CN104900362A - 铁氧体烧结磁铁以及具备其的电动机 - Google Patents
铁氧体烧结磁铁以及具备其的电动机 Download PDFInfo
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- CN104900362A CN104900362A CN201510100724.8A CN201510100724A CN104900362A CN 104900362 A CN104900362 A CN 104900362A CN 201510100724 A CN201510100724 A CN 201510100724A CN 104900362 A CN104900362 A CN 104900362A
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- sintered magnet
- ferrite sintered
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Classifications
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Abstract
本发明目的在于提供一种剩余磁通密度(Br)以及矩形比(Hk/HcJ)优异的铁氧体烧结磁铁以及使用其的电动机。本发明的铁氧体烧结磁铁是一种将具有六方晶结构的M型Sr铁氧体作为主相的铁氧体烧结磁铁,Zn的含量换算成ZnO为0.05~1.35质量%,在将稀土元素(R)的含量以摩尔换算记为M1,将上述Zn的含量以摩尔换算记为M2的情况下,M1/M2为0.43以下。
Description
技术领域
本发明涉及一种铁氧体烧结磁铁以及具备其的电动机。
背景技术
作为被用于铁氧体烧结磁铁的磁性材料,已知有具有六方晶系的结晶结构的Ba铁氧体、Sr铁氧体以及Ca铁氧体。近年来,在这些之中,作为电动机等的磁铁材料,主要采用磁铅石型(magnetoplumbite-type)(M型)的Sr铁氧体。M型铁氧体例如由AFe12O19的通式表示。Sr铁氧体在结晶结构的A位具有Sr。
另外,作为这样的M型Sr铁氧体,广泛利用含有Ca和Si作为成分的物质。对于这样的Sr铁氧体,如果增加Ca则剩余磁通密度(Br)提高但是矩形比(squareness ratio)(Hk/HcJ)会有降低的倾向,如果增加Si则矩形比(Hk/HcJ)改善但是剩余磁通密度(Br)会有降低的倾向,所获得的磁特性自然有极限。
因此,一直以来尝试着去改善磁特性。例如,在专利文献1中公开了通过用特定量的稀土元素以及Co置换A位以及B位的一部分从而提高磁特性的技术。
另外,作为提高磁特性的技术,提案有在上述Sr铁氧体中使Zn以及Ti存在的技术(专利文献2)和使Zn以及Mn存在的技术(专利文献3以及4)等。
但是,如上所述的技术需要使用比以Fe或Sr等为主的原材料更昂贵的成分,如果与现有的Sr铁氧体相比则存在原材料的成本增加的问题。例如,La(稀土元素)或Co等成分,特别是近年来还在涨价,与以Fe或Sr等为主的原材料相比明显昂贵。另外,对于Ti也比以Fe或Sr等为主的原材料昂贵,并不能充分降低原材料的成本。因此,寻求生产成本(特别是原材料的成本)的降低。
另外,作为铁氧体烧结磁铁的代表性的用途,可以列举电动机。虽然要求用于电动机的铁氧体烧结磁铁在剩余磁通密度(Br)和矩形比(Hk/HcJ)两个特性方面都优异,但是已知通常剩余磁通密度(Br)和矩形比(Hk/HcJ)处于一种权衡(trade-off)的关系。因此,要求确立能够进一步提高剩余磁通密度(Br)以及矩形比(Hk/HcJ)两个特性的技术。
现有技术文献
专利文献
专利文献1:日本特开平11-154604号公报
专利文献2:日本特开2001-052912号公报
专利文献3:日本特开平11-251126号公报
专利文献4:日本特开2001-284113号公报
发明内容
发明想要解决的技术问题
本发明是鉴于上述情况而完成的发明,目的在于提供一种剩余磁通密度(Br)以及矩形比(Hk/HcJ)优异的铁氧体烧结磁铁以及使用该铁氧体烧结磁铁的电动机。
解决技术问题的手段
以解决这样的技术问题为目的的本发明的要点如下。
[1]一种铁氧体烧结磁铁,是以具有六方晶结构的M型Sr铁氧体作为主相的铁氧体烧结磁铁,换算成ZnO的Zn的含量为0.05~1.35质量%,在将稀土元素(R)的含量按摩尔换算记为M1,并将上述Zn的含量按摩尔换算记为M2的情况下,M1/M2为0.43以下。
[2]如上述[1]所述的铁氧体烧结磁铁,其中,换算成MnO的Mn的含量小于0.5质量%。
[3]如上述[1]或[2]所述的铁氧体烧结磁铁,其中,在将Sr、R(稀土元素)、Ba以及Ca的合计含量按摩尔换算记为M3,将Fe、Co、Mn、Zn、Cr以及Al的合计含量按摩尔换算记为M4,进一步将Si的含量按摩尔换算记为M5的情况下,
0.5≤[M3-(M4/12)]/M5≤1.2。
[4]如上述[1]~[3]中任一项所述的铁氧体烧结磁铁,其特征为,换算成Na2O的Na的含量为0.01~0.09质量%。
[5]如上述[1]~[4]中任一项所述的铁氧体烧结磁铁,其特征为,上述Sr铁氧体的晶粒的平均粒径为1.0μm以下,粒径为2.0μm以上的上述晶粒的个数基准的比例为2%以下。
[6]如上述[1]~[5]中任一项所述的铁氧体烧结磁铁,其特征为,剩余磁通密度(Br)为440mT以上,矩形比(Hk/HcJ)为85%以上。
[7]一种电动机,具备上述[1]~[6]中任一项所述的铁氧体烧结磁铁。
发明效果
根据本发明,能够得到剩余磁通密度(Br)以及矩形比(Hk/HcJ)高的铁氧体烧结磁铁。
附图说明
图1是示意性地表示本发明的铁氧体烧结磁铁的优选的实施方式的立体图。
图2是示意性地表示本发明的实施例以及比较例所涉及的铁氧体烧结磁铁(样品A)的立体图。
图3是示意性地表示在测定本发明的实施例以及比较例所涉及的铁氧体烧结磁铁(样品A)的抗弯强度时的截面情况的图。
符号说明
10.铁氧体烧结磁铁
具体实施方式
以下根据需要参照附图并针对本发明的优选实施方式进行详细说明。
图1是示意性地表示本实施方式的铁氧体烧结磁铁的立体图。铁氧体烧结磁铁10具有以端面成为圆弧状的形式进行弯曲的形状,一般具有被称为圆弧段形状、C形形状、瓦形形状或者弓形形状的形状。铁氧体烧结磁铁10例如优选作为电动机用的磁铁使用。
铁氧体烧结磁铁10中,作为主成分(主相),含有具有六方晶结构的M型Sr铁氧体的晶粒。
作为这样的M型的Sr铁氧体,例如可以用以下的式(1)来表示。
SrFe12O19 (1)
上述式(1)的M型的Sr铁氧体中的A位的Sr以及B位的Fe可以用杂质或者有意添加的元素来置换其一部分。
这样的M型Sr铁氧体例如可以用以下的通式(2)来表示。
RxSr1-x(Fe12-yMy)zO19 (2)
在上式(2)中,x以及y例如为0.01~0.5,z例如为0.7~1.2。另外,上述式(2)中的M例如可以列举选自Zn(锌)、Co(钴)、Ni(镍)、Mn(锰)、Al(铝)以及Cr(铬)中的1种以上的元素。另外,上述式(2)中的R是稀土元素,例如可以列举选自La(镧)、Ce(铈)、Pr(镨)、Nd(钕)以及Sm(钐)中的1种以上的元素。
另外,上述式(1)和(2)中的A位以及B位的比率或氧(O)的比率实际上显示稍微偏离上述范围的值,因此即使稍微偏离于上述数值也可以。
优选铁氧体烧结磁铁10中的M型Sr铁氧体由上述式(2)表示,并且M至少含有Zn(锌)。进一步,更加优选R为La。
铁氧体烧结磁铁10中的M型Sr铁氧体相的比率优选为90%以上,进一步优选为95%以上,更加优选为97%以上。这样通过降低不同于M型Sr铁氧体相的结晶相的比率,可以进一步提高磁特性。铁氧体烧结磁铁10中的M型Sr铁氧体相的比率(%)可以通过由X射线衍射求得M相的含量比率(摩尔%)来进行确认。M相的含量比率可通过以规定比率混合M型铁氧体、正铁氧体(orthoferrite)、赤铁矿(hematite)、尖晶石、W型铁氧体的各粉末样品,并由它们的X射线衍射强度进行比较计算,从而被计算出。
另外,铁氧体烧结磁铁10中,作为副成分含有不同于M型Sr铁氧体的成分。作为副成分,可以列举作为晶界成分或异相存在的成分。作为这样的成分,例如可以列举氧化物,具体而言,作为构成元素可以列举具有选自R(稀土元素)、Na(钠)、Si(硅)、Ca(钙)、Sr(锶)、Ba(钡)、Fe(铁)、Co(钴)、Mn(锰)、Zn(锌)、Cr(铬)以及Al(铝)中的至少一种的氧化物以及复合氧化物。作为这样的氧化物例如可以列举SiO2、Na2O、CaO、La2O3、ZnO、Fe2O3、MnO等。另外,也可以含有硅酸玻璃。
这样的铁氧体烧结磁铁10中的Fe的含量换算成Fe2O3优选为80~95质量%,更加优选为87~90质量%。通过在上述范围内能够获得良好的磁特性。
另外,铁氧体烧结磁铁10中的Sr的含量换算为SrO优选为9~11质量%,进一步优选为9~10质量%。通过在上述范围内能够获得良好的磁特性。
另外,铁氧体烧结磁铁10中的Zn含量换算成ZnO为0.05~1.35质量%。通过满足上述范围,从而可以少产生外观不良,并具有充分的机械强度(特别是抗弯强度(σ)),而且能够良好地保持磁特性(剩余磁通密度(Br)和矩形比(Hk/HcJ)的平衡)。
此外,从进一步提高铁氧体烧结磁铁10的剩余磁通密度(Br)的观点出发,Zn的含量换算成ZnO优选为0.10质量%以上,更加优选为0.14质量%以上。另外,从进一步提高铁氧体烧结磁铁10的矩形比(Hk/HcJ)的观点出发,Zn的含量换算成ZnO优选为0.76质量%以下,更加优选为0.37质量%以下。
另外,从进一步提高铁氧体烧结磁铁10的机械强度的观点出发,Zn的含量换算成ZnO优选为0.10质量%以上,更加优选为0.20质量%以上。认为通过增加Zn的含量从而烧结密度会提高,伴随于此铁氧体烧结磁铁10的机械强度也会提高。另外,烧结密度伴随于Zn的含量的增加而提高的原理尚不一定明确,但是可以推测如下,除了在烧结时固溶于晶格内的Zn之外,Zn的一部分在晶界与其它成分(例如Si或Ca等)一起形成液相,从而进行理想的致密化。
另外,铁氧体烧结磁铁10优选含有稀土元素(R)。铁氧体烧结磁铁10中的稀土元素(R)的含量与Zn的含量之间满足以下关系。即,在将铁氧体烧结磁铁10中的稀土元素(R)的含量按摩尔换算记为M1,并将Zn的含量按摩尔换算记为M2的情况下,M1/M2为0.43以下,优选M1/M2为0.32以下,进一步优选为0.20以下,更加优选为0.14以下,特别优选满足M1/M2为0.08以下的关系。另外,M1/M2优选大于0,进一步优选为0.001以上,更加优选为0.01以上。特别是通过M1/M2为0.43以下,从而很少产生外观不良并且既能够维持充分的机械强度又能够良好地保持磁特性。
一直以来,在R-Zn系Sr铁氧体中,从电荷补偿的观点出发通常添加与Zn相等摩尔(M1/M2≈1)的R(例如La)。
但是,本发明人等发现在M1/M2为0.43以下的条件下能够获得最优异的磁特性。原理并不一定明确,但是认为可能存在于Sr铁氧体颗粒的晶粒内的微量的氧缺陷等有助于少量的Zn固溶于Fe位时的电荷补偿。
即,认为铁氧体磁铁10中的R的含量可以少于Zn的含量,通过M1/M2成为0.43以下能够做到实质的电荷补偿,组成最优化并且能够获得最优异的磁特性。
另外,从良好地保持磁特性的观点出发,铁氧体烧结磁铁10中的稀土元素(R)的含量换算成氧化物优选大于0质量%,进一步优选为0.001质量%以上,更加优选为0.01质量%以上。另外,从防止原料成本增加的观点出发,铁氧体烧结磁铁10中的R的含量换算成氧化物优选为0.58质量%以下,进一步优选为0.33质量%以下,更加优选为0.16质量%以下。此外,作为R优选为La。
另外,铁氧体烧结磁铁10优选含有选自Mn(锰)、Na(钠)、Si(硅)以及Ca(钙)中的一种以上。
铁氧体烧结磁铁10中的Mn的含量换算成MnO优选为小于0.5质量%,更加优选为0.3质量%以下。通过满足上述范围能够良好地保持磁特性[特别是剩余磁通密度(Br)]。还有,Mn的含量换算成MnO可以是0质量%。
铁氧体烧结磁铁10中的Na含量换算成Na2O优选为0.01~0.09质量%。如果Na的含量变得过少则不能降低烧结温度,并且会存在晶粒生长而难以获得充分高的磁特性的倾向。因此,Na的含量换算成Na2O优选为0.01质量%以上,进一步优选为0.02质量%以上,更加优选为0.04质量%以上。然而,如果Na的含量变得过多则会有容易在铁氧体烧结磁铁10的表面产生白色粉体的倾向。如果在铁氧体烧结磁铁10的表面产生粉体则例如电动机部件与铁氧体烧结磁铁10的粘结力降低,并且铁氧体烧结磁铁10可能从电动机部件剥离。即,铁氧体烧结磁铁10的可靠性被损坏。因此,Na的含量换算成Na2O优选为0.09质量%以下,进一步优选为0.08质量%以下,更加优选为0.07质量%以下。
另外,铁氧体烧结磁铁10中的Si的含量换算成SiO2优选为0.05~2质量%,更加优选为0.2~1质量%。通过满足上述范围可以抑制过度的晶粒生长从而实现优异的磁特性。
铁氧体烧结磁铁10中的Ca含量换算成CaO优选为0.05~2质量%,更加优选为0.1~0.8质量%。通过满足上述范围能够均匀地致密化并实现优异的磁特性。
另外,铁氧体烧结磁铁10可以含有Ba。铁氧体烧结磁铁10中的Ba的含量优选成为例如换算成BaO为0.01~2质量%。
另外,铁氧体烧结磁铁10可以含有Al和/或Cr。Al和/或Cr具有提高矫顽力(HcJ)的效果。但是,Al和/或Cr有降低剩余磁通密度(Br)的倾向。因此,Al以及Cr的合计含量换算成Al2O3以及Cr2O3优选为3.0质量%以下。另外,从充分发挥Al以及Cr的添加效果的观点出发,Al以及Cr的合计含量换算成Al2O3以及Cr2O3优选为0.01质量%以上。
在铁氧体烧结磁铁10中,除了这些成分之外,还可以含有包含于原料中的杂质或来自制造设备的不可避免的成分。作为这样的成分例如可以列举Mg(镁)、Ti(钛)、Mn(锰)、Mo(钼)以及V(钒)等的各种氧化物。
然而,副成分主要包含于铁氧体烧结磁铁10中的Sr铁氧体的晶粒的晶界中。如果包含于副成分的各元素的比率发生变化,则晶界的组成会变化,其结果可能影响到铁氧体烧结磁铁10的磁特性或可靠性。
因此,从进一步提高磁特性以及可靠性的观点出发,铁氧体烧结磁铁10中,以摩尔比α=[M3-(M4/12)]/M5表示的晶界成分比优选满足下述式(3)。
0.5≤[M3-(M4/12)]/M5≤1.2 (3)
上述式(3)中,M3是Sr、R(稀土元素)、Ba及Ca的合计含量(摩尔%),M4是Fe、Co、Mn、Zn、Cr以及Al的合计含量(摩尔%),M5是Si的含量(摩尔%)。
不过,对于M3的Sr、R(稀土元素)、Ba以及Ca的合计含量(摩尔%),在Sr、R(稀土元素)、Ba以及Ca中,在测定时不能检测的元素的含量(摩尔%)可以不包含于合计中。另外,对于M4的Fe、Co、Mn、Zn、Cr和Al的合计含量(mol%),在Fe、Co、Mn、Zn、Cr和Al中,在测定时不能检测的元素的含量(mol%)可以不包含于合计中。
上述式(3)是在认为包含杂质的副成分中,R、Ba、Ca主要固溶于Sr位且Co、Mn、Zn、Cr、Al主要固溶于Fe位的情况下成立的式子。在摩尔比α为规定的范围内的情况下,特别是Si成为中心并且形成各个副成分的液相,能够充分致密化、抑制晶粒生长并且各个副成分均匀固溶。其结果认为铁氧体烧结磁铁10发挥优异的磁特性和高机械强度。
然而,在摩尔比α过小的情况下,会有致密化变得不充分并且剩余磁通密度(Br)或机械强度[特别是抗弯强度(σ)]降低的倾向。因此,铁氧体烧结磁铁10中的摩尔比α优选为0.5以上,进一步优选为0.6以上,更加优选为0.7以上。另外,在摩尔比α过大的情况下会有不能获得充分的晶粒生长抑制效果并且粒径变得不均匀而且矩形比(Hk/HcJ)降低的倾向。因此,铁氧体烧结磁铁10中的摩尔比α优选为1.2以下,进一步优选为1.1以下,更加优选为1.0以下。
另外,铁氧体烧结磁铁10的各个成分的含量可以由X射线荧光分析以及电感耦合等离子体发射光谱分析(ICP分析)来测定。
铁氧体烧结磁铁10中的Sr铁氧体的晶粒的平均粒径优选为2.0μm以下,进一步优选为1.0μm以下,更加优选为0.3~1.0μm。如果Sr铁氧体的晶粒的平均粒径大于2.0μm,则会有变得难以获得充分优异的磁特性的倾向。另一方面,Sr铁氧体的晶粒平均粒径小于0.3μm的铁氧体烧结磁铁有变得难以进行制造(量产)的倾向。
另外,优选包含于铁氧体烧结磁铁10中的Sr铁氧体的晶粒偏差小。具体而言,相对于Sr铁氧体晶粒整体的该晶粒的粒径为2.0μm以上的Sr铁氧体晶粒的个数基准的比例优选为2%以下,进一步优选为1%以下。通过提高Sr铁氧体晶粒的均匀性能够既进一步提高高的磁特性又提高可靠性。
另外,包含于铁氧体烧结磁铁10中的Sr铁氧体晶粒的纵横比的个数平均值(平均纵横比)优选为大约1.0。由此,就能够制得具有充分高的磁特性的铁氧体烧结磁铁10。
铁氧体烧结磁铁10的Sr铁氧体晶粒的粒径可以按以下所述顺序测定。使从铁氧体烧结磁铁切下来的样品薄片化并用TEM来观察。或者,对该样品的截面进行镜面研磨用氢氟酸等酸来进行蚀刻处理,从而用SEM等进行观察。在包含数百个晶粒的SEM或者TEM的观察图像中将晶粒的轮廓清晰化之后,进行图像处理等,并测定a面的粒径分布。本说明书中的“粒径”是指在a面上的长径(a轴方向的直径)。进一步,在将通过重心的最大直径作为长径并且将通过重心的最小直径作为短径时,长径相对于短径之比为“纵横比”。另外,也可以替代由酸进行的蚀刻,而通过加热样品来进行蚀刻,即,所谓的热蚀刻(thermal etching)。
从所测定的个数基准的粒径分布计算出晶粒的粒径的个数基准的平均值。另外,从所测定的粒径分布和平均值算出标准偏差。在本说明书中,将这些作为Sr铁氧体的晶粒的平均粒径以及标准偏差。
另外,铁氧体烧结磁铁10的剩余磁通密度(Br)优选为440mT以上,进一步优选为445mT以上,更加优选为450mT以上。另外,铁氧体烧结磁铁10的矩形比(Hk/HcJ)优选为85%以上,进一步优选为87%以上,更加优选为90%以上。特别是铁氧体烧结磁铁10优选剩余磁通密度(Br)为440mT以上并且矩形比(Hk/HcJ)为85%以上。通过具有这样优异的磁特性能够进一步适宜用于电动机或发电机。
另外,铁氧体烧结磁铁10具有充分的机械强度,由3点弯曲试验测定的抗弯强度(σ)优选为150N/mm2以上,进一步优选为155N/mm2以上,更加优选为160N/mm2以上。机械强度高的铁氧体烧结磁铁10容易处理,能够有效地防止运送中的破碎或缺损所以提高了成品率,并且有助于成本降低。进一步,机械强度高的铁氧体烧结磁铁10组装到电动机等产品中之后也不容易被破坏所以能够提高产品的可靠性。
另外,为了既维持铁氧体烧结磁铁10的剩余磁通密度(Br)以及抗弯强度(σ)良好(Br≥440mT,σ≥150N/mm2)又能够将矩形比(Hk/HcJ)提高到87%以上,而优选将Zn的含量设为换算成ZnO为0.05~0.76质量%且M1/M2设为0.43以下,进一步将Na的含量设为换算成Na2O为0.08质量%以下。
进一步,为了将铁氧体烧结磁铁10的矩形比(Hk/HcJ)提高到90%以上,优选将Zn的含量设为换算成ZnO为0.05~0.37质量%且M1/M2设为0.03~0.32,将Na的含量设为换算成Na2O为0.08质量%以下。
另外,为了既维持铁氧体烧结磁铁10的剩余磁通密度(Br)以及矩形比(Hk/HcJ)良好(Br≥440mT,Hk/HcJ≥85%)又能够将抗弯强度(σ)提高到155N/mm2以上,优选将Zn的含量设为换算成ZnO为0.10~1.35质量%,且M1/M2设为0.32以下。
进一步,为了将铁氧体烧结磁铁10的抗弯强度(σ)提高到160N/mm2以上,优选将Zn的含量设为换算成ZnO为0.20~1.35质量%;且M1/M2设为0.14以下,将Mn的含量设为换算成MnO为0.30质量%以下。
另外,从其它观点出发,为了既维持铁氧体烧结磁铁10的剩余磁通密度(Br)以及矩形比(Hk/HcJ)良好(Br≥440mT,Hk/HcJ≥85%)又能够将抗弯强度(σ)提高到155N/mm2以上,优选将Zn的含量设为换算成ZnO为0.10~1.35质量%,将La的含量设为换算成La2O3为0.19质量%以下。
进一步,为了将铁氧体烧结磁铁10的抗弯强度(σ)提高到160N/mm2以上,优选将Zn的含量设为换算成ZnO为0.20~1.35质量%,将La的含量设为换算成La2O3为0.10质量%以下,并将Mn的含量设为换算成MnO为0.30质量%以下。
铁氧体烧结磁铁10例如能够作为燃油泵用、电动车窗用、ABS(防抱死制动系统)用、风扇用、刮水器用、动力转向装置用、主动(制导)悬挂系统用、起动器用、门锁用、电动反光镜用等汽车用电动机的磁铁来使用。另外,能够作为FDD主轴用、VTR主导轴用、VTR旋转头用、VTR卷盘用、VTR加载(loading)用、VTR摄像机主导轴用、VTR摄像机旋转头用、VTR摄像机变焦距用、VTR摄像机对焦用、收录机等主导轴用、CD/DVD/MD主轴用、CD/DVD/MD加载用、CD/DVD光拾波器用等OA/AV设备用电动机的磁铁使用。进一步,还能作为空调压缩机用、冷冻库压缩机用、电动工具驱动用、电吹风风扇用、电动剃须刀驱动用、电动牙刷用等家电机器用电动机的磁铁使用。再有,还能够作为机器人轴、关节驱动用、机器人主驱动用、机器工作台驱动用、机器工作皮带驱动用等FA机器用电动机的磁铁来使用。
铁氧体烧结磁铁10粘结于上述电动机部件而被设置于电动机内。具有优异磁特性的铁氧体烧结磁铁10能够充分抑制裂纹的产生以及表面上的异物(白粉)的产生,因此能够充分牢固地被粘结于电动机部件。这样能够充分抑制铁氧体烧结磁铁10从电动机部件剥离。因此,具备铁氧体烧结磁铁10的各种电动机兼备高效率以及高可靠性。
铁氧体烧结磁铁10的用途不限定于电动机,例如还能够作为发电机、扬声器·耳机用磁铁、磁控管、MRI用磁场发生装置、CD-ROM用夹持器、配电盘用传感器、ABS用传感器、燃料·燃油液位传感器、磁锁、或隔离器等的部件使用。另外,还能够作为在用蒸镀法或者溅射法等来形成磁记录介质的磁性层的时候的靶材(小球pellet)来使用。
接下来,说明铁氧体烧结磁铁10的制造方法。铁氧体烧结磁铁10的制造方法具有调配工序、预烧工序、粉碎工序、磁场中成型工序以及烧成工序。以下详细说明各个工序。
调配工序是调制预烧用混合粉末的工序。在调配工序中首先秤量初始原料并以规定比例进行调配,用湿式磨碎机或者球磨机等进行1~20小时左右的混合并且进行粉碎处理。作为初始原料准备具有作为主成分的Sr铁氧体的构成元素的化合物。
在调配工序中,也可以添加SiO2、CaCO3、Na2CO3、将稀土元素作为构成元素的氧化物(例如La2O3)以及ZnO等粉末。作为具有Na作为构成元素的化合物除了碳酸盐之外可以使用硅酸盐或含Na的有机化合物(分散剂等)。作为具有Zn作为构成元素的化合物不限定于氧化物,可以从无机锌、有机锌化合物中适当选择。
另外,对于稀土元素(R),如上所述可以使用稀土元素的氧化物等,但是从降低原料成本并且廉价地获得铁氧体烧结磁铁10的观点出发,可以通过使用作为杂质少量含有稀土元素(R)的原材料(例如LaCo系铁氧体磁铁的回收材料等)从而实质性地包含于铁氧体烧结磁铁10中。
作为具有Sr铁氧体的构成元素的化合物能够使用氧化物或者通过烧成会变成氧化物的碳酸盐、氢氧化物或者硝酸盐等化合物。作为这样的化合物例如可以列举SrCO3、Fe2O3等。初始原料的平均粒径不特别限定,例如为0.1~2.0μm。初始原料没有必要在预烧前的调配工序中混合全部,可以在预烧之后添加各化合物的一部分或者全部。
预烧工序为预烧在调配工序中获得的原料组合物的工序。预烧能够在空气等氧化性气氛中进行。预烧温度优选为800~1450℃,进一步优选为850~1300℃,更加优选为900~1200℃,预烧温度下的预烧时间优选为1秒~10小时,进一步优选为1分~3小时。通过预烧获得的预烧物中的Sr铁氧体的含量优选为70质量%以上,进一步优选为90质量%以上。预烧物的一次粒径优选为10μm以下,进一步优选为2.0μm以下。
粉碎工序是通过粉碎预烧物获得铁氧体磁铁粉末的工序。粉碎工序既可以以一个阶段进行也可以分成粗粉碎工序和微粉碎工序两个阶段进行。因为预烧物通常是颗粒状或者块状,所以优选首先进行粗粉碎工序。在粗粉碎工序中使用振动棒磨机等以干式进行粉碎,从而调制出平均粒径为0.5~5.0μm的粉碎粉。将这样调制出的粉碎粉用湿式磨碎机、球磨机或者喷射研磨机等以湿式进行粉碎,从而获得平均粒径为0.08~2.0μm,优选为0.1~1.0μm,更加优选为0.2~0.8μm的微粉末。
微粉末的用BET法测得的比表面积优选为5~14m2/g,更加优选为7~12m2/g。粉碎时间例如在使用湿式磨碎机的情况下为30分钟~20小时,在使用球磨机的情况下为5~50小时。这些时间优选根据粉碎方法来进行适当调整。
在粉碎工序中除了SiO2、Na2CO3以及ZnO的粉末之外,还可以添加CaCO3、SrCO3、BaCO3以及将稀土元素作为构成元素的氧化物(例如La2O3)等的粉末。作为具有Na作为构成元素的化合物除了碳酸盐之外可以使用硅酸盐或含有Na的有机化合物(分散剂等)。另外,作为具有Zn作为构成元素的化合物并不限定于氧化物,还可以从无机锌、有机锌化合物中适当选择。
通过添加这样的成分,可以提高烧结性并且提高磁特性。另外,因为这些成分在以湿式来成型的情况下可能与浆料的溶剂一起流出,所以优选要调配多于铁氧体烧结磁铁中的目标含量。
为了提高铁氧体烧结磁铁的磁取向度,优选在上述成分之外,在微粉碎工序中添加多元醇。多元醇的添加量相对于添加对象物为0.05~5.0质量%,优选为0.1~3.0质量%,更加优选为0.1~2.0质量%。另外,所添加的多元醇在磁场中成型工序后的烧成工序中被热分解而除去。
磁场中成型工序为在磁场中对由粉碎工序所获得的微粉末进行成型来制作成型体的工序。磁场中成型工序可以用干式成型或湿式成型的任一种方法进行。从提高磁取向度的观点出发,优选湿式成型。在进行湿式成型的情况下,可以以湿式进行微粉碎工序,从而调整所获得的浆料到规定的浓度并作为湿式成型用浆料。浆料的浓缩可以通过离心分离或压滤等来进行。
湿式成型用浆料中微粉末的含量优选为30~85质量%。作为浆料的分散介质可以使用水或者非水系溶剂。在湿式成型用浆料中在水之外还可以添加葡糖酸、葡糖酸盐、或者山梨糖醇等表面活性剂。使用这样的湿式成型用浆料来进行磁场中成型。成型压力例如为0.1~0.5吨/cm2,施加的磁场例如为5~15kOe。
烧成工序是烧成成型体并获得烧结体的工序。烧成工序通常是在空气等氧化性气氛中进行的。烧成温度优选为1050~1300℃,进一步优选为1150~1250℃。烧成温度下的烧成时间优选为0.5~3小时。由以上所述工序能够获得烧结体即铁氧体烧结磁铁10。另外,本发明的铁氧体烧结磁铁的制造方法并不限定于上述方法。
以上说明了本发明的优选的实施方式,但是本发明的铁氧体烧结磁铁以及电动机不限定于上述内容。例如,铁氧体烧结磁铁的形状并不限定于图1的形状,可以适当变更成适于上述各用途的形状。
实施例
以下参照实施例以及比较例进一步详细地说明本发明的内容,但是本发明并不限定于这些实施例。
(铁氧体烧结磁铁的制作)
首先,准备以下的初始原料。
·Fe2O3粉末(一次粒径:0.3μm)
·SrCO3粉末(一次粒径:2μm)
·SiO2粉末(一次粒径:0.01μm)
·CaCO3粉末
·MnO粉末
·ZnO粉末
·La2O3粉末
·Na2CO3粉末
[实施例1]
用湿式磨碎机粉碎并混合1000g的Fe2O3粉末、161.2g的SrCO3粉末以及2.3g的SiO2粉末,并且进行干燥和整粒。将这样获得的粉末在空气中在1250℃温度下烧成3小时,并获得了颗粒状的预烧物。使用干式振动棒磨机,将该预烧物进行粗粉碎,从而调制出用BET法测得的比表面积为1m2/g的粉末。
在200g粗粉碎了的粉末中添加规定量的山梨糖醇、SiO2粉末、CaCO3粉末、MnO粉末、La2O3粉末以及ZnO粉末,用球磨机进行24小时湿式粉碎从而获得了浆料。山梨糖醇的添加量为将粗粉碎了的粉末的质量作为基准为0.25质量%。粉碎后的微粉末的比表面积为8~10m2/g。
相对于粉碎结束后的浆料添加规定量的Na2CO3粉末而进行搅拌。之后,调整浆料的固体成分浓度,使用湿式磁场成型机并在12kOe的施加磁场中进行成型从而获得了成型体。制作了3个这样的成型体。将这些成型体在空气中分别在1170℃、1185℃以及1200℃下烧成,从而获得烧成温度不同的3种圆柱形状的铁氧体烧结磁铁(实施例1)。
[实施例2~23、比较例1~8]
另外,除了变更预烧前的SrCO3粉末的添加量、湿式粉碎之前的SiO2粉末的添加量、CaCO3粉末的添加量、ZnO粉末的添加量、MnO粉末的添加量、La2O3粉末的添加量以及添加到浆料的Na2CO3粉末的添加量中的至少一个之外,其余均以与实施例1同样的方法制作与实施例1组成不同的实施例2~23以及比较例1~8的铁氧体烧结磁铁。在各实施例以及比较例中,制作了烧成温度不同的3种铁氧体烧结磁铁。
(铁氧体烧结磁铁的评价)
〈组成分析〉
由电感耦合等离子体发射光谱分析(ICP分析)测定制作出的各实施例以及各比较例的铁氧体烧结磁铁的组成。铁氧体烧结磁铁除了含有Fe、Sr、Si、Ca等之外还被检测出来自包含于初始原料中的杂质的元素(Ba等)。
在表1中示出被检测出的将Fe、Sr、Ba、Al、Si、Ca、Mn、Zn、Cr、La、Co以及Na分别换算成Fe2O3、SrO、BaO、Al2O3、SiO2、CaO、MnO、ZnO、Cr2O3、La2O3、CoO以及Na2O时的含量。这些含量是以铁氧体烧结磁铁整体作为基准的值(质量%)。
进一步,针对在上述的组成分析中被检测出的Zn和La计算摩尔比La/Zn。
另外,上述组成分析中被检测出的Co、Mn、Zn、Cr以及Al与Fe一起构成通式(1)所表示的Sr铁氧体的B位,且La、Ba以及Ca与Sr一起构成通式(1)所表示的Sr铁氧体的A位,在此前提下,计算摩尔比α。
〈磁特性的评价〉
在加工了所制作出的圆柱形状的铁氧体烧结磁铁的上下面之后,使用最大施加磁场为25kOe的B-H测试仪测定了磁特性。在测定中,求得剩余磁通密度(Br)以及矫顽力(HcJ),并且测定剩余磁通密度(Br)成为90%时的外部磁场强度(Hk),据此求得矩形比(Hk/HcJ)(%)。在各实施例以及比较例中,将在分别以烧成温度为1170℃、1185℃以及1200℃制作出的铁氧体烧结磁铁中,剩余磁通密度(Br)与矩形比(Hk/HcJ)的平衡最为良好的1185℃下制作出的铁氧体烧结磁铁的磁特性示于表1中。
〈外观评价〉
在将所制作的铁氧体磁铁放置于空气中7天之后,目视其表面进行观察,并按以下的基准进行了评价。评价结果示于表1中。
A:在磁铁的表面没有产生裂纹。
B:在磁铁的表面产生了裂纹。
〈机械强度的评价〉
由以下的条件,通过3点弯曲试验来测定抗弯强度(σ)。
首先,与上述圆柱形状的铁氧体烧结磁铁不同,准备了如图2所示的弧状铁氧体烧结磁铁(长度L为36mm,宽度W为29mm,厚度T为2.5mm,从在设想包含弧的圆的情况下的圆的中心引出到弧的两端部的接线之间的角度R为78度)(样品A)。另外,烧成温度为1185℃。
接下来,如图3所示在水平的台的上面放置弧状铁氧体烧结磁铁(样品A),从上方向在箭头所指方向上加压(加压速度3mm/min)从而测定样品被破坏时的破坏最大负载F[N],由下述式(4)求得抗弯强度(σ)。结果示于表1中。另外,表1中所示的抗弯强度(σ)为30个样品的平均值。
σ[N/mm2]=3×L×F/(2×W×T2) (4)
如表1所示,实施例的铁氧体烧结磁铁没有产生裂纹,抗弯强度(σ)为150N/mm2以上,剩余磁通密度(Br)为440mT以上,且矩形比(Hk/HcJ)为85%以上。即,确认了本发明的铁氧体烧结磁铁通过ZnO的含量为特定的范围内并且M1/M2(La/Zn)的摩尔比在特定值以下从而发挥优异的磁特性。
进一步,对于实施例1~23的铁氧体烧结磁铁评价了Sr铁氧体的晶粒。具体如下进行。
在对铁氧体烧结磁铁的截面(a面)进行镜面研磨之后,用氢氟酸实施蚀刻。之后,用FE-SEM来观察蚀刻面。在将所观察的图像中的Sr铁氧体的晶粒轮廓清晰化之后,通过图像处理来测定Sr铁氧体晶粒的个数基准的粒度分布。进一步,根据粒度分布的数据求得Sr铁氧体的晶粒的个数基准的平均粒径以及标准偏差。
其结果,实施例1~23的铁氧体烧结磁铁的平均粒径都为1.0μm以下,标准偏差都为0.42以下。另外,粒径为2.0μm以上的晶粒相对于Sr铁氧体晶粒整体的个数基准的比例都在2%以下。这样确认了在实施例1~23的铁氧体烧结磁铁中所包含的Sr铁氧体晶粒充分细微并且具有高均匀性。
Claims (7)
1.一种铁氧体烧结磁铁,其特征在于:
以具有六方晶结构的M型Sr铁氧体作为主相,
Zn的含量换算成ZnO为0.05~1.35质量%,
在将稀土元素R的含量以摩尔换算记为M1,将所述Zn的含量以摩尔换算记为M2的情况下,M1/M2为0.43以下。
2.如权利要求1所述的铁氧体烧结磁铁,其特征在于:
Mn的含量换算成MnO小于0.5质量%。
3.如权利要求1或者2所述的铁氧体烧结磁铁,其特征在于:
在将Sr、R、Ba以及Ca的合计含量以摩尔换算记为M3,将Fe、Co、Mn、Zn、Cr以及Al的合计含量以摩尔换算记为M4,进一步将Si的含量以摩尔换算记为M5的情况下,满足
0.5≤[M3-(M4/12)]/M5≤1.2,
其中R表示稀土元素。
4.如权利要求1~3中任一项所述的铁氧体烧结磁铁,其特征在于:
Na的含量换算成Na2O为0.01~0.09质量%。
5.如权利要求1~4中任一项所述的铁氧体烧结磁铁,其特征在于:
所述Sr铁氧体的晶粒的平均粒径为1.0μm以下,粒径为2.0μm以上的所述晶粒的个数基准的比例为2%以下。
6.如权利要求1~5中任一项所述的铁氧体烧结磁铁,其特征在于:
剩余磁通密度Br为440mT以上,矩形比Hk/HcJ为85%以上。
7.一种电动机,其特征在于:
具备权利要求1~6中任一项所述的铁氧体烧结磁铁。
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JP2015181147A (ja) | 2015-10-15 |
US20150255198A1 (en) | 2015-09-10 |
US9627112B2 (en) | 2017-04-18 |
EP2916328A2 (en) | 2015-09-09 |
EP2916328A3 (en) | 2015-11-11 |
CN104900362B (zh) | 2017-09-01 |
EP2916328B1 (en) | 2017-02-08 |
KR20150105256A (ko) | 2015-09-16 |
KR101696343B1 (ko) | 2017-01-13 |
JP6596828B2 (ja) | 2019-10-30 |
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