CN114207158A - 无方向性电磁钢板及其制造方法 - Google Patents
无方向性电磁钢板及其制造方法 Download PDFInfo
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- CN114207158A CN114207158A CN202080054575.5A CN202080054575A CN114207158A CN 114207158 A CN114207158 A CN 114207158A CN 202080054575 A CN202080054575 A CN 202080054575A CN 114207158 A CN114207158 A CN 114207158A
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- electrical steel
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- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
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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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- C23C22/07—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 containing phosphates
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
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- C21D6/001—Heat treatment of ferrous alloys containing Ni
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- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C21D6/005—Heat treatment of ferrous alloys containing Mn
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- C21D6/008—Heat treatment of ferrous alloys containing Si
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- C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
- C21D8/1233—Cold rolling
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- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1283—Application of a separating or insulating coating
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- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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Abstract
本发明提供一种即便减薄绝缘被膜,该被膜的密合性也优异的无方向性电磁钢板。本发明的无方向性电磁钢板在钢板的至少单面具有绝缘被膜,所述绝缘被膜在表面侧和与基体铁的界面侧这两方具有P浓度比所述基体铁中的P浓度高的P稠化层。
Description
技术领域
本发明涉及一种无方向性电磁钢板及其制造方法。
背景技术
无方向性电磁钢板是广泛用作马达等铁芯材料的软磁性材料中的一种。近年来,电动汽车、混合动力汽车的实用化进展,马达的驱动系统得到发展,马达的驱动频率有逐年增加的趋势。目前,通常驱动频率为几百~几kHz,高频率区域的铁芯的铁损特性越来越受到重视。因此,通过添加Si和Al等合金元素或者降低板厚等来实现高频区域的低铁损化。另外,对通过控制板厚方向的Si浓度分布来改善高频区域的铁损特性的技术等也进行了研究。
这些技术中,由于减少板厚会使高频区域的铁损的改善效果非常好,因此对近年来的电磁钢板进行了薄板化。另一方面,因薄板化而导致层叠电磁钢板而制造的马达磁芯的占空系数降低成为课题,在制造马达时,产生扭矩降低等问题。其原因是形成于钢板表面的绝缘被膜的厚度不变,但是板厚变薄,使除去了绝缘被膜的电磁钢板部分在铁芯中所占的相对比例降低。根据上述的背景,为了不使占空系数降低,对形成于电磁钢板的表面的绝缘被膜,要求比目前为止更薄的薄度。为了满足绝缘被膜的薄膜化,研究了各种技术。
例如,专利文献1中记载了通过在绝缘被膜中含有20mg/m2~160mg/m2的C,从而制造绝缘被膜的密合性优异的电磁钢板的技术。
现有技术文献
专利文献
专利文献:日本专利第3603385号公报。
发明内容
然而,迄今为止的技术中,在减薄绝缘被膜的情况下,无法充分确保钢板与绝缘被膜的密合性,改善板厚薄的电磁钢板的占空系数并不充分。
本发明是鉴于上述问题而完成的,目的在于提供一种即便减薄绝缘被膜,该被膜的密合性也优异的电磁钢板及其制造方法。
发明人等为了解决上述课题,着眼于绝缘被膜的表面、以及电磁钢板与绝缘被膜的界面的P(磷)的稠化状态,进行了深入的研究。研究的结果,新发现了通过在绝缘被膜的表面侧以及与构成电磁钢板的基体铁的界面侧这两方使P稠化,得到绝缘被膜优异的密合性,从而完成了本发明。对于该机理,发明人等如下考虑。通过在绝缘被膜的表面侧和与基体铁的界面侧这两方使P稠化,从而被膜本身变得稳固,并且在与基体铁的界面侧稠化的P作为基体铁与绝缘被膜间的粘合剂发挥作用。根据该效果,即使绝缘被膜本身变薄,也可得到具有稳固且密合性高的绝缘被膜的电磁钢板。无论绝缘被膜是有机系、无机系或者其混合等、种类、结构等如何,均可得到该效果。
另外,作为在绝缘被膜的与基体铁的界面侧使P稠化的方法,可以使以板坯为代表的出钢成分中含有0.005~0.20质量%的P,以1100℃以上进行最终退火,也可以使用在最终冷轧的轧制油中以1%以上的浓度含有磷酸酯型的乳化剂的轧制油,使P附着于钢板表面。另外,在最终退火与最终冷轧之间实施涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥的工序也能够在绝缘被膜的与基体铁的界面侧形成P稠化层,得到发明的效果。
另一方面,对于绝缘被膜的表面侧的P稠化层而言,在形成绝缘被膜的过程中,如果使用在涂布液体中添加了1质量份以上的磷酸化合物等,则在该液体干燥时,P在绝缘被膜的表面浮上,能够形成稠化层。
根据以上的组合,通过在绝缘被膜的表面侧和与基体铁的界面侧这两者形成P稠化层,能够得到即使绝缘被膜薄,被膜密合性也优异的电磁钢板。
以下,记载本发明的主要构成。
(1)一种无方向性电磁钢板,在钢板的至少单面具有绝缘被膜的电磁钢板中,所述绝缘被膜在表面侧和与基体铁的界面侧这两方具有P浓度比所述基体铁的P浓度更高的P稠化层。
(2)根据上述(1)所述的无方向性电磁钢板,其中,所述钢板以质量%计具有如下成分组成,含有C:小于0.010%、Si:1.5%~10.0%、Al:0.001%~2.0%和Mn:0.005%~1.0%,且剩余部分为Fe和不可避免的杂质。
(3)根据上述(2)所述的无方向性电磁钢板,其中,所述钢板以质量%计进一步含有P:0.005%~0.20%。
(4)根据上述(2)或(3)所述的无方向性电磁钢板,其中,所述成分组成以质量%计进一步含有Sn:0.002%~0.10%、Mo:0.005%~0.10%、Sb:0.005%~0.30%、Cu:0.01%~0.50%、Cr:0.01%~0.50%、Ni:0.010%~1.0%中的1种以上。
(5)根据上述(1)~(4)中任一项所述的无方向性电磁钢板,其中,所述绝缘被膜在与所述基体铁的界面侧具有Fe的稠化层。
(6)根据上述(1)~(5)中任一项所述的无方向性电磁钢板,其中,所述钢板的厚度为0.20mm以下。
(7)根据上述(1)~(6)中任一项所述的无方向性电磁钢板,其中,所述钢板具有Si浓度从所述钢板的表面侧向所述钢板的中心部侧变低的浓度梯度,该浓度梯度中的钢板表层与钢板中心层的Si浓度差为1.0~5.0质量%。
(8)根据上述(1)~(7)中任一项所述的电磁钢板的制造方法,其中,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
所述冷轧通过使用含有1%以上的磷酸酯型的乳化剂的轧制油进行,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
(9)根据上述(1)~(7)中任一项所述的电磁钢板的制造方法,在对该电磁钢板用的板坯实施热轧、冷轧、接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
包括在所述冷轧后且所述最终退火前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥的工序,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
(10)根据上述(1)~(7)中任一项所述的电磁钢板的制造方法,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
所述冷轧通过使用含有1%以上的磷酸酯型的乳化剂的轧制油进行,
在所述冷轧后且所述最终退火前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥,所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
(11)根据上述(1)~(7)中任一项所述的电磁钢板的制造方法,其中,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
使所述板坯中含有0.005~0.20质量%的P,将所述最终退火的退火温度设为1100℃以上,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
(12)根据上述(11)所述的电磁钢板的制造方法,其中,所述冷轧通过使用含有1%以上的磷酸酯型的乳化剂的轧制油进行。
(13)根据上述(11)或(12)所述的电磁钢板的制造方法,其中,具有在所述冷轧后且所述最终退火前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥的工序。
(14)根据上述(8)~(13)中任一项所述的无方向性电磁钢板的制造方法,其中,在对所述电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
对所述最终退火后实施渗硅处理,或者将所述最终退火设为兼具渗硅处理的最终退火。
根据本发明,无方向性电磁钢板无论绝缘被膜的种类如何,由于具有即使薄也不损害被膜密合性的绝缘被膜,因此在板厚薄的电磁钢板中能够改善以往成为问题的占空系数低的情况。
附图说明
图1是表示发明例的GDS测定分布的图。
具体实施方式
本发明的特征在于在带绝缘被膜的无方向性电磁钢板中,绝缘被膜具有以下所示的构成,成为绝缘被膜母板的电磁钢板并不需要特别限定,可以根据电磁钢的一般规定进行。
[绝缘被膜在表面侧和与基体铁的界面侧这两方具有P浓度比基体铁的P浓度高的P稠化层]
通过在绝缘被膜的表面侧和与基体铁的界面侧这两方使P稠化,从而被膜变得稳固,并且在与基体铁的界面侧稠化的P作为基体铁与绝缘被膜之间的粘合剂发挥作用。根据该效果,可得到具有即使绝缘被膜自身薄,仍为稳固且密合性高的绝缘被膜的电磁钢板。
应予说明,绝缘被膜中的P的稠化可使用辉光放电发射分析仪(Glow DischargeSpectroscopy:GDS)进行评价。本实施方式的GDS评价使用堀场制作所制GDS-Profiler2,在Ar气压力600Pa、高频输出35W的条件下实施,但只要是可进行同等评价的装置,就可以是任何机种。这里,有无P稠化层可以如下进行判断。
图1中示出满足本发明的要件的带绝缘被膜的钢板中的P与Fe的GDS分布测定结果的一个例子。首先,绝缘被膜的与基体铁的界面侧是指Fe强度朝向绝缘被膜的表面侧(换言之图1的图表的分析深度的左方向)急剧减少的区域。这里,将基体铁区域的P的探针检测强度设为Ia,将绝缘被膜中的与基体铁的界面侧的P检测强度峰值设为Ib,将绝缘被膜的表面侧的P检测强度峰值设为Ic。绝缘被膜与基体铁的界面侧的P稠化层是指满足下述式(1)的层,绝缘被膜的表面侧的P稠化层是指满足下述式(2)的层。应予说明,上述的“基体铁的P浓度”为上述Ia。因此,P稠化是指满足下述式(1)和式(2)这两方。
Ib>Ia…(1)
Ic>Ia…(2)
[绝缘被膜厚和组成]
绝缘被膜厚优选为2.0μm以下。膜厚越薄,占空系数越提高,因此进一步优选为1.0μm以下。优选的膜厚没有下限,根据所形成的绝缘被膜的种类,控制在可确保层间的绝缘的薄度即可。作为上述绝缘被膜,可以使用仅有机成分、仅无机成分,由有机·无机复合物等构成。具体而言,作为有机成分,可举出丙烯酸系、丙烯酸硅系、聚酯系、环氧系、氟系的树脂等。作为无机成分,可举出铬酸盐系、重铬酸盐系、硼酸盐系、硅酸盐系等。另外,作为有机·无机复合物(半有机),可举出上述有机成分与无机成分的复合物等。
本发明的无方向性电磁钢板的成分组成根据电磁钢板的一般规则即可,但以下对优选的成分组成进行说明。
C:小于0.010质量%
C引起磁时效,使磁特性劣化,因此含量越少好。然而,过度的C量的减少导致制造成本的上升。因此,C量优选实用上磁时效不成问题的小于0.010质量%。C量更优选为小于0.0050质量%。
Si:1.5质量%~10.0质量%
Si是提高钢的电阻率,改善铁损特性的元素,本发明中为了得到铁损特性改善效果,优选为含有1.5质量%以上。然而,如果Si含有超过10.0质量%,则饱和磁通密度显著降低,在制造马达时反而会导致扭矩大幅降低。因此,本发明中,Si量优选为1.5质量%以上,更优选为2.0质量%以上,优选为10.0质量%以下,更优选为7.0质量%以下。另外,Si量更优选为1.5~10.0质量%的范围,进一步优选为2.0~7.0质量%。应予说明,这里的Si量是相对于板厚方向的Si含量的平均值。
Al:0.001质量%~2.0质量%
Al与Si同样地是因提高钢的电阻率而对铁损改善有效的元素。另一方面,如果过量地添加Al,则不仅降低饱和磁通密度,而且因与钢中N或由去应力退火时的钢板氮化带来的N结合而使AlN析出,因此优选为2.0质量%以下,更优选为0.50质量%以下。为了得到对铁损的改善有效的电阻率增加,优选将Al量设为0.001质量%以上,更优选为0.002质量%以上。进一步优选Al量为0.002~0.50质量%。
Mn:0.005质量%~1.0质量%
Mn为了改善热轧时的加工性优选含有0.005质量%以上,优选为含有1.0质量%以下,更优选为0.005~1.0质量%的范围。如果Mn量小于0.005质量%,则上述加工性改善效果小,另一方面,如果超过1.0质量%,则饱和磁通密度降低。更优选Mn量为0.01质量%以上,为0.30质量%以下,进一步优选为0.010~0.30质量%。
P:0.005质量%~0.20质量%
P是如后所述通过添加到板坯中进行热处理,在绝缘被膜中的与基体铁的界面侧形成P稠化层的手段之一。另外,不仅对被膜产生影响,而且对织构改善、由电阻率的增加带来的磁特性的改善也有效发挥作用,优选含有0.005质量%以上P,优选含有0.030质量%以上。另一方面,P量超过0.20质量%时,急剧脆化,损害制造性、加工性,因此优选为0.20质量%以下,优选为0.10质量%以下。P量更优选为0.030~0.10质量%。
另外,作为在绝缘被膜中的与基体铁的界面侧形成P稠化层的手段,也可举出含有磷酸酯型乳化剂的轧制油的使用、在钢板表面涂布干燥含有磷酸化合物的水溶液。在这种情况下,并不总是需要在板坯中含有P,在这种情况下,为了改善织构,优选添加0.001质量%以上的P,优选添加0.10质量%以下,更优选添加0.001~0.10质量%。
除了上述的优选基本成分,还可以根据需要,添加以下的成分。
Sn:0.002质量%~0.10质量%;Mo:0.005质量%以上,0.10质量%以下;Sb:0.005质量%以上,0.30质量%以下;Cu:0.01质量%以上,0.50质量%以下;Cr:0.01质量%以上,0.50质量%以下;Ni:0.010质量%以上,1.0质量%以下
上述成分均是为了实现磁特性的改善而添加的有效的元素,进一步优选以各元素的下限值以上添加上述成分中的1种以上。其中,过量添加会导致磁特性的劣化、制造性的恶化,优选在各自示出的上限值以下的范围内进行添加。
[在绝缘被膜的与基体铁的界面侧具有Fe的稠化层]
如图1示出的例子所示,在绝缘被膜的与基体铁的界面侧,由于P和Fe同时稠化,从而Fe与P的化合物作为基体铁与绝缘被膜的粘合剂发挥作用,成为在电磁钢板上更稳固地形成的绝缘被膜。这里,有无Fe稠化可以根据GDS进行评价,在得到Fe的峰强度的分析深度与得到P的峰强度Ib的分析深度之差为0.5μm以下的情况下,绝缘被膜的与基体铁的界面侧具有Fe的稠化层。
[电磁钢板的厚度]
板厚越薄,占空系数的降低越成问题,因此在板厚比0.25mm以下更薄的情况下容易得到本发明的效果。并且,本发明在板厚为0.20mm以下时发挥更高的效果。从该效果的观点考虑,不需要设定板厚的下限,但板厚为0.05mm以下时,核心的制造中的冲压等的成本大幅增大,因此优选超过0.05mm。
这里,“电磁钢板的厚度”或者简称“板厚”也包含在绝缘被膜的厚度中。
[Si浓度具有从钢板的表面侧向钢板的中心部侧变低的浓度梯度,该浓度梯度中的钢板表层与钢板中心层的Si浓度差为1.0~5.0质量%]
通过在钢板的板厚方向具有Si浓度梯度,从而可改善高频的铁损。作为用于实现该浓度梯度的方法,例如可以在含SiCl4的气氛中进行渗硅处理,也可以是基于层叠Si浓度不同的材料而使用的包层的制造方法。这里,Si的浓度差足以获得涡流损耗的改善效果,因此下限值优选为1.0质量%,更优选为1.5质量%。另外,Si的浓度差抑制磁滞损耗的劣化,因此,上限值优选为5.0质量%,更优选为3.5质量%。更优选为Si的浓度差为1.5~3.5%。
应予说明,具体而言“钢板表层”和“钢板中心层”被定义为从钢板的两表面(不包括绝缘被膜)起分别到板厚1/3的区域设为“钢板表层”,将剩余的板厚1/3的区域定义为“钢板中心层”。另外,将钢板中心层的Si浓度设为相应的区域的平均浓度,钢板表层的Si浓度是将在两表面分别相应的区域的平均浓度进一步平均而得的值(换言之,两表层的平均浓度)。而且,上述平均浓度可以使用EPMA测定板厚方向的Si浓度,根据其浓度曲线进行评价。
[制造方法]
本发明的电磁钢板可以根据常规方法,通过对电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火而制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序来制造。
[在绝缘被膜中的与基体铁的界面侧形成P稠化层的方法]
为了在绝缘被膜中的与基体铁的界面侧形成P的稠化层,在上述的制造工序中需要进行下述中的任一处理。
·冷轧时使用含有1%以上的磷酸酯型的乳化剂的轧制油
·在上述冷轧后且上述最终退火(或渗硅处理)前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥
·使板坯含有0.005质量%~0.20质量%的P,将最终退火中的退火温度设为1100℃以上
[在绝缘被膜的表面侧形成P的稠化层的方法]
另外,为了在绝缘被膜的表面侧形成P的稠化层,需要进行下述的处理。
·在绝缘被膜形成工序中,涂布含有1质量份以上的磷酸化合物的液体
[渗硅处理]
为了设置所述Si浓度差,从进一步在最终退火后进行渗硅处理,或者降低成本的理由考虑,可以将所述最终退火设为兼具渗硅处理的最终退火。这里,作为进行渗硅处理时的气氛气体,可使用四氯化硅与氮气的混合气体。进行渗硅处理时的热处理温度优选为1100~1300℃,退火时间根据所需的渗硅量优选为30~120秒。
[形成Fe稠化层的方法]
为了在绝缘被膜中形成Fe稠化层,优选将渗硅处理温度或最终退火温度设为1000℃以上。出于减少高频下的涡流损耗的理由,需要避免使粒径粗大,因此优选为1300℃以下。
通过将表1所示的成分的板坯加热到1200℃,通过热轧得到1.8mm的热轧板。接着,实施1050℃的热轧板退火后,通过冷轧分别进行轧制至表1所示的板厚(制品板厚)。这里,在一部分的条件中,冷轧时,使用含有1%的ADEKA COLPS807的轧制油(为轧制油A)作为磷酸酯型的乳化剂,其它的条件中,使用不含磷酸酯型的乳化剂的一般的铁用冷轧油(为轧制油B)。一部分的条件中,进一步在冷轧后最终退火前,进行涂布作为含有5质量份以上的磷酸化合物的水溶液的磷酸Al并使其干燥的前处理,将其有无在表1的“退火前处理”的栏中表示为“有”、“无”。
接着,在20%H2-80%N2干燥气氛下在1000℃×10s的条件下实施最终退火。应予说明,表1的No.21、23和24是在1100℃×10s的条件下实施最终退火,No.25是在950℃×10s的条件下实施最终退火。
另外,为了形成绝缘被膜,涂布在含有铬酸和丙烯酸树脂的有机·无机复合涂液中添加了1质量份磷酸Mg的液体后,在300℃下烧结制成电磁钢板制品。应予说明,仅表1的No.22因用于比较而未在涂体中添加磷酸Mg。对以上得到的电磁钢板制品,评价占空系数、绝缘被膜的密合性(被膜剥离)和铁损W10/1000。占空系数通过基于JIS C 2550-5的方法进行评价,磁特性通过基于JIS C 2550-1的方法进行评价。绝缘被膜的密合性的评价基于JIS K5600-5-6(划格法),利用刀具在钢板表面以1mm间隔切入6条切痕,张贴玻璃粘性胶带后,对其进行剥离,由此评价被膜剥离的状态。如果剥离面积相对于划格部分的面积的比例小于10%,则为良好,为10%以上则不良。另外,用GDS评价钢板表面的被膜结构,进行是否满足上述的式1和式2这两方的判定,将满足两方的情况表示为○,任一方不满足的情况表示为×。另外,在具有Fe的峰强度、且Fe的峰强度与P的峰强度Ib的深度之差为0.5μm以下的情况下,作为具有Fe的稠化层的情况(Fe峰:有)。
[表1]
表1示出结果。涂布在有机·无机复合涂液中添加了1质量份磷酸Mg而成的液体,除此之外,使用作为磷酸酯型的乳化剂的含有1%的ADEKACOL PS807的轧制油,进行在冷轧后最终退火前涂布作为含有5质量份以上的磷酸化合物的水溶液的磷酸Al并使其干燥的前处理、或者使用含有0.005质量%~0.20质量%的P的板坯且在进行1100℃以上的最终退火中的任一者的情况下,得到满足式1和式2这两者的被膜结构,得到结果良好的被膜剥离试验结果。
通过将表2所示的成分的板坯加热到1200℃,利用热轧,得到1.7mm的热轧板。接着,在实施1050℃的热轧板退火后,利用冷轧,分别进行轧制至表2所示的板厚(制品板厚)。在冷轧时,使用作为磷酸酯型的乳化剂的含有1%的ADEKACOL PS807的轧制油(轧制油A)。接着,对冷轧板,在四氯化硅+N2气体中,实施1200℃×60s的热处理,从而进行兼具渗硅处理的最终退火。在该渗硅处理中,通过控制炉内的四氯化硅气体流量,从而控制钢板表层的Si浓度(表层Si浓度)。板厚方向的Si浓度梯度通过EPMA进行确认。在作为钢板的中心部侧的钢板中心层为母材成分本身的Si浓度,可得到在板厚方向具有Si浓度从钢板的表面侧向钢板的中心部侧变低的Si浓度梯度的钢板。
并且,涂布了在以磷酸Al为主的无机复合涂液中添加了1质量份的磷酸Mg而成的液体后,在320℃下进行烧结,得到电磁钢板制品。对以上得到的电磁钢板制品进行与实施例1相同的评价,并将其结果汇总示于表2。
[表2]
表2中示出了结果。在与实施例1同样地具有满足式1和式2这两者的被膜结构的无方向性电磁钢板中,得到良好的被膜剥离试验结果。并且,通过渗硅处理,使Si浓度差设为1.0~5.0质量%,从而改善铁损。
Claims (14)
1.一种无方向性电磁钢板,在钢板的至少单面具有绝缘被膜的电磁钢板中,所述绝缘被膜在表面侧和与基体铁的界面侧这两方具有P浓度比所述基体铁的P浓度高的P稠化层。
2.根据权利要求1所述的无方向性电磁钢板,其中,所述钢板以质量%计具有如下成分组成:含有C:小于0.010%、Si:1.5%~10.0%、Al:0.001%~2.0%和Mn:0.005%~1.0%,且剩余部分为Fe和不可避免的杂质。
3.根据权利要求2所述的无方向性电磁钢板,其中,所述钢板以质量%计进一步含有P:0.005%~0.20%。
4.根据权利要求2或3所述的无方向性电磁钢板,其中,所述成分组成以质量%计进一步含有Sn:0.002%~0.10%、Mo:0.005%~0.10%、Sb:0.005%~0.30%、Cu:0.01%~0.50%、Cr:0.01%~0.50%、Ni:0.010%~1.0%中的1种以上。
5.根据权利要求1~4中任一项所述的无方向性电磁钢板,其中,所述绝缘被膜在所述与基体铁的界面侧具有Fe的稠化层。
6.根据权利要求1~5中任一项所述的无方向性电磁钢板,其中,所述钢板的厚度为0.20mm以下。
7.根据权利要求1~6中任一项所述的无方向性电磁钢板,其中,所述钢板具有Si浓度从所述钢板的表面侧向所述钢板的中心部侧变低的浓度梯度,该浓度梯度中的钢板表层与钢板中心层的Si浓度差为1.0~5.0质量%。
8.根据权利要求1~7中任一项所述的电磁钢板的制造方法,其中,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
所述冷轧使用含有1%以上的磷酸酯型的乳化剂的轧制油进行,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
9.根据权利要求1~7中任一项所述的电磁钢板的制造方法,其中,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
具有在所述冷轧后且所述最终退火前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥的工序,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
10.根据权利要求1~7中任一项所述的电磁钢板的制造方法,其中,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
所述冷轧通过使用含有1%以上的磷酸酯型的乳化剂的轧制油进行,
具有在所述冷轧后且所述最终退火前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥的工序,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
11.根据权利要求1~7中任一项所述的电磁钢板的制造方法,其中,在对该电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
使所述板坯中含有0.005~0.20质量%的P,将所述最终退火的退火温度设为1100℃以上,
所述绝缘被膜的形成通过涂布含有1质量份以上的磷酸化合物的液体进行。
12.根据权利要求11所述的电磁钢板的制造方法,其中,所述冷轧通过使用含有1%以上的磷酸酯型的乳化剂的轧制油进行。
13.根据权利要求11或12所述的电磁钢板的制造方法,其中,具有在所述冷轧后且所述最终退火前,在经过所述冷轧的钢板的表面涂布含有5质量份以上的磷酸化合物的水溶液并使其干燥的工序。
14.根据权利要求8~13中任一项所述的无方向性电磁钢板的制造方法,其中,在对所述电磁钢板用的板坯实施热轧、冷轧,接着实施最终退火,制成最终退火板,在该最终退火板的表面形成绝缘被膜的工序中,
对所述最终退火后实施渗硅处理,或者将所述最终退火实施为兼具渗硅处理的最终退火。
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- 2020-04-28 MX MX2022001312A patent/MX2022001312A/es unknown
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EP4006184A1 (en) | 2022-06-01 |
EP4006184A4 (en) | 2022-08-31 |
WO2021019859A1 (ja) | 2021-02-04 |
MX2022001312A (es) | 2022-03-02 |
TWI736255B (zh) | 2021-08-11 |
TW202106897A (zh) | 2021-02-16 |
US20220243298A1 (en) | 2022-08-04 |
JP7044165B2 (ja) | 2022-03-30 |
JPWO2021019859A1 (ja) | 2021-09-13 |
KR20220028054A (ko) | 2022-03-08 |
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