CN103548101A - 磁铅石型铁氧体磁性材料以及由其得到的分段式永磁体 - Google Patents
磁铅石型铁氧体磁性材料以及由其得到的分段式永磁体 Download PDFInfo
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- CN103548101A CN103548101A CN201280024984.6A CN201280024984A CN103548101A CN 103548101 A CN103548101 A CN 103548101A CN 201280024984 A CN201280024984 A CN 201280024984A CN 103548101 A CN103548101 A CN 103548101A
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- magnetic material
- ferrite
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- permanent magnet
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 49
- 239000000696 magnetic material Substances 0.000 title claims abstract description 28
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- 238000011156 evaluation Methods 0.000 claims description 3
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- 238000012545 processing Methods 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
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- 238000004519 manufacturing process Methods 0.000 abstract description 5
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- 235000012054 meals Nutrition 0.000 description 9
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
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- 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
- 230000005415 magnetization Effects 0.000 description 2
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000306 component Substances 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- CMGJQFHWVMDJKK-UHFFFAOYSA-N lanthanum;trihydrate Chemical compound O.O.O.[La] CMGJQFHWVMDJKK-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
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- 150000002894 organic compounds Chemical class 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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Abstract
一种包含磁铅石型六方晶系铁氧体主相的铁氧体磁性材料,所述主相具有由式(I)表示的组成,可以提供在残留磁通量密度(Br)、内禀矫顽力(iHc)、矩形比(Hk/iHc)和最大能量积(B.Hmax)方面的改进的磁特性。因此,由其得到的分段式永磁体可以用于制造汽车的小型电动机、电气设备和家用电器的电动机,以及其他设备。
Description
技术领域
本发明涉及具有改进的磁特性的磁铅石(Magnetoplumbite)型(六方晶系)铁氧体磁性材料,以及由其得到的分段式(segment-type)永磁体,所述分段式永磁体用于制造汽车的小型电动机、电气设备和家用电器的电动机,以及其他设备。
背景技术
将具有磁铅石型(M型)晶体结构的烧结铁氧体磁体用作汽车的小型电动机和电气设备/家用电器的电动机的核心组件的永磁体。
常规的M型Sr基或Ba基烧结铁氧体磁体一般通过以下步骤来制备;首先,使铁的氧化物与Sr或Ba的碳酸盐混合,并通过煅烧使混合物进行反应以形成SrO·nFe2O3或BaO·nFe2O3。将所得的经煅烧的材料粉碎以获得粗粉末。将粗粉末与烧结助剂如SiO2、SrCO3和CaCO3混合,然后湿法粉碎以获得具有均匀颗粒尺寸的细粉末的浆料。为了提高最终产品的磁特性如内禀矫顽力(iHc),将Cr2O3或Al2O3与烧结助剂一起添加到细粉末浆料中。将所得细粉末浆料使用压制装置在磁场下模塑、干燥、烧结和加工以制备具有期望形状的磁体。
近来,汽车、电气设备和家用电器需要改进的性能特性和更高效率。为了满足这些需求,近来已经进行了许多研究以开发在残留磁通量密度(Br)、内禀矫顽力(iHc)、矩形比(Hk/iHc)和最大能量积(B.Hmax)方面具有改进磁特性的永磁体。
例如,欧洲专利特许公开第0905718号公开了包含由A1-xRxFe12-yMyO19表示的含有A、R、Fe和M的六方晶系铁氧体主相的烧结磁体,其中A为选自锶、钡、钙和铅中的至少一种元素,A中实质上含有锶;R为选自包括镧和钇的稀土元素以及铋中的至少一种元素,R中实质上含有镧;M为钴或者钴和锌的混合物(M中钴的比例为至少10原子%);并且相对于金属元素的总量,A、R、Fe和M元素的比例分别为3原子%至9原子%、0.5原子%至4.0原子%、86原子%至93原子%和0.5原子%至3.0原子%。
欧洲专利第0940823B1号(对应于日本专利第3,181,559号和USPNo.6,402,980)公开了包含由Ca1-xRx(Fe12-yMy)zO19表示的含Ca、R、Fe和M的六方晶系铁氧体主相的烧结磁体,其中M为选自Co、Ni和Zn中的至少一种元素,M中实质上含有Co(M中钴的比例为至少10原子%);R为选自包括La、Y的稀土元素和Bi中的至少一种元素,R中实质上含有La;并且相对于金属元素的总量,Ca、R、Fe和M元素的比例分别为1原子%至13原子%、0.05原子%至10原子%、80原子%至95原子%和1.0原子%至7.0原子%。
US专利第6,139,766号公开了具有A1-xRx(Fe12-yMy)zO19组成的烧结铁氧体磁体,其中A为选自Sr、Ba和Pb中的至少一种元素,A中实质上含有Sr;R为选自包括La和Y的稀土元素中的至少一种元素,R中实质上含有La;M为钴或者钴和锌的混合物;并且x、y和z分别满足0.04≤x≤0.9、0.04≤y≤0.5和0.7≤z≤1.2的条件。
韩国专利第10-0839206号公开了包含六方晶系铁氧体主相的磁性材料,所述主相由LaxCamα1-x-y(Fe12-yCoy)z表示,α为Ba、Sr或它们的混合物,其中构成主相的金属元素的构成比满足以下条件:在由下列点约束的区域内,A:(0.53,0.27)、B:(0.64,0.27)、C:(0.64,0.35)、D:(0.53,0.45)、E:(0.47,0.45)和F:(0.47,0.32),在(x,m)坐标中,1.3≤x/yz≤1.8、9.5≤12z≤11.0并且(1-x-m)/(1-x)≤0.42。
然而,这类传统铁氧体磁性材料仍然显示出不理想的磁特性。因此,继续努力开发具有改进磁特性的磁性材料以满足目前的需求,即用于汽车的电动机和用于电气设备以及用于家用电器的电动机的高性能、高效率、小型化和重量减轻。
发明内容
因此,本发明的一个主要目的是提供一种铁氧体磁性材料以及由其得到的分段式永磁体,所述铁氧体磁性材料可提供在残留磁通量密度(Br)、内禀矫顽力(iHc)、矩形比(Hk/iHc)和最大能量积(B.Hmax)方面改进的磁特性。
根据本发明的一方面,提供了包含磁铅石型六方晶系铁氧体主相的铁氧体磁性材料,所述主相具有由式(I)表示的组成:
Ca(1-x-y-z)SrxBayAzFe(2n-m1-m2)Mm1M’m2O19 (I)
其中,
A为选自包括La、Nd、Pr和Sm的稀土元素以及Bi中的至少一种元素,A中实质上含有La;
M为选自Co、Mn、Ni和Zn中的至少一种元素,M中实质上含有Co;
M’为Cr或者为Cr和Al的混合物;
0.02≤x≤0.3;
0.01≤y≤0.09;
0.1≤z≤0.5;
0.1≤m1≤0.6;
0.01<m2≤0.07;以及
9.02≤n≤11.0。
根据本发明的另一方面,提供了通过烧结铁氧体磁性材料获得的烧结铁氧体磁体;由铁氧体磁性材料得到的分段式永磁体;以及包含分段式永磁体的产品。
附图说明
本发明的上述及其它的目的和特征将由结合以下附图给出的本发明的以下描述变得明显,所述附图分别示出:
图1至图4:分别是在实施例1和比较例1至3中制备的相应烧结磁体(烧结温度1190℃)的磁特性,Br(G)、iHc(Oe)、Hk/iHc(%)和SFC(综合评价指数,synthetic evaluationindex,{Br+(1/3)iHc}×(Hk/iHc));
图5至图8:分别是作为实施例1中制备的烧结磁体烧结温度的函数的磁特性,Br(G)、iHc(Oe)、Hk/iHc(%)和SFC的变化;
图9和图10:分别是实施例2和比较例4中制备的分段式永磁体的磁特性,ΦR–ΦRG和HGF(80);
图11和图12:分别是用于制造实施例2和比较例4中的分段式(33.4R×21.9W×6.16T×45L)铁氧体永磁体的模塑的右视图/三维视图和前视图/横截面视图;
图13至16:分别是用于制造实施例2和比较例4中的分段式(33.4R×21.9W×6.16T×45L)铁氧体永磁体的模塑的下冲头结构、模具结构、上冲头结构和装配图;以及
图17至19:分别是作为实施例3至实施例21和比较例5至比较例15中制备的烧结磁体的Ba/(Sr+Ba)(即y/x+y的值)、Ba+Cr(即y+m2的值)和Cr(即m2的值)函数的SFC的变化。
具体实施方式
本发明的铁氧体磁性材料(经煅烧材料)的特征在于,包含磁铅石型六方晶系铁氧体主相,其中构成主相的元素具有由式(I)表示的组成。
一般而言,当Fe(氧化物铁氧体磁性材料的基本元素)的含量变得更大时,生成了不希望的非磁性相(如α–Fe2O3),降低磁特性。与此相反,当Fe的含量变得更小时,对应于具有磁矩的Fe离子位点的A位点变得过多,导致不希望的非磁性颗粒组分的增加,从而明显降低磁特性。烧结M型铁氧体氧化物磁体的磁特性基于Fe离子的磁矩,其具有以反向平行方向排列的铁氧体磁性材料的磁性结构。为了提高磁特性如饱和磁化强度和磁各向异性系数,使得在具有以反向平行方向定向的磁距的位点中的Fe离子可以被具有更小磁矩或无磁性的其它元素所取代;在对应于以平行方向定向的磁矩的位点中的Fe离子可以被具有更大磁矩的其它元素所取代;Fe离子可以被具有更大晶格和更强相互作用的其它元素所取代。
相对于本发明铁氧体磁性材料的构成元素的组成,对应于A含量的值z为0.1至0.5,优选0.35至0.5。当A含量低时(即小于0.1),为提高磁特性的A的充分替代变得困难;而当A含量高时(即大于0.5),未反应的A氧化物的量增加,导致差的磁特性。
M(如Co)取代部分Fe,作用是提高M型氧化物氧体磁性材料的饱和磁性强度和结晶磁各向异性系数。M含量的值m1是0.1至0.6,优选0.2至0.4。当M含量少于0.1时,其对Fe的替代率降低,使得难以提高磁特性。当M含量高于0.6时,A位点元素的离子价被破坏,导致不希望的杂质相(foreign phase)的形成,导致磁特性的急剧退化。
M’(如Cr)取代部分Fe,其抑制颗粒的生长并增加临界颗粒半径,导致磁各向异性系数的增加,以及最终M型氧化物铁氧体磁性材料的iHc的增加。
优选地,x、y、z、m1和m2的值满足以下条件:0.1≤x+y<0.3,0.03≤y+m2≤0.16,0.09≤y/(x+y)≤0.5,0.3≤(x+y)/(m1+m2)≤0.8和1.2≤(1-z)/(m1+m2)≤2.0,其中式(1-z)/(m1+m2)表示(Sr+Ba+Ca)/(M+M’)的原子含量比并且其可以更优选地落入1.4至1.6的范围内。
在式(I)中,原子含量比(Fe+M+M’)/(Ca+A+Sr+Ba)对应于2n。
在下文中,对作为本发明的实施方案的铁氧体磁性材料和烧结磁体的示例性制备方法进行详细说明。
<混合过程>
首先,根据由期望的组成计算的重量百分数值称重起始原料,通常将它们使用湿式球磨机或湿式超微磨碎机湿法混合1小时至24小时以达到均匀混合。
可使用SrCO3、BaCO3、CaCO3、La2O3、Fe2O3、Cr2O3、Co3O4、Pr6O11、Nd2O3、Sm2O3等作为起始原料,其优选的平均粒径可落入0.2μm至1.0μm的范围内。
如果需要,还可以在混合过程中添加SiO2、H3BO3等以在随后的煅烧过程中促进形成铁氧体的反应以及颗粒的均匀生长。
<煅烧过程>
在煅烧过程中,起始原料的混合物进行固相铁氧体反应以形成具有磁铅石型晶体结构的经煅烧材料。煅烧通常可在氧化气氛(例如空气)中在1080℃至1350℃下进行,优选持续1小时至5小时。经煅烧的材料的粒径优选为0.3μm至2μm。
<粗粉碎过程>
所得经煅烧的材料是渣块或颗粒的形式,因此需要粗粉碎。粗粉碎可以使用干式振动磨机或干式球磨机,优选干式振动磨机进行。粗粉碎后的粗粉末的平均粒径优选为2μm至4μm。
<热处理过程>
由于在前述粉碎过程中施加的物理应力,所得的粗粉末具有缺陷如不一致性、畸变和裂纹。这样的缺陷可以通过在900℃至1000℃的温度下热处理粗粉末而除去。
<细粉碎过程>
当使平均粒径为1.0μm或以上的粉末经历烧结过程时,由于颗粒生长,粗晶粒的比例变高,导致iHc急剧下降。因此,使经热处理的粉末经历细粉碎以获得平均颗粒直径为0.3μm至0.8μm的细粉末。细粉碎可使用湿式球磨机或湿式超微磨碎机进行。在使用湿式球磨机的情况下,粉碎时间可以控制在5小时至40小时内,而在使用湿式超微磨碎机的情况下,根据预定的期望平均颗粒直径可控制在2小时至20小时内。
为了在随后烧结过程中控制颗粒的生长及其直径,可以在细粉碎过程中加入添加剂(如SiO2、CaO或它们的混合物)。此外,可以加入La2O3、SrO、CaO、Cr2O3、Al2O3、CoO或它们的混合物以促进替代效应和在随后的烧结过程中控制颗粒生长。当所使用的添加剂的量过少或过多时,产生不希望的效果。因此,按100重量份的经粉碎粉末计,可使用的每种添加剂的量为0.1重量份至0.6重量份。
在细粉碎过程中还可以添加分散剂,以提高在磁场中进行的随后的压制过程中的取向效果并通过降低其粘度改善浆料的流动性。可以使用水性或非水性分散剂,但是考虑到环境方面,优选使用水性分散剂。适合于用作水性分散剂的为含有羟基和羧基基团的有机化合物、山梨糖醇、葡萄糖酸钙等。按100重量份的粗粉末计,分散剂的用量优选为0.05重量份至1.0重量份。
<压制过程>
压制过程可以通过湿式或干式方法进行,其中每种方法可以以或各向同性或各向异性排列沉积。为了实现高的磁特性,优选湿法各向异性压制。在该过程中,使细粉碎之后的浆料在所施加磁场中压力下压制然后由此获得用于各向异性烧结磁体的生坯。
在湿式各向异性压制的一个实施方案中,使细粉碎后的浆料经历脱水和浓缩,然后在固定浓度在10kOe至20kOe的磁场中300kgf/cm2至500kgf/cm2压力下压制。可以通过使用离心分离器或压滤机进行脱水和浓缩。
优选地,在随后烧结过程之前,为了防止裂纹的产生,可使由此形成的含有残余水量为10%至15%的生坯体干燥。如果含残余水的生坯经过烧结过程,当温度升高时在脱水过程中可以出现裂纹。因此,优选在室温或低温(即,50℃-100℃)下大气中干燥生坯。
<烧结过程>
通过在氧化气氛中连续干燥和烧结所得生坯获得烧结铁氧体磁体。为了消除在保留在生坯中的残余水和分散剂,在50℃至300℃下进行脱水和脱脂。
可以通过调节烧结条件(例如烧结时间、加热速率、最高温度、在预定温度下停留时间等)优化烧结铁氧体磁体的磁特性。换句话说,烧结条件(烧结时间、加热速率、最高温度、停留时间)的调节可以影响取代元素的浓度、晶粒生长、粒径、烧结磁体的密度,从而决定烧结铁氧体磁体的磁特性,即Br、bHc、iHc、B.Hmax、矩形比等。
在优选实施方案中,烧结可以通过在空气中以如下方式处理铁氧体基体进行:温度从25℃至500℃处理1小时,从500℃至1000℃处理5小时,从1000℃至Tmax(1180℃至1210℃)处理3小时,在Tmax(1180℃至1210℃)下1-2小时,从Tmax(1180℃至1210℃)至1000℃处理2小时,和从1000℃至室温处理5小时。
根据本发明的磁铅石型烧结铁氧体磁体具有优异的磁特性,包括:4550G或更高的残留磁通量密度(Br),4700Oe或更高的内禀矫顽力(iHc),92%或更高的矩形比(Hk/iHc),以及5800或更高的综合评价指数(SFC={Br+(1/3)iHc}×(Hk/iHc))。
此外,由本发明磁铅石型铁氧体磁性材料得到的并表现出具有33.4R的外半径、21.9W的宽度、6.16T的厚度和45L的长度的分段式永磁体,当使用磁特性测试系统Robograph2(ECKEL)测试时,表现出为ΦR≥0.330(mVs)、ΦRG≥0.320(mVs)和HGF(80)≥310(kA/m)的良好的磁特性。如结果中所示,本发明的烧结铁氧体磁体可以满足所需特征如高性能、高效率、小型化和重量减轻,因此,其可以用在用于汽车的小型电动机、用于电气设备以及用于家用电器和其他设备的电动机的制造上。
在下文中,通过以下实施例更具体的描述本发明,但是提供这些仅用于说明目的,并且本发明并不限于此。
实施例1
使用碳酸锶(SrCO3)、碳酸钡(BaCO3)、碳酸钙(CaCO3)、氧化镧(La2O3)、氢氧化镧(La(OH)3)、氧化铁(Fe2O3)、氧化铬(Cr2O3)和氧化钴(CoO)作为起始原料。将这些原料根据表2中所示的组成称重,并共混以获得表3中所示的Ca(1-x-y-z)SrxBayLazFe(2n-m1-m2)Com1Crm2O19的烧结铁氧体磁体。在共混之前,将所有的原料预先粉碎并碎裂至粒径为0.6μm至1.0μm。
将混合物稀释至浓度为40%,并湿润并循环搅拌20小时。然后,将所得混合物按顺序在200℃干燥24小时并在1120℃煅烧2小时。将所得煅烧材料使用干式振动磨机磨碎以获得平均直径为3μm的粗粉末。将粗粉末在1000℃加热处理2小时并放入含水的湿式超微磨碎机中以得到43%的浓度。按100重量份的粗粉末计,将La2O3(0.5重量份)、CaO(0.45重量份)、SiO2(0.4重量份)和分散剂葡萄糖酸钙(0.3重量份)加入到其中,并粉碎8小时以得到平均粒径为0.65μm的浆料。
将由此制备的浆料置于直径为40mm和高度为10mm的圆筒形的模塑中,使其经历在15kOe磁场中0.4Ton/cm2的成型压力下压制以形成生坯。
使由此形成的生坯在200℃下干燥10小时,根据表1中规定的条件在空气中烧结,然后将烧结产物加工成直径为35mm并且厚度为10mm。烧结的最高温度(Tmax)分别设置为1180℃、1190℃、1200℃、1210℃和1220℃。
[表1]
根据Tmax值使用B-H曲线示踪测量所制备的M型烧结铁氧体磁体的磁特性及其结果示于表4a至4e。烧结磁体的组成记录于表3中。
比较例1至3
重复上述实施例1的步骤以制备M型烧结铁氧体磁体,不同在于原料为根据表2中描述的组成称重而不使用碳酸钡(BaCO3)和氧化铬(Cr2O3),以满足表3中所规定的最终组成。
根据Tmax值的烧结磁体的组成和磁特性的结果分别示于表3和表4a至4e中。
在实施例1、和比较例1至3中制备的相应烧结磁体(烧结温度1190℃)的磁特性,Br、iHc、Hk/iHc和SFC的结果分别示于图1至4中。此外,作为在实施例1中制备的烧结磁体的烧结温度的函数,磁特性,Br、iHc、Hk/iHc和SFC的变化分别示于图5至8中。
[表2]Ca(1-x–y-z)SrxRyAzFe(2n-m1-m2)Mm1M’m2O19(混合组成)
[表3]Ca(1-x–y-z)SrxRyAzFe(2n-m1-m2)Mm1M’m2O19(烧结磁体组成)
[表4a]烧结磁体(1180℃)的磁特性
[表4b]烧结磁体(1190℃)的磁特性
[表4c]烧结磁体(1200℃)的磁特性
[表4d]烧结磁体(1210℃)的磁特性
[表4e]烧结磁体(1220℃)的磁特性
如表4a至4e和图1至4所示,实施例1中制备的烧结磁体相较于比较例1至3中制备的那些在所有最高烧结温度下表现出显著改善的包括Br、iHc、和SFC的磁特性。特别是,图5至8示出了在最高温度1190℃烧结的实施例1的烧结磁体具有5927的SFC,这表明其为最佳条件。此外,确认在最高烧结温度1210℃的Hk/iHc示出了95.5%的最高水平,并且在最高烧结温度1180℃至1210℃,SFC={Br+(1/3)iHc}×(Hk/iHc)的值为5904至5934。
同时,Br的值随烧结温度的增加而增加,而iHc的值逐渐减小并在最高烧结温度1220℃迅速下降。据预计,这种现象的发生是因为由于最高烧结温度的上升导致的颗粒的过度生长。
实施例2
重复上述实施例1的步骤以制备分段式铁氧体永磁体33.4R×21.9W×6.16T×45L,不同在于使用分段式模塑(33.4R(外半径)×21.9W(宽度)×6.16T(厚度)×45L(长度))替代圆筒形模塑(直径40mm×高度10mm);最高烧结温度设置为1180℃;以及使所得到的烧结产品通过使用分段式研磨机加工。
使用磁特性测试系统Robograph2(ECKEL)测量由此制备的分段式永磁体的磁特性,并且ΦR、ΦRG和HGF(80)的磁特性结果示于表5中,其中“ΦRG”值为至少0.94×ΦRmin(测试系统设置为ΦRmin≤ΦR≤ΦRmax),其用于评价磁滞回线的矩形比。此外,“HGF(80)”表示80%的ΦR与第二象限去磁曲线相交处的值,其用于评价磁滞回线的矩形比和iHc。
[表5]
如表5中所示,实施例2中制备的永磁体满足ΦR≥0.333(mVs)、ΦRG≥0.320(mVs)并且HGF(80)≥339(kA/m)的条件。
比较例4
重复上述比较例2的步骤以制备分段式永磁体33.4R×21.9W×6.16T×45L,不同在于使用Sr(1-x-y)CaxLayFe(2n-z)CozO19(n=5.85,x=0,y=0.25,z=0.2)作为所述煅烧过的材料的组成。
由此制备的具有样品尺寸的永磁体的磁特性示于表6。
此外,实施例2和比较例4中制备的分段式永磁体的磁特性ΦR-ΦRG和HGF(80)分别示于图9和10。
[表6]
如表5-6和图9-10所示,实施例2中制备的永磁体的ΦR、ΦRG和HGF(80)分别比比较例4中制备的永磁体的ΦR、ΦRG和HGF(80)高11.7%、10.7%和8.2%。
实施例3至21和比较例5至15
重复上述实施例1的步骤以制备M型烧结铁氧体磁体,不同在于所述原料为根据表7中描述的组成称重并使用CaCO3(0.8重量份)替换CaO(0.45重量份)作为细粉碎助剂以满足表8中所规定的最终组成,以及最高烧结温度设置为1180℃。
由此制备的烧结磁体的组合和磁特性分别记录于表8和9中。
此外,将作为实施例3至21和比较例5至15中制备的烧结磁体的Ba/(Sr+Ba)(即y/x+y的值)、Ba+Cr(即y+m2的值)和Cr(即m2的值)的函数的SFC的变化进行分别测量并记录于图17至19中。
[表7]Ca(1-x–y-z)SrxRyAzFe(2n-m1-m2)Mm1M’m2O19(混合组成)
[表8]Ca(1-x–y-z)SrxRyAzFe(2n-m1-m2)Mm1M’m2O19(烧结磁体组成)
如表9和图17至19所示,实施例3至21中制备的烧结磁体与比较例5至15中制备的那些相比表现出显著改善的磁特性。
[表9]
虽然已对本发明的实施方案进行了描述和说明,但是明显在不脱离本发明精神下可以进行各种变化和改进,其不应仅限于所附权利要求的范围。
Claims (12)
1.一种包含磁铅石型六方晶系铁氧体主相的铁氧体磁性材料,所述主相具有由式(I)表示的组成:
Ca(1-x-y-z)SrxBayAzFe(2n-m1-m2)Mm1M’m2O19 (I)
其中,
A为选自包括La、Nd、Pr和Sm的稀土元素以及Bi中的至少一种元素,A中实质上含有La;
M为选自Co、Mn、Ni和Zn中的至少一种元素,M中实质上含有Co;
M’为Cr或者为Cr和Al的混合物;
0.02≤x≤0.3;
0.01≤y≤0.09;
0.1≤z≤0.5;
0.1≤m1≤0.6;
0.01<m2≤0.07;以及
9.02≤n≤11.0。
2.根据权利要求1所述的铁氧体磁性材料,其中所述z为0.35至0.5。
3.根据权利要求1所述的铁氧体磁性材料,其中所述m1为0.2至0.4。
4.根据权利要求1所述的铁氧体磁性材料,其中所述x、y和m2的值满足0.1≤x+y<0.3,和0.03≤y+m2≤0.16的条件。
5.根据权利要求1所述的铁氧体磁性材料,其中所述x、y、z、m1和m2的值满足0.09≤y/(x+y)≤0.5、0.3≤(x+y)/(m1+m2)≤0.8并且1.2≤(1-z)/(m1+m2)≤2.0的条件。
6.根据权利要求5所述的铁氧体磁性材料,其中(1-z)/(m1+m2)的值为1.4至1.6。
7.一种通过烧结根据权利要求1至6中任一项所述的铁氧体磁性材料获得的烧结铁氧体磁体。
8.根据权利要求7所述的烧结铁氧体磁体,其中所述铁氧体的所述烧结是通过以如下方式处理所述铁氧体基体进行的:温度从25℃至500℃处理1小时,从500℃至1000℃处理5小时,从1000℃至最高温度处理3小时,在最高温度下1-2小时,从最高温度至1000℃处理2小时,和从1000℃至室温处理5小时,所述最高温度为1180℃至1210℃。
9.根据权利要求7所述的烧结铁氧体磁体,其具有4550G或更高的残留磁通量密度(Br),4700Oe或更高的内禀矫顽力(iHc),92%或更高的矩形比(Hk/iHc),和5800或更高的综合评价指数(SFC={Br+(1/3)iHc}×(Hk/iHc))。
10.一种由根据权利要求1至6中任一项所述的铁氧体磁性材料得到的分段式永磁体。
11.根据权利要求10所述的分段式永磁体,其满足用磁特性测试系统Robograph2(ECKEL)测试时,ΦR≥0.333(mVs)、ΦRG≥0.320(mVs)并且HGF(80)≥339(kA/m)的条件。
12.一种包含根据权利要求10所述的分段式永磁体的产品。
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- 2011-05-31 KR KR1020110052109A patent/KR101082389B1/ko active IP Right Review Request
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- 2012-05-16 CN CN201280024984.6A patent/CN103548101B/zh active Active
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- 2012-05-16 EP EP12793259.8A patent/EP2715747B1/en active Active
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- 2012-05-16 WO PCT/KR2012/003853 patent/WO2012165780A1/en active Application Filing
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CN106278231A (zh) * | 2015-06-03 | 2017-01-04 | 自贡市江阳磁材有限责任公司 | M型稀土永磁铁氧体及其生产工艺 |
CN109311762A (zh) * | 2016-06-20 | 2019-02-05 | 优尼恩材料株式会社 | 铁氧体磁性材料和铁氧体烧结磁体 |
CN112159218A (zh) * | 2020-09-23 | 2021-01-01 | 横店集团东磁股份有限公司 | 一种低成本高性能永磁铁氧体材料的制备方法 |
Also Published As
Publication number | Publication date |
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EP2715747A1 (en) | 2014-04-09 |
BR112013029810A2 (pt) | 2017-07-18 |
MX361918B (es) | 2018-12-19 |
EP2715747B1 (en) | 2018-08-15 |
MX2013014054A (es) | 2014-02-27 |
HUE039686T2 (hu) | 2019-01-28 |
CN103548101B (zh) | 2016-12-07 |
KR101082389B1 (ko) | 2011-11-11 |
US10141091B2 (en) | 2018-11-27 |
PL2715747T3 (pl) | 2019-01-31 |
EP2715747A4 (en) | 2014-12-24 |
US20130307653A1 (en) | 2013-11-21 |
WO2012165780A1 (en) | 2012-12-06 |
BR112013029810B1 (pt) | 2021-12-14 |
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