CN113677625A - 铁氧体烧结磁体、铁氧体颗粒、粘结磁体和旋转电气设备 - Google Patents
铁氧体烧结磁体、铁氧体颗粒、粘结磁体和旋转电气设备 Download PDFInfo
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- CN113677625A CN113677625A CN202080023625.3A CN202080023625A CN113677625A CN 113677625 A CN113677625 A CN 113677625A CN 202080023625 A CN202080023625 A CN 202080023625A CN 113677625 A CN113677625 A CN 113677625A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/66—Cobaltates containing alkaline earth metals, e.g. SrCoO3
- C01G51/68—Cobaltates containing alkaline earth metals, e.g. SrCoO3 containing rare earth, e.g. La0.3Sr0.7CoO3
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2641—Compositions containing one or more ferrites of the group comprising rare earth metals and one or more ferrites of the group comprising alkali metals, alkaline earth metals or lead
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract
该磁体是含有具有磁铅石型的结晶结构的铁氧体相的铁氧体烧结磁体，至少含有金属元素A、金属元素R、Fe、Co、Zn及B。金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca。金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La。金属元素的原子比率满足下式。A1－rRrFexCoyZnz(1)，0.40≤r≤0.70(2)，8.20≤x≤9.34(3)，0.05＜y≤0.50(4)，0＜z≤0.20(5)，另外，Si的含量以SiO2换算计为0～0.60质量％，B的含量以B2O3换算计为0.01～0.70质量％。
Description
技术领域
本发明涉及铁氧体烧结磁体、铁氧体颗粒、粘结磁体和旋转电气设备。
背景技术
作为用于铁氧体烧结磁体的磁性材料，已知具有六方晶系晶体结构的Ba铁氧体、Sr铁氧体及Ca铁氧体。作为这种铁氧体的晶体结构，已知有磁铅石型(M型)和W型等。在这些结构中，作为电动机用等的磁体材料，主要采用磁铅石型(M型)的铁氧体。M型铁氧体通常以AFe12O19的通式表示。
作为铁氧体烧结磁体的磁特性的指标，一般采用残留磁通密度(Br)和矫顽力(HcJ)。目前，从提高Br和HcJ的观点来看，尝试了添加与铁氧体的构成元素不同的各种元素。例如在专利文献1中，尝试着通过使用Ca及稀土元素(R)置换A位点的元素的一部分且使用Co置换B位点的元素的一部分而改善磁特性。
现有技术文献
专利文献
专利文献1：国际公开第2018/117261号
发明内容
发明所要解决的问题
但是，期望进一步提高常温下的Br及HcJ。
因此，本发明的一个方面的目的在于，提供常温下的Br及HcJ优异的铁氧体烧结磁体等。
用于解决问题的技术方案
本发明提供一种铁氧体烧结磁体，其含有具有磁铅石型的结晶结构的铁氧体相。该磁体至少含有金属元素A、金属元素R、Fe、Co、Zn和B。
金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca。
金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La。
在以(1)式表示金属元素的原子比率时，该铁氧体烧结磁体中，
r、x、y和z满足下述(2)～(5)式。
A1－rRrFexCoyZnz(1)，
0.40≤r≤0.70(2)，
8.20≤x≤9.34(3)，
0.05＜y≤0.50(4)，
0＜z≤0.20(5)，
另外，该铁氧体烧结磁体的Si的含量以SiO2换算计为0～0.60质量％，B的含量以B2O3换算计为0.01～0.70质量％。
在此，Si的含量能够以SiO2换算计为0.01～0.40质量％，B的含量能够以B2O3换算计为0.20～0.70质量％。
在此，所述铁氧体烧结磁体的Ca能够占据金属元素A的95原子％以上。
本发明的旋转电气设备具备上述任一项的铁氧体烧结磁体。
本发明提供一种铁氧体颗粒，其含有具有磁铅石型的结晶结构的铁氧体相的铁氧体颗粒。该铁氧体颗粒至少含有金属元素A、金属元素R、Fe、Co、Zn和B。
金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca。
金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La。
以(1)式表示金属元素的原子比率时，铁氧体颗粒中，
r、x、y和z满足下述(2)～(5)式。
A1－rRrFexCoyZnz(1)，
0.40≤r≤0.70(2)，
8.20≤x≤9.34(3)，
0.05＜y≤0.50(4)，
0＜z≤0.20(5)，
而且，铁氧体颗粒的Si的含量以SiO2换算计为0～0.60质量％，B的含量以B2O3换算计为0.01～0.70质量％。
在此，Si的含量能够以SiO2换算计为0.01～0.40质量％，B的含量能够以B2O3换算计为0.20～0.70质量％。
在此，在上述铁氧体颗粒中，Ca能够占据金属元素A的95原子％以上。
本发明提供一种粘结磁体，其含有上述任一项的铁氧体颗粒。
本发明提供一个旋转电气设备，其具备上述粘结磁体。
本发明的另一发明提供的铁氧体烧结磁体或铁氧体颗粒是含有具有磁铅石型的结晶结构的铁氧体相的铁氧体烧结磁体或铁氧体颗粒是，其中，
至少含有金属元素A、金属元素R、Fe、Co、Zn、Si和B，
金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca，
金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La，
以(1)式表示金属元素的原子比率时，
r、x、y和z满足下述(2)～(5)式，
A1－rRrFexCoyZnz(1)，
0.300＜r＜0.800(2)，
8.200＜x≤9.340(3)，
0＜y＜0.500(4)，
0＜z＜0.200(5)，
Si的含量以SiO2换算计为0.010～0.400质量％，B的含量以B2O3换算计为0.200～0.700质量％。
发明效果
根据本发明，提供常温下的Br及HcJ优异的铁氧体烧结磁体等。
附图说明
图1是铁氧体烧结磁体的截面示意图。
图2是表示电动机的一个实施方式的示意剖视图。
具体实施方式
以下，详细地说明本发明的几个实施方式。
本发明的实施方式的铁氧体烧结磁体及铁氧体颗粒是含有具有磁铅石型的结晶结构的铁氧体相的铁氧体烧结磁体。
该铁氧体烧结磁体及铁氧体颗粒至少含有金属元素A、金属元素R、Fe、Co、Zn和B。
金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca。
从抑制Br及HcJ的温度系数的观点来看，金属元素A中的Ca的原子比率能够为50原子％以上，能够为70原子％以上，能够为90原子％以上，能够为95原子％以上，能够为97原子％以上，能够为99原子％以上，也能够为100原子％。占据金属元素A的、Ca以外的原子的比率没有特别限定。
金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La。
稀土元素是钇(Y)、钪(Sc)、镧(La)、铈(Ce)、镨(Pr)、钕(Nd)、钷(Pm)、钐(Sm)、铕(Eu)、钆(Gd)、铽(Tb)、镝(Dy)、钬(Ho)、铒(Er)、铥(Tm)、镱(Yb)和镥(Lu)。
金属元素R优选含有选自由La(镧)、Pr(镨)和Nd(钕)构成的组中的1种以上的元素，更优选必须含有La。在金属元素R中能够含有50原子％以上的La，能够将La含有95原子％以上，能够含有99原子％，也可以为100原子％。
本发明的实施方式的铁氧体烧结磁体及铁氧体颗粒中，以(1)式表示金属元素的原子比率时，r、x、y和z满足下述(2)～(5)式。
A1－rRrFexCoyZnz(1)，
0.40≤r≤0.70(2)，
8.20≤x≤9.34(3)，
0.05＜y≤0.50(4)，
0＜z≤0.20(5)，
从进一步提高Br及HcJ的观点来看，通式(1)中的r也可以为0.45以上。从同样的观点来看，r可以为0.60以下，也可以为0.55以下。
从进一步提高Br的观点来看，通式(1)中的x可以为8.3以上，也可以为8.5以上。从进一步提高Br及HcJ的观点来看，x可以为9.3以下，也可以为9.2以下，也可以为9.15以下。
从进一步提高Br的观点来看，通式(1)中的y也可以为0.45以下，也可以为0.4以下。从同样的观点来看，通式(1)中的y可以为0.1以上，也可以为0.2以上。
从进一步提高，Br及HcJ的观点来看，通式(1)中的z可以为0.001以上，也可以为0.002以上，也可以为0.003以上，也可以为0.005，也可以为0.01以上，也可以为0.05以上。从提高HcJ及降低HcJ的温度系数的绝对值的观点来看，通式(1)中的z也可以为0.15以下，也可以为0.1以下。
本发明的实施方式的铁氧体烧结磁体及铁氧体颗粒中的Si的含量以SiO2换算计为0～0.60质量％，也可以为0.01～0.40质量％，B的含量以B2O3换算计为0.01～0.70质量％，也可以为0.20～0.70质量％。此外，铁氧体烧结磁体也可以不含有Si。
就铁氧体烧结磁体及铁氧体颗粒中的Si的含量而言，从进一步提高Br及HcJ的观点来看，将Si换算成SiO2，例如可以为0.01质量％以上，也可以为0.02质量％以上，也可以为0.05质量％以上，也可以为0.1质量％以上，也可以为0.2质量％以上。从同样的观点来看，就铁氧体烧结磁体及铁氧体颗粒中的Si的含量而言，将Si换算成SiO2，可以为0.5质量％以下，也可以为0.4质量％以下，也可以为0.35质量％以下。
从提高Br及HcJ的观点来看，铁氧体烧结磁体及铁氧体颗粒中的B的含量以B2O3换算计可以为0.1质量％以上，也可以为0.2质量％以上，也可以为0.3质量％以上，也可以为0.4质量％以上。从同样的观点来看，B的上述含量可以为0.65质量％以下，也可以为0.6质量％以下。
本实施方式的铁氧体烧结磁体及铁氧体颗粒也可以作为副成分，除了含有Bi和Si之外，还含有其它的副成分。例如，首先，作为副成分也可以含有Ca成分。但是，本实施方式的铁氧体烧结磁体含有Ca作为上述那样构成主相即铁氧体相的成分。因此，在作为副成分含有Ca的情况下，例如从烧结体分析的Ca的量成为主相及副成分的总量。因此，在使用了Ca成分作为副成分的情况下，(1)式中的金属元素A中的Ca的原子比率成为也含有副成分的值。Ca的原子比率的范围是基于烧结后分析的组成而确定的范围，因此，能够适用于作为副成分含有Ca成分的情况和不含有Ca成分的两种情况。
铁氧体烧结磁体及铁氧体颗粒中，除了上述的成分之外，也可以含有源自原料所含有的杂质或制造设备的不可避免的成分。作为这种成分，例如可举出Ti(钛)、Cr(铬)、Mn(锰)、Mo(钼)、V(钒)及Al(铝)等。这些成分也可以作为各自的氧化物或复合氧化物包含于铁氧体烧结磁体及铁氧体颗粒中。副成分也可以在铁氧体烧结磁体中的铁氧体晶粒的晶界偏析而构成异相。
铁氧体烧结磁体及铁氧体颗粒中的金属元素的含有比率能够通过荧光X射线分析进行测定。
铁氧体烧结磁体及铁氧体颗粒中的B(硼)及Si(硅)等半金属元素的含量能够通过电感耦合等离子体发射光谱分析(ICP发射光谱分析)进行测定。
图1是本发明的实施方式的铁氧体烧结磁体(铁氧体颗粒)100的截面示意图。如图1所示，本发明的实施方式的铁氧体烧结磁体(铁氧体颗粒)100含有具有磁铅石型(M型)的结晶结构的铁氧体相(晶粒)4和存在于铁氧体相(晶粒)4间的晶界相6。
M型铁氧体具有六方晶型的结晶结构。M型铁氧体的例子是由下式(III)表示的铁氧体。
MX12O19(III)
M必须含有Ca，也可以含有Sr及/或Ba。M也可以含有R。X含有Fe，也可以含有Co及Zn。
此外，上式(III)中的M(A位点)及X(B位点)的比率及氧(O)的比率实际上会显示为稍微偏离上述范围的值，因此，也可以稍微偏离上述的数值。
从充分提高磁特性的观点来看，铁氧体烧结磁体及铁氧体颗粒作为主相优选具有上述铁氧体相4。此外，本说明书中“作为主相”是指铁氧体烧结磁体及铁氧体颗粒中质量比例最多的晶相。铁氧体烧结磁体及铁氧体颗粒也可以具有与主相不同的晶相(异相)。主相的比例可以为70质量％以上，也可以为80质量％以上，也可以为90质量％以上，也可以为95质量％以上。
铁氧体烧结磁体中的铁氧体相(晶粒)的平均粒径例如可以为5μm以下，也可以为4.0μm以下，也可以为0.5～3.0μm。通过具有这种平均粒径，能够进一步提高矫顽力。铁氧体相(晶粒)的平均粒径能够使用TEM或SEM的截面的观察图像求得。具体而言，通过图像解析求得含有数百个铁氧体相(晶粒)的SEM或TEM的截面中的各主相粒子的截面面积之后，将具有该截面面积的圆的直径(圆当量直径)定义为该截面中的该主相粒子的粒径并测定粒径分布。根据测定的个数基准的粒径分布，计算铁氧体相(晶粒)的粒径的个数基准的平均值。将这样测定的平均值设为铁氧体相的平均粒径。
晶界相6以氧化物为主成分。具体而言，氧化物的例子可举出具有选自Si(硅)、B(硼)、Ca(钙)、Sr(锶)、Ba(钡)、Fe(铁)、Mn(锰)、Co、钴、Cr(铬)、Zn(锌)和Al(铝)中的至少一种的氧化物以及它们两种以上的复合氧化物。作为这种氧化物，例如可举出：SiO2、B2O3、CaO、BaO、SrO，Fe2O3、Co3O4，ZnO、Al2O3、MnO、Cr2O3等。另外，也可以含有硅酸玻璃。氧化物的质量比例能够为90％以上，也能够为95％以上，也能够为97％以上。
在铁氧体烧结磁体的截面中，晶界相6占据铁氧体相4及晶界相6的合计的面积比率能够设为0.1～5％。
铁氧体烧结磁体的形状没有特别限定，例如能够采用以端面成为圆弧状的方式弯曲的圆弧段形状(C型)形状、平板形状等各种形状。
铁氧体颗粒例如能够通过后述的粉碎工序获得。铁氧体颗粒的平均粒径例如为0.1～7μm。铁氧体颗粒的平均粒径也与铁氧体烧结磁体的晶粒的平均粒径一样，能够使用TEM或SEM的铁氧体颗粒的观察图像求得。具体而言，通过图像解析求得含有数百个铁氧体颗粒的SEM或TEM的各主相粒子的面积之后，将具有该面积的圆的直径(圆当量直径)定义为该铁氧体颗粒的粒径并测定粒径分布。根据测定的个数基准的粒径分布，计算铁氧体颗粒的粒径的个数基准的平均值。将这样测定的平均值设为铁氧体颗粒的平均粒径。
铁氧体烧结磁体的在20℃的矫顽力例如能够为4000Oe以上，能够超过4700Oe。铁氧体烧结磁体的在20℃的残留磁通密度能够为4000G以上，能够为4400G以上。铁氧体烧结磁体优选矫顽力(HcJ)和残留磁通密度(Br)双方优异。
铁氧体颗粒的在20℃的残留磁通密度Br能够为40emu/g以上，矫顽力HcJ能够为3000Oe以上。
铁氧体烧结磁体及铁氧体颗粒的HcJ的温度系数的绝对值可以为0.15[％/℃]以下，也可以为0.1[％/℃]以下。
在此，在将HcJ(20℃)设为在20℃的HcJ的实测值(单位Oe)、将HcJ(100℃)设为在100℃的HcJ的实测值(单位Oe)时，HcJ的温度系数β如下定义。
HcJ温度系数β(％/℃)＝[HcJ(100℃)－HcJ(20℃)]/80(℃)/HcJ(20℃)×100
(作用)
根据本实施方式的铁氧体烧结磁体及铁氧体颗粒，在规定的范围内含有金属元素R、金属元素A、Fe、Co、Zn、Si和B，因此，均能够提高在20℃的矫顽力及残留磁通密度双方。
作为其原因，认为通过利用Zn置换铁氧体的B位点，而提高Br。另外，认为通过添加金属元素R，HcJ及Br变高。还认为通过添加Si及/或Ca，组织致密化且密度提高。还认为通过添加B，HcJ提高。
另外，根据本实施方式的铁氧体烧结磁体及铁氧体颗粒，能够抑制HcJ的温度系数在较低地绝对值。特别是Zn的比例越小(例如z为0.1以下)，HcJ的温度系数趋于越小(例如，0.105％/℃以下)。
(粘结磁体)
接着，以下说明粘结磁体的实施方式。
本实施方式的粘结磁体含有上述的铁氧体颗粒和树脂。树脂的例子为：环氧树脂、酚醛树脂、具有多芳香族环的树脂、具有三嗪环的树脂(三嗪树脂)等热固化性树脂；苯乙烯系、烯烃系、聚氨酯系、聚酯系、尼龙等聚酰胺系的弹性体、离聚物、乙烯丙烯共聚物(EPM)、乙烯－丙烯酸乙酯共聚物等热塑性树脂。
从兼得优异的磁特性和优异的形状保持性的观点来看，粘结磁体中的树脂的含有率例如可以为0.5～10质量％，也可以为1～5质量％。粘结磁体中的树脂的含有率能够通过改变制造时所使用的含有树脂的溶液中的树脂浓度或成形体制作时的成形压力进行调整。从同样的观点来看，粘结磁体中的铁氧体颗粒的含有率例如可以为90～99.5质量％，也可以为95～99质量％。
粘结磁体的形状没有特别限定，能够设为与铁氧体烧结磁体一样。
本实施方式的铁氧体烧结磁体和粘结磁体能够作为电动机及发电机等旋转电气设备、扬声器·头戴式耳机用磁铁、磁控管、MRI用磁场产生装置，CD－ROM用钳位器、分配器用传感器、ABS用传感器、燃料·油位传感器、磁锁或隔离器等磁场产生部件使用。另外，也能够作为通过蒸镀法或溅射法等形成磁记录介质的磁性层时的靶材(粒料)使用。
(旋转电气设备)
接着，图2中表示本发明一个实施方式的电动机200。电动机200具备定子31和转子32。转子32具有轴36及转子铁芯37。本实施方式的电动机200中，在定子31上设置有作为永磁体的C字型的铁氧体烧结磁体或粘结磁体100，在转子32的转子铁芯37上设置有电磁体(线圈)。
此外，也可以是将铁氧体烧结磁体设置于转子，且将电磁体(线圈)设置于定子的电动机。电动机的形式没有特别限定。另外，旋转电气设备的另一例是具有转子及定子的发电机。铁氧体烧结磁体能够设置于转子或定子。
(铁氧体烧结磁体等的制造方法)
接着，对于铁氧体颗粒、铁氧体烧结磁体及粘结磁体的制造方法的一例进行说明。以下说明的制造方法包含配合工序、预烧工序、粉碎工序、成形工序及烧制工序。以下说明各工序的详情。
配合工序是制备预烧用的混合粉末的工序。预烧用的混合粉末能够含有铁氧体的构成元素、例如金属元素A、金属元素R、Fe、Co和Zn。在配合工序中，优选将含有各元素的粉末的混合物通过磨碎机或球磨机等混合1～20小时程度，同时进行粉碎处理，得到混合粉末。
B、Si等添加元素也可以预先包含于上述粉末中，但也可以在配合工序中进一步添加含有该添加元素的其它粉末，从而得到预烧用的混合粉末。其它粉末的例子是含有B的粉末和含有Si的粉末。
含有各元素的粉末的例子是各元素的单体、氧化物、氢氧化物、碳酸盐、硝酸盐、硅酸盐、有机金属化合物。一个粉末可以含有两种以上的金属元素，一个粉末也可以实际上仅含有一个金属元素。
含有Ca的粉末的例子为CaCO3和CaO。
含有Sr的粉末的例子为SrCO3和SrO。
含有R的粉末的例子为La2O3、La(OH)3。
含有Fe的粉末的例子为Fe2O3。
含有Co的粉末的例子为Co3O4。
含有Zn的粉末的例子为ZnO。
含有B的粉末的例子为B2O3。
含有Si的粉末的例子为SiO2。
原料粉末的平均粒径没有特别限定，例如为0.1～2.0μm。
优选配合工序之后，根据需要，使原料组成物干燥，通过筛子除去粗粒。
在预烧工序中，对配合工序中得到的原料组成物进行预烧。预烧优选在例如空气等氧化性气氛中进行。预烧的温度例如可以为1100～1400℃，也可以为1100～1300℃。预烧的时间例如可以为1分钟～10小时，也可以为1分钟～3小时。通过预烧得到的预烧粉(铁氧体颗粒)中的铁氧体相(M相)的比率例如可以为70质量％以上，也可以为75质量％以上。该铁氧体相的比率能够与铁氧体烧结磁体中的铁氧体相的比率同样地求得。
在粉碎工序中，对通过预烧工序成为颗粒状或块状的预烧粉进行粉碎。这样得到铁氧体颗粒。粉碎工序例如也可以分成以将预烧粉制成粗粉末的方式粉碎(粗粉碎工序)后，将其进一步进行微细地粉碎的(微粉碎工序)两个阶段的工序而进行。
粗粉碎能够使用例如振动磨机等进行至预烧粉的平均粒径成为0.1～5.0μm。
在微粉碎中，对粗粉碎中得到的粗粉进一步通过湿式磨碎机、球磨机、喷磨机等进行粉碎。在微粉碎中，以得到的微粉(铁氧体颗粒)的平均粒径成为例如0.08～2.0μm程度的方式进行粉碎。微粉的比表面积(例如通过BET法求得。)例如为7～12m2/g程度。适合的粉碎时间根据粉碎方法不同而各异，例如在湿式磨碎机的情况下，为30分钟～10小时，在球磨机进行的湿式粉碎中为10～50小时。铁氧体颗粒的比表面积能够使用市售的BET比表面积测定装置(Mountech制，商品名：HM Model－1210)测定。
在微粉碎工序中，为了提高在烧制后得到的烧结体的磁取向度，也可以添加例如以通式Cn(OH)nHn+2表示的多元醇。通式中的n例如可以为4～100，也可以为4～30。作为多元醇，例如可举出山梨醇。另外，也可以并用两种以上的多元醇。另外，也可以除了多元醇之外，还并用其它公知的分散剂。
在添加多元醇的情况下，其添加量相对于添加对象物(例如粗粉)例如可以为0.05～5.0质量％，也可以为0.1～3.0质量％。需要说明的是，微粉碎工序中添加的多元醇在后述的烧制工序中进行热分解而被除去。
此外，优选不将原料粉末的全部在配合工序中混合，在粗粉碎工序及/或微粉碎工序中，添加一部分原料粉末、例如CaCO3粉末的一部分及SiO2粉末的一部分或全部。通过在预烧后添加含有这种成分的粉末，能够提高烧制工序中的烧结性及提高磁特性。此外，这些副成分有时在通过湿式进行成形的情况下有时会与浆料的溶剂一起流出，因此，能够配合比铁氧体烧结磁体100中的目标的含量稍多的量。
例如，在预烧后添加含有Ca的粉末的一部分的情况下，就Ca的添加量而言，将Ca换算成CaCO3，相对于铁氧体磁体整体可以为0.01质量％以上，也可以为1.60质量％以下。
在成形工序中，将粉碎工序中得到的铁氧体颗粒在磁场中成形，而得到成形体。成形也能够通过干式成形及湿式成形的任一方法进行。从提高磁取向度的观点来看，优选通过湿式成形进行。
在通过湿式成形进行成形的情况下，例如通过湿式进行上述的微粉碎工序，由此得到浆料后，将该浆料浓缩成规定的浓度，得到湿式成形用浆料。能够使用该湿式成形用浆料进行成形。浆料的浓缩能够通过离心分离或压滤机等进行。湿式成形用浆料中的铁氧体颗粒的含量例如为30～80质量％。浆料中，作为分散铁氧体颗粒的分散介质，例如可举出水。浆料中，也可以添加葡萄糖酸、葡萄糖酸盐、山梨醇等表面活性剂。作为分散介质，也可以使用非水系溶剂。作为非水系溶剂，能够使用甲苯及二甲苯等有机溶剂。在该情况下，也可以添加油酸等表面活性剂。此外，湿式成形用浆料也可以通过向微粉碎后的干燥状态的铁氧体颗粒中添加分散介质等而制备。
在湿式成形中，接着，相对于该湿式成形用浆料进行磁场中成形。在该情况下，成形压力例如为9.8～196MPa(0.1～2.0ton/cm2)。施加的磁场例如为398～1194kA/m(5～15kOe)。
在烧制(正式烧制)工序中，对成形工序中得到的成形体进行烧制，得到铁氧体烧结磁体。成形体的烧制能够在大气中等氧化性气氛中进行。烧制温度例如可以为1050～1270℃，也可以为1080～1240℃。另外，烧制时间(保持在烧制温度的时间)例如为0.5～3小时。
在烧制工序中，在到达至烧结温度之前，例如也可以从室温以0.5℃/分钟左右的升温速度加热至100℃左右。由此，能够在进行烧结之前，充分干燥成形体。另外，能够充分除去成形工序中添加的表面活性剂。此外，这些处理可以在烧制工序开始时进行，也可以在烧制工序之前额外进行。
这样，能够制造铁氧体烧结磁体。在制造粘结磁体而非制造铁氧体烧结磁体的情况下，使上述的成形工序中得到的成形体含浸树脂，进行加热而将树脂固化，由此，能够得到粘结磁体。具体而言，将成形体浸渍于预先制备的含有树脂的溶液中，通过在密闭容器中减压脱泡，使含有树脂的溶液浸透于成形体的空隙内。然后，从含有树脂的溶液中取出成形体，除去附着于成形体的表面的剩余的含有树脂的溶液。为了除去剩余的含有树脂的溶液，只要使用离心分离机等即可。
在浸渍于含有树脂的溶液之前，通过将成形体放入密闭溶液中并保持成减压气氛，且浸渍于甲苯等溶剂中，可促进脱泡，增加树脂的含浸量，能够减少成形体中的空隙。
铁氧体颗粒、铁氧体烧结磁体及粘结磁体的制造方法不限定于上述的例子。例如，在制造粘结磁体的情况下，进行至上述的粉碎工序后，将得到的铁氧体颗粒和树脂混合，将其在磁场中成形，也可以得到含有铁氧体颗粒和树脂的粘结磁体。
另外，例如，成形工序及烧制工序也可以通过以下的顺序进行。即，成形工序也可以通过CIM(Ceramic Injection Molding(陶瓷注塑成形)成形法、或PIM(PowderInjection Molding，粉末注塑成形的一种)进行。CIM成形法中，首先，将干燥的铁氧体颗粒与粘合剂树脂一起加热混炼，而形成粒料。将该粒料在施加了磁场的模具内进行注塑成形，得到预备成形体。通过对该预备成形体进行脱粘合剂处理，而得到成形体。接着，在烧制工序中，将进行了脱粘合剂处理的成形体在例如大气中，优选以1100～1250℃、更优选以1160～1230℃的温度烧结0.2～3小时程度，而能够得到铁氧体烧结磁体。
实施例
参照实施例及比较例更详细地说明本发明的内容，但本发明不限定于以下的实施例。
[铁氧体烧结磁体的制造]
(实施例1～37及比较例1～17)
作为原材料，准备了碳酸钙(CaCO3)、碳酸钡(BaCO3)、碳酸锶(SrCO3)、氢氧化镧(La(OH)3)、氧化铁(Fe2O3)、氧化钴(Co3O4)、氧化锌(ZnO)的粉末。将这些原材料粉末以原子比成为表1～3所示的方式进行配合。但是，如后述，碳酸钙的一部分在粉碎工序时添加，因此，对该部分预先进行了扣除。相对于这样得到的配合物，以铁氧体烧结磁体中的量成为表1～表2的量的方式添加规定量的氧化硼(B2O3)，使用湿式磨碎机及球磨机进行混合及粉碎，得到浆料(配合工序)。在各实施例及比较例中，以得到具有相互不同的组成的铁氧体烧结磁体的方式，如表1～表2所示变更各原材料的配合比。
对该浆料进行干燥，除去粗粒后，在大气中以1280℃进行预烧，得到预烧粉(预烧工序)。利用小型棒振动磨机对得到的预烧粉进行粗粉碎，得到粗粉。相对于该粗粉，添加相对于铁氧体烧结磁体的质量成为0.3质量％的量的氧化硅(SiO2)粉末、成为0.7质量％的量的碳酸钙(CaCO3)粉末和1质量％的山梨糖醇。然后，使用湿式球磨机开心微粉碎，得到含有铁氧体颗粒的浆料(粉碎工序)。
对在微粉碎后得到的浆料的水分量进行调节，得到湿式成形用浆料。使用湿式磁场成型机将该湿式成形用浆料在796kA/m(10kOe)的施加磁场中进行成形，得到具有直径30mm×厚度15mm的圆柱状的成形体(成形工序)。将得到的成形体在大气中以室温进行干燥，接着，在大气中以1170℃进行烧制(烧制(正式烧制)工序)。这样得到圆柱状的铁氧体烧结磁体。
(实施例38、39)
除了以成为表3那样的方式配合组成，然后将烧制(正式烧制)温度设为1150℃以外，与实施例1同样地进行。
[铁氧体烧结磁体的评价1]
＜磁特性的评价＞
对铁氧体烧结磁体的上下表面进行加工后，使用最大施加磁场29kOe的B－H示踪器，分别测定在20℃的Br及HcJ。另外，对于一部分铁氧体烧结磁体，使用振动试样型磁力计测定在100℃的HcJ，求得HcJ的温度系数β。
＜组成分析＞
通过以下的顺序测定铁氧体烧结磁体中的B(硼)及Si(硅)的含量。将铁氧体烧结磁体的试样0.1g与过氧化钠1g及碳酸钠1g混合并加热，将其熔解。将熔解物溶解于纯净水40ml及盐酸10ml的溶液中后，添加纯净水，制成100ml的溶液。使用该溶液，通过ICP发射光谱分析(ICP－AES)求得硼的换算成B2O3的含量和硅的换算成SiO2的含量。ICP发射光谱分析中，使用岛津制作所制的分析装置(装置名：ICPS 8100CL)，在测定时进行了基体匹配。
铁氧体中的r、x、y和z通过荧光X射线分析进行测定。
将这些结果在表1～表3中表示。
[表1]
[表2]
[表3]
如表1～3所示，在满足(2)～(5)式，且Si及B的含量为规定范围的铁氧体磁体中，在20℃的Br及HcJ优异。另外，特别是在Zn少的情况下(例如z为0.1以下)，均将HcJ的温度系数β的绝对值抑制为较低(例如，0.105％/℃以下)。
另外，对比较例10、实施例11、24、28的铁氧体烧结磁体进行粉碎，制成平均粒径为10μm程度的粒子，与上述一样，使用振动试样型磁力计测定在20℃的Br及HcJ和在100℃的HcJ，求得HcJ的温度系数β。将结果在表4中表示。即使在粒子的状态下，在20℃的Br及HcJ也优异，另外，在Zn少的情况下，将HcJ的温度系数β的绝对值抑制得特别低。
[表4]
符号说明
4…铁氧体相(主相)，6…晶界相，31…定子(定子罩)，32…转子，36…轴，37…转子铁芯，100…铁氧体烧结磁体或粘结磁体，200…电动机。
Claims (9)
1.一种铁氧体烧结磁体，其含有具有磁铅石型的结晶结构的铁氧体相，其特征在于，
至少含有金属元素A、金属元素R、Fe、Co、Zn和B，
金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca，
金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La，
以(1)式表示金属元素的原子比率时，
r、x、y和z满足下述(2)～(5)式，
A1－rRrFexCoyZnz (1)，
0.40≤r≤0.70 (2)，
8.20≤x≤9.34 (3)，
0.05＜y≤0.50 (4)，
0＜z≤0.20 (5)，
Si的含量以SiO2换算计为0～0.60质量％，
B的含量以B2O3换算计为0.01～0.70质量％。
2.根据权利要求1所述的铁氧体烧结磁体，其特征在于，
Si的含量以SiO2换算计为0.01～0.40质量％，B的含量以B2O3换算计为0.20～0.70质量％。
3.根据权利要求1或2所述的铁氧体烧结磁体，其特征在于，
Ca占据金属元素A的95原子％以上。
4.一种旋转电气设备，其特征在于，具备权利要求1～3中任一项所述的铁氧体烧结磁体。
5.一种铁氧体颗粒，其是含有具有磁铅石型的结晶结构的铁氧体相的铁氧体颗粒，其特征在于，
至少含有金属元素A、金属元素R、Fe、Co、Zn和B，
金属元素A是选自Sr、Ba、Ca和Pb中的至少一种元素，必须含有Ca，
金属元素R是选自含有Y的稀土元素及Bi中的至少一种元素，必须含有La，
以(1)式表示金属元素的原子比率时，
r、x、y和z满足下述(2)～(5)式，
A1－rRrFexCoyZnz (1)，
0.40≤r≤0.70 (2)，
8.20≤x≤9.34 (3)，
0.05＜y≤0.50 (4)，
0＜z≤0.20 (5)，
Si的含量以SiO2换算计为0～0.60质量％，
B的含量以B2O3换算计为0.01～0.70质量％。
6.根据权利要求5所述的铁氧体颗粒，其特征在于，
Si的含量以SiO2换算计为0.01～0.40质量％，B的含量以B2O3换算计为0.20～0.70质量％。
7.根据权利要求5或6所述的铁氧体颗粒，其特征在于，
Ca占据金属元素A的95原子％以上。
8.一种粘结磁体，其特征在于，其含有权利要求5～7中任一项所述的铁氧体颗粒。
9.一种旋转电气设备，其特征在于，其具备权利要求8所述的粘结磁体。
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