CN116745444A - 方向性电磁钢板的制造方法 - Google Patents
方向性电磁钢板的制造方法 Download PDFInfo
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- CN116745444A CN116745444A CN202280010404.1A CN202280010404A CN116745444A CN 116745444 A CN116745444 A CN 116745444A CN 202280010404 A CN202280010404 A CN 202280010404A CN 116745444 A CN116745444 A CN 116745444A
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- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 19
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 19
- 239000010959 steel Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 10
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- 238000005098 hot rolling Methods 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 239000003112 inhibitor Substances 0.000 abstract description 17
- 239000011248 coating agent Substances 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 10
- 238000000746 purification Methods 0.000 description 20
- 238000003756 stirring Methods 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 238000001953 recrystallisation Methods 0.000 description 8
- 238000010008 shearing Methods 0.000 description 8
- 238000005097 cold rolling Methods 0.000 description 7
- 238000005261 decarburization Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 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
- 229910052758 niobium Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004993 emission spectroscopy Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000011817 metal compound particle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000009036 growth inhibition Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
本发明提供一种通过有效地纯化抑制剂来稳定地制造磁特性优异的方向性电磁钢板的方法。上述方向性电磁钢板的制造方法中使用含有规定量的Ti、Zr、Hf、V、Nb以及Ta中的任一种以上的钢坯，相对于MgO：100质量份添加1～10质量份的金属化合物的退火分离剂，以在钢板表面上金属化合物的粒径：1μm以上的粒子的比率为0.0010个/μm2以下进行涂布。
Description
技术领域
本发明涉及一种方向性电磁钢板的制造方法，特别是涉及一种在将Ti、Zr、Hf、V、Nb、Ta用作抑制剂的情况下，促进其纯化，稳定地制造磁特性优异的方向性电磁钢板的方法。
背景技术
方向性电磁钢板主要是用于变压器等铁芯的软磁性材料，作为其磁特性，要求低铁损且高磁通密度。该方向性电磁钢板利用二次再结晶现象将称为Goss取向的{110}＜001＞取向集成在钢板组织中进行制造。
并且，作为提高该Goss取向的集成度的方法，通常是利用称为抑制剂的析出物、例如MnS、MnSe以及AlN对二次再结晶进行控制。
然而，近年来，出于节能化的目的，低铁损且高磁通密度的方向性电磁钢板的需求不断增加。作为制造该方向性电磁钢板的方法，例如专利文献1和2中提出了将Nb等用作抑制剂的方法。Nb等能够增强晶粒生长的抑制力，提高Goss取向的集成度。
这里，抑制剂需要从钢中除去(纯化)，但作为促进抑制剂的纯化的方法，例如专利文献3中提出了通过降低纯化退火的氮分压来促进氮的纯化的方法。
现有技术文献
专利文献
专利文献1：日本特开平6－25747号公报
专利文献2：日本特开2008－115421号公报
专利文献3：日本特开平9－143562号公报
发明内容
如上所述，在使用抑制剂的情况下，如果抑制剂残存于产品，则阻碍磁畴壁移动，增大铁损。因此，需要最终退火时实施二次再结晶退火后，通过在高温下实施纯化退火而将其分解，从钢中除去(纯化)。
然而，如专利文献1和2记载的方法那样在将Ti、Zr、Hf、V、Nb或者Ta(以下也称为Nb等)用作抑制剂的情况下，存在无法将它们纯化的问题。即存在在高温下分解的Nb等再次析出，该析出物使铁损增大的问题。
另外，在上述专利文献3记载的方法中，存在即使能够将氮纯化，也无法使Nb等纯化，铁损增大的问题。
本发明有利地解决了上述的问题，目的在于特别是提出了通过有效地纯化Nb等抑制剂而稳定地制造磁特性优异的方向性电磁钢板的方法。
发明人等为了解决上述的问题，反复深入地进行了研究，其结果新发现了通过使用金属化合物均匀分散的退火分离剂进行最终退火，能够促进Ti、Zr、Hf、V、Nb以及Ta的氧化，促进它们的纯化。
本发明是基于上述见解进一步研究而完成的。即，本发明的构成主旨如下。
1.一种方向性电磁钢板的制造方法，其特征在于，包括如下的一系列工序：对如下的钢坯实施热轧，实施一次或隔着中间退火的二次以上的冷轧后，实施脱碳退火，接着涂布退火分离剂，实施最终退火，所述钢坯以质量％计含有C：0.01～0.1％、Si：2.0～5.0％以及Mn：0.01～1％、进一步合计含有0.0010～0.0100％的Ti、Zr、Hf、V、Nb以及Ta中的任一种或者两种以上，剩余部分为Fe和不可避免的杂质，
上述退火分离剂为相对于MgO：100质量份添加金属化合物：1～10质量份，以钢板表面上述金属化合物中粒径1μm以上的粒子的比率为0.0010个/μm2以下涂布上述退火分离剂。
2.根据上述1所述的方向性电磁钢板的制造方法，其特征在于，上述金属化合物为选自Ti、Cr、Mo、W、Mn、Zn、Sn、Pb、Sb以及Bi中的至少一种氧化物、氢氧化物、硝酸盐以及硫酸盐中的任一种以上。
3.根据上述1或2所述的方向性电磁钢板的制造方法，其特征在于，上述钢坯以质量％计进一步含有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％以及Bi：0.001～0.05％中的任一种或者两种以上。
根据本发明，即使特别是在将Ti、Zr、Hf、V、Nb以及Ta中的任1种或者2种以上用作抑制剂的情况下，通过使用金属化合物均匀地分散的退火分离剂进行最终退火，也能够促进该纯化，稳定地制造磁特性优异的方向性电磁钢板。
附图说明
图1是对以10s－1和15s－1的剪切速度进行搅拌的情况下的SnO2的分散状态进行比较的图。
具体实施方式
以下，对作为开发本发明的契机的实验进行说明。
对以质量％计含有C：0.03％、N：0.004％、Al：0.007％、Si：3.2％、Mn：0.06％、进一步含有作为抑制剂成分的Nb：0.0070％、剩余部分由Fe和不可避免的杂质构成的钢坯，在1380℃、30分钟的条件下进行加热，进一步实施热轧后，实施冷轧，接着在1050℃、1分钟的条件下实施中间退火，进一步再次实施冷轧而制成0.23mm厚度的冷轧板。对该冷轧板在湿氢气氛中，在840℃、2分钟的条件下实施脱碳退火。
然后，对上述脱碳退火后的11片冷轧板，如表1所示对其中6片冷轧板应用相对于MgO：100质量份添加5质量份的SnO2的退火分离剂，对剩余的5片冷轧板应用利用MgO的退火分离剂。任一退火分离剂均是在改变剪切速度进行搅拌后涂布于冷轧板的表面，在850℃、50小时的条件下实施了二次再结晶退火后，在干氢气氛中，在1200℃、5小时的条件下实施纯化退火，并且涂布以磷酸盐作为主体的涂层，在850℃、1分钟的条件下实施平坦化退火，制成试验片。然后，进行该试验片的磁性测定，并且从该试验片除去被膜后，进行Nb的分析。
应予说明，磁性测定按照JISC2550的规定进行，另外，成分分析使用发射光谱分析进行。另外，在使用未添加SnO2的退火分离剂的情况下，也与上述测定等同样地进行测定等。
将各测定等结果一并标注于表1。
[表1]
表1
如该表所示，在添加了SnO2的情况下，特别是以15s－1以上的剪切速度进行搅拌时，Nb小于10质量ppm(0.0010质量％)，促进纯化。
该促进纯化的原因的细节尚不明确，但发明人等考虑如下。
即二次再结晶退火中，已知Nb以NbN的形式析出，使通过抑制剂抑制钢板组织的晶粒生长的力增强，在更高温的纯化退火中，其分解，N和Nb分别固溶。这里，在该纯化退火时，如果添加SnO2，则与SnO2相比Nb2O5更稳定，因此认为在钢板的表层发生以下的反应，从而Nb被氧化，纯化进行。
4Nb+5SnO2→2Nb2O5+5Sn
另外，认为该氧化反应的结果是产生Nb的活性梯度，Nb扩散，从而Nb以Nb2O5的形式进入到被膜和退火分离剂中，促进该纯化。
应予说明，为了评价SnO2的分散状态，对钢板涂布退火分离剂，烧结后，使用扫描式电子显微镜，在其表面选择750μm2左右大小的视场中的10个视场左右，在倍率：2000倍的条件下进行观察。
将在退火分离剂中添加SnO2后，分别观察以10s－1和15s－1的剪切速度进行了搅拌的情况下的SnO2的分散状态的结果示于图1。
如该图所示，在剪切速度慢的情况下，随处可见粒径为1μm以上的SnO2粒子。另一方面，在剪切速度快的情况下，几乎看不到这样的粒子。具体而言，以10s－1的剪切速度进行搅拌的情况下，粒径为1μm以上的SnO2粒子的比率为0.0080个/μm2左右，与此相对，以15s－1的剪切速度搅拌的情况下，该比率为0.0010个/μm2以下。
根据该结果，认为在添加SnO2后的搅拌中，在剪切速度慢的情况下，SnO2凝聚，其分布产生不均，粒径为1μm以上的SnO2粒子的比率达不到0.0010个/μm2以下。因此，认为Nb的氧化变得不均匀，该纯化不会被促进。
接下来，对本发明的退火分离剂的成分组成进行说明。
在本发明中，SnO2这样的金属化合物是促进钢板的纯化的重要成分，含量相对于MgO：100质量份不足1质量份时得不到充分的效果。另一方面，如果超过10质量份，则MgO的比率降低，被膜特性、甚至是磁特性劣化。因此，在本发明中限定为1～10质量份的范围。
本发明的上述金属化合物被用作抑制剂的元素所分解，如果该金属化合物中的金属具有氧化物、氢氧化物、硝酸盐和硫酸盐，则这些金属化合物均可以优选使用。认为用作抑制剂的元素以代替该金属化合物的金属而作为化合物进入到被膜和退火分离剂中的形态促进该纯化。
应予说明，更具体而言，上述金属化合物为选自Ti、Cr、Mo、W、Mn、Zn、Sn、Pb、Sb和Bi中的至少一种氧化物、氢氧化物、硝酸盐以及硫酸盐中的任一种以上。
另外，本发明中，出于改善被膜特性和磁特性的目的，可以在该退火分离剂中一并添加以往公知的Li、Na、Mg、Al、Si、K、Ca、Ti、V、Fe、Co、Ni、Cu、Sr、Ba、镧的氧化物、氢氧化物、硼酸盐、碳酸盐、硝酸盐、磷酸盐、硫酸盐、卤化物。
应予说明，这些化合物可以单独使用，也可以使用多种。在使用该化合物的情况下，作为含量，相对于MgO：100质量份优选0.01～15质量份的范围。如果比0.01质量份少，则得不到充分的效果，另一方面，如果比15质量份多，则过度促进被膜形成，或者上述的抑制力过度增强，导致磁特性劣化。
接下来，对钢坯的成分组成进行说明。
C是对于改善织构很重要的元素，如果含量不满足0.01质量％，则无法得到足够的效果，另一方面，如果超过0.1质量％，则脱碳很困难，使磁特性劣化。因此，在本发明中，限定为0.01～0.1质量％的范围。
Si是是增大比电阻、改善涡流损耗很重要的元素，如果含量不满足2.0质量％，则得不到充分的效果，另一方面，如果超过5.0质量％，则使冷轧性劣化。因此，在本发明中限定为2.0～5.0质量％的范围。
Mn与Si相同地增大比电阻，改善涡流损耗。另外，是改善热轧性很重要的元素，但含量不满足0.01质量％时，无法得到充分的效果，另一方面，如果超过1质量％，则引起γ相变，使磁特性劣化。因此，在本发明中限定为0.01～1质量％的范围。
Ti、Zr、Hf、V、Nb和Ta是增强上述的抑制力、改善磁特性很重要的元素，但含量合计不足0.0010质量％时得不到充分的效果，另一方面，如果超过0.0100质量％，则难以进行该纯化。因此，本发明中，Ti、Zr、Hf、V、Nb以及Ta中的任一种或者两种以上合计限定为0.0010～0.0100质量％的范围。
另外，本发明中可以将一般的方向性电磁钢板中使用的MnS、MnSe、以及AlN等用作抑制剂。在使用MnS或者MnSe的情况下，优选添加0.01～1质量％的Mn、以及0.002～0.03质量％的S或者0.002～0.03质量％的Se。另一方面，在使用AlN的情况下，优选添加0.004～0.04质量％的Al以及0.002～0.01质量％的N。应予说明，上述抑制剂可以单独使用，也可以使用多种。
并且，除了上述成分之外，出于改善磁特性的目的，以质量％计可以适当地添加B：0.0001～0.005％、P：0.005～0.1％、Cr：0.01～0.5％、Ni：0.01～1.5％、Cu：0.01～0.5％、Mo：0.005～0.1％、Sn：0.005～0.5％、Sb：0.005～0.5％以及Bi：0.001～0.05％中的任一种或者两种以上。
接下来，对本发明的方向性电磁钢板的制造方法进行说明。
对调整为上述优选的成分组成的钢坯，按照公知的方法实施热轧，根据需要实施热轧板退火，实施一次或者隔着中间退火的二次以上的冷轧，制成最终板厚，进一步进行脱碳退火，接着涂布相对于MgO：100质量份添加1～10质量份的金属化合物的退火分离剂。这里，在本发明中，对搅拌的方式没有特别限定，例如优选在使用搅拌翼的情况下，通过改变其旋转速度，并且使用静态混合器的情况下，改变排出压力，从而调整剪切速度来进行搅拌。应予说明，进行该搅拌时，优选以15s－1以上的剪切速度进行搅拌。这是因为从钢板表面观察时，该粒径为1μm以上的金属化合物的粒子的比率为0.0010个/μm2以下。应予说明，上述金属化合物的粒子的比率优选为0.0005个/μm2以下。另一方面，该下限没有特别限定，可以为0个/μm2。另外，上述剪切速度更优选为20s－1以上。另一方面，该上限并没有特别限定，但工业上为300s－1左右。
并且，在脱碳退火后，根据需要实施氮化处理对磁特性改善有利。
然后，实施二次再结晶退火后，实施纯化退火，根据需要实施绝缘涂布、平坦化退火以及磁畴细化处理，制成作为最终产品的方向性电磁钢板。
应予说明，本发明的制造方法中，本说明书中没有记载的项目均可以使用常规方法。
实施例
[实施例1]
对以质量％计含有C：0.03％、N：0.004％、Al：0.007％、Si：3.2％、Mn：0.06％、Nb：0.0050％、剩余部分由Fe和不可避免的杂质构成的钢坯，在1380℃、30分钟的条件下实施板坯加热，实施热轧，进一步实施冷轧后，在1050℃下1分钟的条件下实施中间退火，再次实施冷轧，制成0.23mm的冷轧板，在湿氢气氛中，在840℃、2分钟的条件下进行脱碳退火，制成脱碳退火板。在该脱碳退火板中，相对于MgO：100质量份，添加作为金属化合物的表2记载的各种氧化物，以表2记载的剪切速度涂布经过搅拌的退火分离剂后，实施850℃、50小时的条件的二次再结晶退火、进而实施1200℃、5小时的条件的纯化退火，接着，涂布以磷酸盐作为主体的涂层后，在850℃、1分钟的条件下实施平坦化退火，制成试验片。
然后，进行该试验片的磁性测定，进一步除去被膜后，进行Nb的分析。应予说明，磁性测定基于JISC2550，成分分析使用发射光谱分析法进行。
将各测定和分析结果一并标注于表2。
如该表所示可知，在使用本发明的情况下，Nb量充分地减少(纯化)的同时，磁特性得到改善。
[实施例2]
对含有表3记载的各种成分的钢坯，在1380℃、30分钟的条件下实施板坯加热，实施热轧，进一步实施冷轧后，在1050℃、1分钟的条件下实施中间退火，再次实施冷轧而制成0.23mm的冷轧板，在湿氢气氛中，在840℃、2分钟的条件下进行脱碳退火，制成脱碳退火板。对该脱碳退火板，相对于MgO：100质量份添加5质量份的作为金属化合物的MoO3，涂布以15s－1的剪切速度进行经搅拌的退火分离剂后，实施850℃、50小时的条件的二次再结晶退火，进而实施1200℃、5小时的条件的纯化退火，接着，涂布以磷酸盐作为主体的涂层后，在850℃、1分钟的条件下实施平坦化退火，制成试验片。应予说明，1μm以上的粒径的粒子的比率中任一试验片均为0.0010〔个/μm2〕以下。
然后，进行该试验片的磁性测定，进一步除去被膜后，进行成分分析。应予说明，磁性测定按照JISC2550进行，成分分析使用发射光谱分析法进行。
将各测定和分析结果一并标注于表3。
如该表所示可知，在使用本发明的情况下，在充分地减少(纯化)各元素的同时，改善了磁特性。
Claims (3)
1.一种方向性电磁钢板的制造方法，其特征在于，包括如下的一系列工序：对如下的钢坯实施热轧，实施一次或隔着中间退火的二次以上的冷轧后，实施脱碳退火，接着涂布退火分离剂，实施最终退火，所述钢坯以质量％计含有C：0.01～0.1％、Si：2.0～5.0％和Mn：0.01～1％，进一步合计含有0.0010～0.0100％的Ti、Zr、Hf、V、Nb以及Ta中的任一种或者两种以上，剩余部分为Fe和不可避免的杂质，
所述退火分离剂为相对于MgO：100质量份添加金属化合物：1～10质量份，以钢板表面所述金属化合物中粒径1μm以上的粒子的比率为0.0010个/μm2以下涂布所述退火分离剂。
2.根据权利要求1所述的方向性电磁钢板的制造方法，其特征在于，所述金属化合物为选自Ti、Cr、Mo、W、Mn、Zn、Sn、Pb、Sb以及Bi中的至少一种氧化物、氢氧化物、硝酸盐以及硫酸盐中的任一种以上。
3.根据权利要求1或2所述的方向性电磁钢板的制造方法，其特征在于，所述钢坯以质量％计进一步含有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％以及Bi：0.001～0.05％中的任一种或者两种以上。
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| JPS6123771A (ja) * | 1984-07-12 | 1986-02-01 | Nippon Steel Corp | 方向性電磁鋼板のグラス皮膜形成方法 |
| JPS6179781A (ja) * | 1984-09-27 | 1986-04-23 | Nippon Steel Corp | 方向性電磁鋼板のグラス皮膜形成方法 |
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