CN1288573A - 铁氧体磁铁粉末、用该磁铁粉末的磁铁及它们的制造方法 - Google Patents

铁氧体磁铁粉末、用该磁铁粉末的磁铁及它们的制造方法 Download PDF

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CN1288573A
CN1288573A CN99802267A CN99802267A CN1288573A CN 1288573 A CN1288573 A CN 1288573A CN 99802267 A CN99802267 A CN 99802267A CN 99802267 A CN99802267 A CN 99802267A CN 1288573 A CN1288573 A CN 1288573A
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magnet
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ferrite
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CN1167087C (zh
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丰田幸夫
细川诚一
穴本修司
古地勇
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Hitachi Metals Ltd
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Abstract

一种La－Co系铁氧体磁铁粉末是用La置换Sr,并且用Co置换Fe,通过在超过1300℃及1450℃以下的温度进行焙烧来制造。由于用Co置换在沿晶体C轴向上或向下的状态的Fe的磁矩中的位置数具有多向的磁矩的Fe,其结果,发挥高的矫顽力。这样,能抑制饱和磁化σs的降低,同时能提高矫顽力。

Description

铁氧体磁铁粉末、用该磁铁粉末的磁铁及它们的制造方法
本发明涉及一种铁氧体磁铁粉末、用该磁铁粉末的磁铁以及这种磁铁粉末和磁铁的制造方法。
铁氧体是二价阳离子金属氧化物与三价铁的化合物的总称，而铁氧体磁铁用作电机或发电机等各种用途。作为铁氧体磁铁的材料，广泛采用具有氧化铅铁淦氧磁体型的六方晶体结构的Sr铁氧体(SrFe12O19)或Ba(Fe12O19)。这些铁氧体是以氧化铁和Sr或Ba等的碳酸盐为原料，通过粉末冶金法比较廉价地被制造。
氧化铅铁淦氧磁体型铁氧体的基本组成，通常用化学式“MO·nFe2O3”表示。元素M为由二价阳离子构成的金属，可从Sr、Ba、Pb、Ni或其它金属中选择。该铁氧体中的各位置的铁离子(Fe3+)具有自旋磁矩，由氧离子(O-2)通过超交换互相作用而结合。在Fe3+的各位置上，Fe3+的磁矩沿C轴处于“向上”或“向下”的状态。当在具有“向上”的磁矩位置的个数与具有“向下”的磁矩位置的个数之间有差异时，作为整个晶体显示出强磁性(铁磁性体)。
在氧化铅铁淦氧磁体型铁氧体磁铁的磁性能中，人们知道剩余磁感应强度(Br)能提高晶体的Is、并通过增加烧结体的密度及晶体的取向性，得以改善。另外，人们也知道通过提高单磁晶体的存在率能改善矫顽力(HCJ)。但是，以提高剩余磁感应强度为目的当提高烧结体的密度时，由于助长了晶体成长，降低了矫顽力(HCJ)。相反，通过添加Al2O3等，控制晶粒大小并由此提高矫顽力，则造成烧结体的密度降低，并降低了剩余磁感应强度。为了改善这种铁氧体磁铁的磁特性，曾对铁氧体的组成、添加物及制造条件进行了各种研究，但是难于开发能同时提高剩余磁感应强度和矫顽力两者的铁氧体磁铁。
本申请人曾开发了一种通过向原料中添加Co在不使剩余磁感应强度降低的同时又能提高矫顽力的铁氧体磁铁(特公平4-40843公报)。
其后，又提出通过用Zn置换Fe并用La置换Sr提高饱和磁化(σs)的铁氧体磁铁(特开平9-115715号公报以及特开平10-149910号公报)。铁氧体磁铁为如上述，Fe3+的磁矩通过各位置向相反方向的铁磁体，因此其饱和磁化相对的低。但是，在上述公报中，通过将具有比Fe的磁矩小的磁矩的离子置于Fe离子的特定位置上，减少“向下”的磁矩，由此能提高饱和磁化σs。另外，在该公报中，是用Nd或Pr代替La为例，也可用Mn、Co、Ni代替Zn。
在日本应用磁学会学术讲演集(1998年9月20日发表)，报导了一种利用添加了La及Co的Sr1-xLaxCox·Fe12-xO19组合物可使矫顽力(HCJ)和饱和磁化(σs)都提高的铁氧体磁铁。
但是，即使在这些铁氧磁铁中，对改善矫顽力及磁化两者的特性是不充分的。特别是对用Co置换Fe并用La置换Sr的Sr1-xLaxCox·Fe12-xO19组合物，在如特开平10-149910号公报中所公开的温度(1200℃)下进行焙烧时，存在即使饱和磁化σs高但矫顽力不高的问题。
在上述日本应用磁学会学术讲演集(1998年9月20日发表)中，报导了通过用Co代替Zn并置换铁能一定程度改善矫顽力，但是，没说明其原因，并且改善矫顽力及改善剩余磁感应强度的程度也不充分。
鉴于上述问题，本发明的主要目的是提供一种能使饱和磁化和矫顽力都提高的铁氧体磁铁粉末以及用该磁铁粉末的磁石。
本发明的磁铁粉末为具有用(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO所表示的铁氧体为主相的磁铁粉末，x和y表示摩尔比，0.1≤x≤0.4，0.1≤y≤0.4，5.5≤n≤6.5，并且用Co置换Fe,Fe是在沿晶体的C轴向上或向下的状态的Fe的磁矩中的位置数具有多向的磁矩的Fe。
上述焙烧在超过1300℃的温度下进行是理想的。
在理想的实施例中，室温的各向异性磁场HA为1750KA/m(22KOe)以上，室温的饱和磁化σs为84.78μWbm/kg(67.5emu/g)以上。
本发明的粘结磁铁，其特征在于含有上述磁铁粉末。另外，本发明的烧结磁铁，其特征在于由磁铁粉末所形成的。
本发明的磁铁粉末的制造方法，包括准备对SrCO3及Fe2O3的粉末中添加La及Co的各自氧化物粉末的原料混合粉末的工序、在超过1300℃的温度及在1450℃以下温度焙烧上述原料混合粉末并且由此，形成是具有(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO(0.1≤x≤0.4、0.1≤y≤0.4、5.5≤n≤6.5)组成的铁氧体的焙烧物的工序，和粉碎所述焙烧物的工序。另外，所谓准备原料混合粉末的情况，也包括购入商品原料混合粉末的情况或者混合商品粉末的情况。
上述焙烧在超过1350℃温度下进行是理想的。
本发明的磁铁的制造方法，包括准备对SrCO3及Fe2O3的粉末中添加La及Co的各自氧化物粉末的原料混合粉末的工序，在超过1300℃的温度和在1450℃温度以下焙烧上述原料混合粉末，并且由此形成是具有(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO(0.1≤x≤0.4、0.1≤y≤0.4、5.5≤n≤6.5)组成的铁氧体的焙烧物的工序，粉碎上述焙烧物并形成铁氧体磁铁粉末的工序，和成型并烧结上述铁氧体磁铁粉末的工序。
本发明的另一种磁铁的制造方法，包括准备对SrCO3及Fe2O3的粉末中添加La及Co的各自氧化物粉末的原料混合粉末的工序、在超过1300℃的温度及1450℃以下的温度焙烧所述原料混合粉末，并且由此形成具有(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO(0.1≤x≤0.1、0.1≤y≤0.4、5.5≤n≤6.5)的组成的铁氧体的焙烧物的工序，粉碎上述焙烧物并形成铁氧体磁铁粉末的工序，和由所述铁氧体磁铁粉末形成粘结磁铁的工序。
上述的焙烧在1350℃以上温度进行是理想的。
本发明的磁铁粉末，是具有用(1-x)AO·(x/2)B2O3·(n-y/2)Fe2O3·yCoO所表示的铁氧体为主相的磁铁粉末；元素A为从Sr、Ba、Ca及Pb中选择至少一种元素，元素B含有从含Y的稀土元素及Bi中所选择的至少一种元素，X及Y表示摩尔比为0.1≤x≤0.4、0.1≤y≤0.4、5.5≤n≤6.5；并且用Co置换Fe，该铁是在沿晶体的C轴为向上或向下状态的Fe的磁矩中位置数具有多向的磁矩的铁。
上述焙烧在超过1300℃的温度下进行是理想的。
本发明的其它的磁铁，其特征在于可由上述磁铁粉末所形成。
下面对附图进行简单的说明。
图1为表示对于本发明的实施例及比较例的饱和磁化σs与焙烧温度的关系的曲线图。
图2为表示对于本发明的实施例及比较例的各向异性磁场HA与焙烧温度的关系的曲线图。
图3为表示对于本发明的实施例及比较例的饱和磁化σs及各向异性磁场HA与置换量的关系的曲线图(x=y)。
图4为表示本发明的实施例的焙烧温度为1200℃、1300℃及1400℃时的X射线衍射图谱的曲线图。
图5-(a)为表示焙烧温度为1300℃以下时的Fe与Co的置换的模式图，图5(b)为表示焙烧温度超过1300℃时的Fe与Co的置换的模式图。
本发明的磁铁粉末具有用(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO所表示的氧化铅铁淦氧磁体型铁氧体的为主相。一部分Sr用La置换，其置换量X为0.1≤x≤0.4的范围。一部分Fe用Co置换，其置换量Y为0.1≤y≤0.4的范围。另外，n为5.5≤n≤6.5的范围。
在用Co置换Fe时，焙烧温度若为通常的温度范围(1200℃左右)，则提高饱和磁化。但是，当使焙烧温度上升到比通常的温度范围高时，则可观察到饱和磁化降低的现象。
本发明人发现，当将La及Co添加到原料粉末中并在超过1300℃的温度下进行焙烧时，则既能抑制饱和磁化的降低又能提高矫顽力(各向异性磁场)。可以认为其理由是通过增加焙烧温度变更Co与Fe的置换位置(地点)，由此能改善磁特性，更详细的如下述。
在氧化铅铁淦氧磁体型铁氧体中，化学组成为Sr0.6(Fe2O3)时，每个晶胞单位含有12个Fe3+离子。其中，8个Fe3+离子沿晶体C轴具有向上的磁矩，而4个F3+沿晶体C轴具有向下的磁矩。另外，在本说明书中，8个Fe3+离子(位置数多的)以具有的磁矩的取向为“向上”形式表现，但是也可以将该取向为“向下”，而将其余4个F3+离子所表示的磁矩的取向为“向上”。下面为了简化，以位置数多的磁矩取向为“向上”进行说明。
在这样的铁氧体中，当用Co置换部分Fe时，可以认为焙烧温度为1200℃以上1300℃以下时，Co与具有向下的磁矩的Fe置换(图5(a))，而当焙烧温度超过1300℃时，Co与具有向上的磁矩的Fe置换(图5(b))。由于Co磁矩与Fe的磁矩相比小，因此当Co置换具有向下的磁矩的Fe时，则铁氧体的饱和磁化提高，如图5(b)所示，当Co置换具有向上的磁矩的铁时，则铁氧体的饱和磁化将降低。但是能充分地提高各向异性磁场(矫顽力)。
另外，当焙烧温度超过1450℃时，晶粒过于生长，在粉碎工序中可能会产生需要加大粉碎时间的情况。
如上所述，焙烧温度超过1300℃，并且设定在1450℃的温度范围内是理想的。为了实现更高的磁特性，焙烧温度在1350℃到1450℃的范围是理想的。
按本发明，能得到室温的各向异性磁场HA超过19×79.58KA/m(=19KOe=1512KA/m)，并且饱和磁化σs超过66.5×1.256μWbm/kg(=66.5emu/g=83.52μWbm/kg)的磁特性。通过调整组成比(置换量)与焙烧温度，可以达到具有各向异性磁场HA为19.5×79.58KA/m(=19.5KOe=1631KA/m)，饱和磁化σs为69.2×1.256μWbm/kg(=69.2emu/g=86.91μWbm/kg)，并且各向异性磁场HA为26×79.58KA/m(=26KOe=2069KA/m)饱和磁化σs为67.71×1.256μWbm/kg(=67.7emu/g=85.03μWbm/kg)的磁特性。
另外，在本发明中，由于用价数不同的Co2+置换氧化铅铁淦氧磁体型铁型氧体的Fe3+，用La置换部分Sr，并补充上述价数的不同。因此，置换量X大致等于置换量Y是理想的。但是，本发明不限定于X=Y的情况。
下面，说明本发明的磁铁粉末的制造方法。
首先，按从1∶5.5到1∶6.5范围的摩尔比混合SrCo3的粉末与Fe2O3(α氧化铁)的粉末。这时，将La2O3及CoO等添加到原料粉末中。各粉末的一次粒径如下：SrCo3：约0.8μm、Fe2O3：约0.5μm、La2O3：约1.0μm、CoO：约为1.0μm。
添加La及Co为以La及Co的各自氧化物的粉末进行添加是理想的，但是也可以为除氧化物外的化合物(例如碳酸盐、氢氧化物、硝酸盐等)的粉末状态。
对于上述粉末，根据需要也可添加1重量％程度的含SiO2、CaCO3、SrCO3、Al2O3、Cr2O3等的其它的化合物。
然后，用转炉在空气中将混合的原料粉末加热到1300-1450℃，并通过固相反应形成氧化铅铁淦氧磁体型铁氧体的铁氧体化合物。将该过程称之为“焙烧”，而将所得的化合物称之为“焙烧物”。焙烧时间为1-5小时是理想的。
由该焙烧工序所得的焙烧物具有用以下化学式所表示的氧化铅铁淦氧磁体型铁氧体为主相，且其平均粒径为1-10μm范围，
(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO,0.1≤x=y≤0.4、5.5≤n≤6.5。
通过粉碎或解碎该焙烧物能得到本发明的磁铁粉末。
图1及图2表示对于不同置换量X的各种试料磁特性与焙烧温度的关系。图1曲线的纵轴表示饱和磁化，横轴表示置换量X(=Y)。图2的曲线的纵轴表示各向异性磁场，而横轴表示置换量X(=Y)。
在图1及图2中，记录对置换量为0-0.5的样品的测定值，而饱和磁化σs及各性异性磁场HA都可由脉冲磁化装置进行测定。测定在室温(23℃)下进行，其测定法如下。
通常，强磁体(铁磁性体)或在铁磁性体的强磁场的磁化曲线用下式表示。
I=Is(1-a/H-b/H2+…)+XoμoH
该式被称作饱和渐近法则，第一项的磁矩为除晶体各向异性外其它原因完全不包括磁场的方向所产生的项。第2项的磁矩的大小为根据磁场所增加的项。为了由实验求出自发磁化Is，在磁各向异性不特别大时(K1-104J/m3)对于H为106A/m以上的磁场，由于几乎可以不计b/H2项，因此，对于其以外的磁场通过讨论H或a/H构成项存在的有无并对前者以H为O，而后者1/H为O可求出Is。
另外，在测定摩尔比6.0的氧化铅铁淦氧磁体型Sr铁氧体(SrO·6Fe2O3)的焙烧粉末的磁化曲线中，磁化I的外部磁场H在30×79.58KA/m(=30KOe=2387KA/m)以上成直线。为此，上式中的第一项成Is，第二项的H成一次式，因此，将H外插入O，使其Y部分成σs。其结果，Sr0.6Fe2O3的饱和磁化为(69.2±0.1)×1.256μWb/kg。另外，各向异性磁场HA利用同脉冲磁化测定装置由二阶微分磁化率的测定可以求得。其结果，Sr0.6Fe2O3的HA为1.43MA/m(18KOe)。
图3表示各向异性磁场HA及饱和磁化σs与置换量的关系。
由图1-图3可知：
1．当添加La及Co时，则磁特性变得依赖焙烧温度。特别是，各向异性磁场HA与焙烧温度关系，当La及Co的置换量大时变大；
2．在置换量为0.1以上时，各向异性磁场HA增大到18KOe以上。另外，焙烧温度越高，各向异性磁场HA的增加越显著。各向异性磁场HA的增加程度在置换量为0.3时最大(图2)；
3．当置换量X超过0.4并再增大时，随着焙烧温度的增加饱和磁化σs出现降低的倾向(图3)；
4．在将饱和磁化σs维持在67.5×1.256μWbm/kg(=67.5emu/g=84.78μWbm/kg)以上的同时为达到22×79.58KA/m(=22KOe=1750KA/m)以上的各向异性磁场，可将置换量为0.2-0.3的范围，并且使焙烧温度超过1300℃。
图4表示焙烧温度为1200℃、1300℃及1400℃时的X射线衍射图。衍射图与焙烧湿度几乎没有关系。但是，从图1所示的数据可知，焙烧温度越高，焙烧物的各向异性磁场HA越提高。焙烧温度越高，越能改善各向异性磁场的理由可认为是，如前所述，是因为产生Co与Fe的置换的位置由于焙烧温度的高低变化所致。
按本发明，焙烧温度超过1300℃并在1450℃以下，通过用Co置换Fe能抑制饱和磁化σs的降低，同时能大幅度提高各向异性磁场HA。
其次，说明本发明的铁氧体磁铁的制造方法。
首先，按上述方法制造焙烧物。其次，通过用振动磨机、球磨机和/或粉碎机微粉碎焙烧物的工序将焙烧物粉碎成微粒子。微粒子的平均粒径为0.4-0.7μm程度(用空气透过法)是理想的。微粉碎工序将干式粉碎和湿式粉碎组合进行是理想的。在进行湿式粉碎时，可用水等水系溶剂或各种非水系溶剂。在湿式粉碎时，生成混合溶剂和焙烧物粉末的料浆。在料浆中添加各种公知的表面活性剂是理想的。
然后，除去料浆中的溶剂，同时在磁场中或非磁场中加压成型。在加压成型后，经过脱脂工序、烧结工序、加工工序、洗涤工序、检查工序等公知的制造过程，最后完成铁氧体磁铁的制品。烧结工序在空气中，例如从1200℃到1250℃的温度范围进行0.5-2小时。在烧结工序所得的烧结磁铁的平均粒径例如为1-1.5μm。
另外，使上述铁氧体磁铁粉末与具有弹性的橡胶或硬轻质的塑料等混合并固化也可制作粘结磁铁。这时，将本发明的磁铁粉末与胶粘剂及添加物混合和混练之后，进行成型加工。成型加工可通过注射成型、挤压成型、滚轧成型等方法进行。
在本发明中，通过在此前述的比较高的温度下进行焙烧，能谋求提高磁特性，当提高焙烧温度，则通常其后的粉碎变得困难，烧结性也变差。因此，焙烧温度低(例如，为1200℃)被认为是理想的。在本发明中，由于将焙烧温度提高到1300℃以上的高温，在焙烧前进行微细地造粒，不使在造粒粉以上晶粒成长，或通过辊磨机或棒磨机等粗粉碎晶粒成长的粒子等的处理可排除由高焙烧温度的弊病。
还有，也可用从Ba、Ca及Pb中所选择的至少一种元素代替Sr。另外，也可用与La同时，从含Y的稀土元素及Bi中选择至少一种元素代替La置换一部分Sr。
实施例
首先，在(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO的组成中，通过在1350℃焙烧按X=Y=0.3所配合的原料粉末制作本发明的磁铁粉末。
其次，将该磁铁粉末再微粉碎到0.52μm的大小后，在所得的微粉碎物中添加并混合CaCO3=0.7wt％、SiO2=0.4wt％。在磁场中成型这样所得的微粉碎粉后，在1230℃焙烧30分钟，制作烧结磁铁。
所得的烧结磁铁的特性，剩余磁感应强度Br=0.44T、矫顽力Hcj=4.6×79.58kA/m、(BH)max=4.7×7.958KJ/m3。
按本发明，由于同时能实现提高焙烧物及磁铁粉末的饱和磁化及矫顽力，因此，可以制造磁特性优异的磁铁。

Claims (13)

1．一种铁粉末，其特征在于是具有用(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO所表示的铁氧体为主相，x及y表示摩尔比为
0.1≤x≤0.4，
0.1≤y≤0.4，
5.5≤n≤6.5，
并且，用Co置换在沿晶体C轴为向上或向下状态的Fe的磁矩中位置数具有多向的磁矩的Fe。
2．根据权利要求1所述的磁铁粉末，其特征在于在超过1300℃的温度下进行焙烧。
3．根据权利要求1或2所述的磁铁粉末，其特征在于在室温中，各向异性磁场HA为1750KA/m以上，饱和磁化可为84.78μm Wbm/kg以上。
4．一种粘结磁铁，含有权利要求1-3中任何一项所述的磁铁粉末。
5．一种烧结磁铁，是由权利要求1-3中任何一项所述的磁铁粉末所形成的。
6．一种磁铁粉末的制造方法，包括准备对SrCO3及Fe2O3的粉末中添加La及Co的各自氧化物粉末的原料混合粉末的工序、在超过1300℃的温度及在1450℃以下温度焙烧上述原料混合粉末并且由此形成是具有(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO(0.1≤x≤0.4、0.1≤y≤0.4、5.5≤n≤6.5)组成的铁氧体的焙烧物的工序，和粉碎所述焙烧物的工序。
7．根据权利要求6所述的磁铁粉末的制造方法，其特征在于在1350℃以上温度进行所述焙烧。
8．一种磁铁的制造方法，包括准备对SrCO3及Fe2O3的粉末中添加La及Co的各自氧化物粉末的原料混合粉末的工序、在超过1300℃的温度和在1450℃以下的温度焙烧所述原料混合粉末，并且由此形成是具有(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO(0.1≤x≤0.4、0.1≤y≤0.4、5.5≤n≤6.5)组成的铁氧体的焙烧物的工序，粉碎所述焙烧物并形成铁氧体磁铁粉末的工序和成型并烧结所述铁氧体磁铁粉末的工序。
9．一种磁铁的制造方法，包括准备对SrCO3及Fe2O3的粉末中添加La及Co的各自氧化物粉末的原料混合粉末的工序、在超过1300℃的温度和1450℃以下的温度焙烧所述原料混合粉末，并且由此形成具有(1-x)SrO·(x/2)La2O3·(n-y/2)Fe2O3·yCoO(0.1≤x≤0.1、0.1≤y≤0.4、5.5≤n≤6.5)组成的铁氧体的焙烧物的工序，粉碎所述焙烧物并形成铁氧体磁铁粉末的工序和由所述铁氧体磁铁粉末形成粘结磁铁的工序。
10．根据权利要求8或9所述的磁铁的制造方法，其特征在于在1350℃以上温度进行所述焙烧。
11．一种磁铁粉末，其特征在于为具有用(1-x)AO·(x/2)B2O3·(n-y/2)Fe2O3·yCoO所表示的铁氧体为主相的磁铁粉末；元素A为从Sr、Ba、Ca及Pb中选择至少一种元素，元素B含有从含Y的稀土元素及Bi中所选择的至少一种元素，X及Y表示摩尔比为0.1≤x≤0.4、0.1≤y≤0.4、5.5≤n≤6.5；并且用Co置换Fe，该Fe为沿晶体的C轴为向上或向下状态的Fe的磁矩中位置数具有多向的磁矩的铁。
12．根据权利要求11所述的磁铁粉末，其特征在于在1300℃的温度下进行焙烧。
13．一种磁铁，是由权利要求11或12所述的磁铁粉末所形成的。
CNB998022675A 1998-11-26 1999-11-25 铁氧体磁铁粉末、用该磁铁粉末的磁铁及它们的制造方法 Expired - Lifetime CN1167087C (zh)

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