されないが、工業的には300s-1程度である。
さらに、脱炭焼鈍後に、必要に応じて、窒化処理を施すことは磁気特性改善に有利である。
なお、本発明の製造方法では、本明細に記載のない項目は、いずれも常法を用いることができる。
質量%で、C:0.03%、N:0.004%、Al:0.007%、Si:3.2%、Mn:0.06%、Nb:0.0050%を含有し、残部がFeおよび不可避的不純物からなる鋼スラブに、1380℃、30分間の条件でスラブ加熱を施して、熱間圧延を施し、さらに冷間圧延を施した後、1050℃、1分間の条件で中間焼鈍を施し、再度冷間圧延を施して0.23mmの冷延板とし、湿水素雰囲気中、840℃、2分間の条件で脱炭焼鈍し脱炭焼鈍板とした。かかる脱炭焼鈍板にMgO:100質量部に対して、金属化合物として表2に記載する各種酸化物を添加して表2に記載するせん断速度で撹拌した焼鈍分離剤を塗布した後、850℃、50時間の条件の二次再結晶焼鈍、さらには1200℃、5時間の条件の純化焼鈍を施し、次いで、リン酸塩を主体とするコーティングを塗布した後、850℃、1分間の条件で平坦化焼鈍を施し試験片とした。
その後、かかる試験片の磁気測定を行い、さらに被膜を除去した後、Nbの分析を行った。なお、磁気測定はJISC2550に準じ、成分分析は発光分光分析法を用いて行った。
それぞれの測定および分析結果を表2に併記する。
表3に記載の各種成分を含有する鋼スラブに、1380℃、30分間の条件でスラブ加熱を施して、熱間圧延を施し、さらに冷間圧延を施した後、1050℃、1分間の条件で中間焼鈍を施し、再度冷間圧延を施して0.23mmの冷延板とし、湿水素雰囲気中、840℃、2分間の条件で脱炭焼鈍し脱炭焼鈍板とした。かかる脱炭焼鈍板に、MgO:100質量部に対して、金属化合物としてMoO3を5質量部添加して15s-1のせん断速度で撹拌した焼鈍分離剤を塗布した後、850℃、50時間の条件の二次再結晶焼鈍、さらには1200℃、5時間の条件の純化焼鈍を施し、次いで、リン酸塩を主体とするコーティングを塗布した後、850℃、1分間の条件で平坦化焼鈍を施し試験片とした。なお、1μm以上の粒子径の粒子の比率は、何れの試験片も0.0010〔個/μm2〕以下であった。
その後、かかる試験片の磁気測定を行い、さらに被膜を除去した後、成分分析を行った。なお、磁気測定はJISC2550に準じ、成分分析は発光分光分析法を用いて行った。
それぞれの測定および分析結果を表3に併記する。
Claims (2)
- 質量%で、C:0.01~0.1%、Si:2.0~5.0%およびMn:0.01~1%を含有し、さらにTi、Zr、Hf、V、NbおよびTaのうちのいずれか一種、または二種以上を合計で0.0010~0.0100%含有し、残部がFeおよび不可避的不純物である鋼スラブに、熱間圧延を施し、一回、または中間焼鈍を挟む二回以上の冷間圧延を施した後、脱炭焼鈍を施し、次いで焼鈍分離剤を塗布して、仕上げ焼鈍を施す一連の工程からなる方向性電磁鋼板の製造方法であって、
上記焼鈍分離剤は、MgO:100質量部に対して金属化合物:1~10質量部添加し、上記金属化合物のうち粒子径:1μm以上の粒子の比率を、鋼板表面において0.0010個/μm2以下として塗布し、
前記金属化合物が、Ti、Cr、Mo、W、Mn、Zn、Sn、Pb、SbおよびBiのうちから選んだ少なくとも一種の酸化物、水酸化物、硝酸塩および硫酸塩のうちのいずれか一種以上である(但し、前記鋼スラブについて、上記Ti、Zr、Hf、V、NbおよびTaのうちからTiのみが選択され、かつ、前記金属化合物について、上記Ti、Cr、Mo、W、Mn、Zn、Sn、Pb、SbおよびBiのうちからTiのみが選択される場合を除く)、
ことを特徴とする方向性電磁鋼板の製造方法。 - 前記鋼スラブが、さらに質量%で、B:0.0001~0.005%、N:0.002~0.01%、Al:0.004~0.04%、P:0.005~0.1%、S:0.002~0.03%、Cr:0.01~0.5%、Ni:0.01~1.5%、Cu:0.01~0.5%、Se:0.002~0.03%、Mo:0.005~0.1%、Sn:0.005~0.5%、Sb:0.005~0.5%、およびBi:0.001~0.05%のうちのいずれか一種、または二種以上を含有することを特徴とする、請求項1に記載の方向性電磁鋼板の製造方法。
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