CN101808943A - 粘结磁体用铁氧体粉末及其制造方法、及使用其的粘结磁体 - Google Patents
粘结磁体用铁氧体粉末及其制造方法、及使用其的粘结磁体 Download PDFInfo
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- CN101808943A CN101808943A CN200880108680A CN200880108680A CN101808943A CN 101808943 A CN101808943 A CN 101808943A CN 200880108680 A CN200880108680 A CN 200880108680A CN 200880108680 A CN200880108680 A CN 200880108680A CN 101808943 A CN101808943 A CN 101808943A
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- ferrite powder
- powder
- ferrite
- micro mist
- permanent magnet
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 163
- 239000000843 powder Substances 0.000 title claims abstract description 150
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 238000000034 method Methods 0.000 title claims description 11
- 239000002245 particle Substances 0.000 claims abstract description 40
- 238000009826 distribution Methods 0.000 claims abstract description 39
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 18
- 150000003624 transition metals Chemical class 0.000 claims abstract description 18
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- 239000003595 mist Substances 0.000 claims description 56
- 235000012054 meals Nutrition 0.000 claims description 41
- 150000001875 compounds Chemical class 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 19
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 7
- 239000006247 magnetic powder Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000006866 deterioration Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 18
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 17
- 229910000018 strontium carbonate Inorganic materials 0.000 description 17
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 16
- 238000002156 mixing Methods 0.000 description 15
- 238000005303 weighing Methods 0.000 description 13
- 238000001354 calcination Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000000700 radioactive tracer Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- YWXYYJSYQOXTPL-SLPGGIOYSA-N isosorbide mononitrate Chemical compound [O-][N+](=O)O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 YWXYYJSYQOXTPL-SLPGGIOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
本发明提供一种粘结磁体用铁氧体粉末,其即使为了获得流动性、压缩密度而扩大粒度分布范围,也能够抑制因其导致的SFD的增加,抑制取向性、磁化性的降低。制造一种粘结磁体用铁氧体粉末,其为平均粒径在0.20μm以上且不到5.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体粉,其中,通过激光衍射式粒度分布测定装置求得的该磁铅石型铁氧体粉的粒度分布中,粒径1μm以下的颗粒的比例为20质量%以上。
Description
技术领域
本发明涉及粘结磁体用铁氧体粉末及其制造方法、以及使用其的粘结磁体。
背景技术
要求高磁力的视听(AV、Audio Visual)、办公自动化(OA)机器、汽车电气部品等中使用的小型电动机、复印机的磁力辊等中使用的磁体中,使用了铁氧体系烧结磁体。但是,该铁氧体系烧结磁体会发生开裂,或者由于需要研磨而生产效率差,而且存在难以加工成复杂的形状等固有的问题。最近,一部分使用了稀土类磁体的粘结磁体在该领域中被使用。但是,稀土类磁体的成本高,为铁氧体系烧结磁体的20倍,且存在容易生锈等问题。因此,要求用铁氧体系粘结磁体来代替铁氧体系烧结磁体。
但是,粘结磁体和烧结磁体中,铁氧体的含有率大大不同。例如铁氧体系烧结磁体仅含有铁氧体,与此相对,铁氧体系粘结磁体中,由于含有树脂、橡胶等粘合剂,因而当然铁氧体的含有率比其低,磁力下降。因此,为了提高铁氧体系粘结磁体的磁力,增加铁氧体粉末的含有率成为必须的课题。但是,若增加铁氧体系粘结磁体中铁氧体粉末的含有率,则下次将铁氧体粉末与粘合剂混炼时,该混炼物变为高粘度,负荷增大而生产效率降低,极端的情况下则无法混炼。并且,即使能够混炼,下次成形时由于混炼物的流动性差,因而生产效率仍然低下,极端的情况下则无法成形。
为了解决该铁氧体系粘结磁体特有的问题,在粘合剂的选择、铁氧体粉末的表面处理等方面进行了改良。例如专利文献1中提出了将平均粒径为0.5~1.5μm的范围的铁氧体微粉、与平均粒径为30~250μm的范围的铁氧体粗粉配合的方法。
专利文献1:日本特公昭63-34610号公报
发明内容
发明要解决的问题
但是,根据本发明人等的研究,例如通过专利文献1中记载的方法,虽然能够获得压缩密度高、高填充性的铁氧体粉末,但从取向度的观点出发,发现了重要的SFD增大的问题。
本发明是在这样的状况下做出的,课题在于提供一种能够制造粘结磁体的粘结磁体用铁氧体粉末,所述粘结磁体即使为了获得流动性、压缩密度而扩大粒度分布范围,也能够保持取向度,具有高磁力。
另外,本发明中SFD是指将滞后曲线微分而获得的iHc的分布曲线的半幅值除以iHc而得到的值。该SFD的值越小,iHc分布范围越小。
用于解决问题的方案
本发明人为了解决上述问题进行了反复深入研究,结果想到了以下折衷关系:若将具有大粒径分布的M型铁氧体、和具有小粒径分布的M型铁氧体混合,则由于iHc的分布范围变宽,因此SFD的值也增加,且取向度降低。关于iHc,通过晶体各向异性和形状各向异性、单畴结构等进行说明,当平均粒径变小,则由于接近单轴结构,因而iHc变大。
这里,本发明人等想到了如下技术方案:使具有小粒径分布的M型铁氧体粉末中含有适量的过渡金属氧化物,从而使该具有小粒径分布的M型铁氧体粉末的iHc与具有大粒径分布的M型铁氧体的iHc相近。并且想到了如下划时代的见解:通过将该iHc相近的具有大、小粒径分布的磁铅石型铁氧体粉末混合,能够保持混炼物的流动性且提高取向度,从而完成了本发明。
即,用于解决上述问题的第1方案是一种粘结磁体用铁氧体粉末,其特征在于,
其为平均粒径在0.20μm以上且不到5.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn及Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体粉,其中,
通过激光衍射式粒度分布测定装置求得的该磁铅石型铁氧体粉的粒度分布中,粒径1μm以下的颗粒的比例为20质量%以上。
第2方案为一种粘结磁体用铁氧体粉末,其特征在于,
其含有:平均粒径在0.20μm以上且不到1.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体的微粉;和,平均粒径为1.00μm以上且不到5.00μm的磁铅石型铁氧体的粗粉,
所述磁铅石型铁氧体的微粉的配合量为15质量%以上、40质量%以下。
第3方案为根据第2方案所述的粘结磁体用铁氧体粉末,其特征在于,
所述含有过渡金属的氧化物的磁铅石型铁氧体的微粉含有0.01质量%以上、3质量%以下的Zr氧化物和/或Ti氧化物。
第4方案为根据第2方案所述的粘结磁体用铁氧体粉末,其特征在于,
所述含有过渡金属的氧化物的磁铅石型铁氧体的微粉含有0.01质量%以上、3质量%以下的Ti氧化物和Zn氧化物。
第5方案为一种粘结磁体用铁氧体粉末的制造方法,其特征在于,具有如下工序:
准备含有过渡金属氧化物的磁铅石型铁氧体,并将其制成平均粒径在0.20μm以上且不到1.00μm的范围的微粉的工序;
准备磁铅石型铁氧体,并将其制成粉平均粒径在1.00μm以上且不到5.00μm的范围的粗粉的工序;
将该微粉和该粗粉混合,制造具有微粉的配合量为15质量%以上且40质量%以下、剩余部分为粗粉的混合比率的铁氧体粉末的工序。
第6方案为一种粘结磁体,其特征在于,
采用第1~第4方案的任一项所述的粘结磁体用铁氧体粉末作为磁性粉。
发明的效果
根据本发明,能够获得尽管粒度分布范围宽、压缩密度高,SFD也小、且饱和磁化强度σs高的粘结磁体制造用铁氧体粉末。
具体实施方式
以下,对本发明的粘结磁体用铁氧体粉末进行详细说明。另外,本说明书中,只要没有特别说明,“%”表示质量百分率。
根据本发明人等的研究,关于铁氧体系粘结磁体,为了实现高磁力化,必要条件为:(1)铁氧体粉末在粘结磁体中的高填充、(2)提高铁氧体粉末的取向度。
以下,对用于满足该(1)、(2)的必要条件的实施方式和制造方法进行说明。
<1.铁氧体粉末在粘结磁体中的高填充>
为了获得高填充的铁氧体粉末,扩大该铁氧体粉末的粒度分布范围是有效的。
关于磁铅石型铁氧体粉末,本发明人等为了得知填充性和取向度高的制造条件而进行了广泛的试验研究。
并且,该试验研究的结果发现,下述粘结磁体用铁氧体粉末能够带来高填充性,所述粘结磁体用铁氧体粉末的特征在于,其为平均粒径在0.20μm以上且不到5.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体粉,其中,通过激光衍射式粒度分布测定装置求得的该磁铅石型铁氧体粉的粒度分布中,粒径1μm以下的颗粒的比例为20质量%以上。
另外,本发明中磁铅石型铁氧体(有时也称为“M型铁氧体”。)是指通式“AFe12O19”所表示的铁氧体。其中,A元素例如为Sr、Ba、Ca和Pb的1种以上。此外也包括Fe的一部分被Al那样的3价元素、以及Ti和Co那样的4价和2价元素置换而得到的物质。
并且本发明人等发现,将平均粒径为0.20μm以上且不到1.00μm的范围的磁铅石型铁氧体的微粉;和,平均粒径为1.00μm以上且不到5.00μm的范围、优选1.3μm以上且不到2.2μm的范围的M型铁氧体的粗粉混合,且该混合时平均粒径为0.30μm以上且不到1.00μm的范围的磁铅石型铁氧体的微粉的配合量为15~40%时,所得粉末能够带来高填充性。
<2.铁氧体粉末的取向度的提高>
根据本发明人等的研究,为了获得高取向性的铁氧体粉末,减小该铁氧体粉末的SFD是有效的,期待改善电动机的磁波形等。然而如<1>中所说明的,为了提高铁氧体粉末的填充性,由于扩大粒度分布范围提高压缩密度是有效的,因而SFD也会增加。为了克服该折衷关系,兼顾高取向和高填充,本发明人等想到了使上述微粉部分和粗粉部分的iHc接近的方案。
为了实现该方案,本发明人等对铁氧体进行了广泛的试验研究。
其结果发现,通过在磁铅石型铁氧体的微粉部分中添加0.01~3.00%、优选0.5~2.5%的过渡金属氧化物,该微粉部分的iHc变低,微粉部分与粗粉部分的iHc之差缩小,能够得到作为磁铅石型铁氧体整体的SFD小的磁性粉。另外,该过渡金属氧化物的添加量若为0.01%以上,则能够发挥iHc的降低效果,若为3.00%以下,则能够避免iHc的过于降低。
进而,根据本发明人等的研究,作为该过渡金属氧化物种,Zr、Ti、Zn、Co、Mn或Ni以及将它们任意组合的氧化物,从控制iHc方面出发而优选。其中,含有Zr、Ti的一种或两种元素的氧化物、含有Ti和Zn两种元素的氧化物,从提高σs的观点出发,也优选。
<3.铁氧体粉末制造方法>
为了制造本发明的磁铅石型铁氧体粉末,首先准备微粉原料和粗粉原料。
作为微粉原料,例如将含有过渡金属氧化物的铁氧体粉碎,或者粉碎后分级,以获得平均粒径为0.20μm以上且不到1.00μm的范围的微粉。该铁氧体的粉碎时,通过使平均粒径为0.20μm以上,能够避免该粉碎时间的长时间化,还能够避免粘结磁体制造时的磁特性降低。
另一方面,通过使平均粒径不到1.00μm,能够降低粒径超过1.00μm的颗粒的比例。通过降低粒径超过1.00μm的颗粒的比例,与后述粗粉混合时,能够提高混合粉的压缩密度,能实现粘结磁体中的高填充。
另一方面,作为粗粉原料,例如准备平均粒径为3.0μm以上且不到4.0μm的范围的铁氧体,将其粉碎,或者粉碎后分级,以获得平均粒径为1.00μm以上且不到50μm的范围的粗粉。该粉碎时,通过减少粒径不到1.00μm的颗粒的比例,与上述微粉的混合粉中,能够提高混合粉的压缩密度,能实现粘结磁体中的高填充。
另一方面,通过降低粒径超过5.00μm的颗粒的比例,能够较高地保持粘结磁体制造时的取向度和矫顽磁力。
将这样准备的平均粒径为0.20μm以上且不到1.00μm的范围的微粉;和,平均粒径为1.00μm以上且不到5.00μm的范围的粗粉混合,能够制造具有微粉的配合量为15~40%、剩余部分为粗粉的混合比率的铁氧体粉末。
若微粉的配合量为15%以上,则不仅能够提高混合粉的压缩密度,实现高填充,而且成形为粘结磁体后的矫顽磁力也变高。另外认为,若微粉的配合量为40%以下,则制造粘结磁体时,能够避免与粘合剂的混炼和成形时的粘度过高而难以粘结磁体化的情况,进而,能够避免成形后磁粉的取向度降低,剩余磁通密度Br降低的情况。
按照上述混合比将微粉和粗粉混合后,对该混合粉实施退火处理,或者,预先对微粉和粗粉分别实施退火处理后混合,获得本发明的粘结磁体用铁氧体粉末。通过该退火处理,制造微粉和粗粉时的粉碎时,能够除去颗粒中的结晶所产生的应变。该退火温度优选为800~1100℃。若为800℃以上,则能够充分地达到退火的效果,能够提高矫顽磁力和饱和磁化强度。此外,通过为1100℃以下,能够避免烧结的过度进行,避免压缩密度和取向性的降低。
<4.本发明的铁氧体粉末的特征>
如以上详细的说明,本发明的铁氧体粉末,不仅能够在粘结磁体中进行高填充,还能够提高铁氧体粉末的取向度。因此,通过使用本发明的铁氧体粉末,能够提供AV、OA机器、汽车电气部件等中使用的小型电动机、复印机的磁力辊等领域中前所未有的高磁力的粘结磁体。
实施例
以下,通过实施例对本发明进行具体说明,但本发明不限于这些实施例。
首先,对本实施例中制造的铁氧体粉的粉体特性的测定方法进行说明。
<平均粒径>
铁氧体粉的平均粒径,使用岛津制作所制的SS-100型,并根据空气透过法进行测定。
<比表面积>
铁氧体粉的比表面积(SSA),根据BET法,使用YuasaIonics Co.,Ltd.制的monosorb进行测定。
<压缩密度>
铁氧体粉的压缩密度,在内径2.54cmφ的圆筒形模具中填充10g铁氧体粉后,在1ton/cm3的压力下压缩。以此时的铁氧体粉的密度作为压缩密度进行测定。
<磁特性>
铁氧体粉的磁特性,使用VSM(东英工业株式会社制,VSM-P7),进行σs(emu/g)、SFD的测定。
<粒度分布>
铁氧体粉的粒度分布,使用干式激光衍射式粒度分布测定装置(Japan Laser Corp.制,HELOS&RODOS),在焦距(focallength)=20mm、分散压5.0bar、吸引压130mbar的条件下进行测定。
(实施例1)
(1)微粉的制造
按照以摩尔比计为氧化铁5.6:碳酸锶1秤量氧化铁和碳酸锶,相对于该秤量物添加0.5质量%的ZrO2并混合。接着,将该混合物用水造粒,干燥后,在电炉中1020℃下煅烧40分钟得到煅烧物。将该煅烧物用锤磨机(商品名:样品磨)粉碎,再用湿式粉碎机(商品名:湿磨机)进行湿式粉碎,获得实施例1的微粉。
所得微粉含有0.5质量%的ZrO2,平均粒径:0.65μm,σs:57.3emu/g。
(2)粗粉的制造
按照以摩尔比计为氧化铁5.6∶碳酸锶1秤量并混合氧化铁和碳酸锶。接着,将该混合物用水造粒,干燥后,在电炉中1200℃下煅烧2小时,获得煅烧物。将该煅烧物用样品磨粉碎,再用湿式粉碎机(商品名:湿磨机)湿式粉碎,获得实施例1的粗粉。
所得粗粉的平均粒径:2.11μm,σs:54.4emu/g。
(3)混合粉(铁氧体粉末)的制造
秤量上述(1)中得到的微粉(20%)和(2)中得到的粗粉(80%),并将其很好地混合,将该混合粉在电炉中950℃下煅烧(退火)1小时,获得实施例1的铁氧体粉末。
所得铁氧体粉末为:平均粒径:1.22μm,比表面积:2.48m2/g,压缩密度:3.45g/cm3,σs:57.4emu/g,SFD:0.9129。
(4)粘结磁体的制造
在90份上述(3)中得到的铁氧体粉末中添加0.6份硅烷系偶联剂(Dow Corning Toray制,Z-6094N),用混合机(共立理工制,SK-10型)搅拌以进行该铁氧体粉末的表面处理。接着,向该铁氧体粉末中添加8.6份粉末状的6-尼龙(宇份兴产株式会社制,P-1011F)和0.8份滑剂(Henkel制,VPN-212P),得到混合物。
接着,将该混合物用混炼机(东洋精机制作所制,100C100型)在230℃下混炼颗粒化。然后将该混炼颗粒在3.4KOe的磁场中注塑成型,获得实施例1的直径15mm×高8mm的圆柱状各向异性粘结磁体。这里,该混炼、注塑成型能够顺利实施。
将该实施例1的磁体用BH示踪剂进行测定,显示为S Q(区域、Area)0.893、Hk/iHc0.803。该结果记载于一览表即表1中。
(实施例2)
实施例1中(1)制造微粉时,ZrO2添加量为2.0质量%,除此之外,与实施例1同样地进行操作,获得实施例2的铁氧体粉末。
实施例2的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
另外,表2中,D5、D10、…D90分别为累积粒度分布为5%、10%…90%时的粒径。另一方面,0.3μm↓(0.3μm以下)、1μm↓(1μm以下)、…14.6μm↑(14.6μm以上)分别为粒径0.3μm以下的颗粒的存在比例、粒径1μm以下的颗粒的存在比例、…粒径4.6μm以上的颗粒的存在比例。
(实施例3)
秤量实施例1的(1)中得到的微粉(30%)、和(2)中得到的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得实施例3的铁氧体粉末。
实施例3的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(实施例4)
实施例1中(1)制造微粉时所加入的纤维金属氧化物种为TiO2、添加量为2.0质量%,除此之外,与实施例1同样地操作,获得实施例4的铁氧体粉末。
实施例4的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中。
(实施例5)
实施例1中(1)制造微粉时摩尔比为氧化铁5.8∶碳酸锶1,除此之外,与实施例1同样地操作,获得实施例5的铁氧体粉末。
实施例5的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中。
(实施例6)
秤量实施例1中(1)制造微粉时的摩尔比为氧化铁5.5∶碳酸锶1、所添加的过渡金属氧化物种为TiO2、添加量为0.05质量%所获得的微粉(30%)、和(2)制造粗粉时的摩尔比为氧化铁5.9∶碳酸锶1、在电炉中1230℃下煅烧所获得的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得实施例6的铁氧体粉末。
实施例6的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(实施例7)
秤量实施例1中(1)制造微粉时的摩尔比为氧化铁5.5∶碳酸锶1、所添加的过渡金属氧化物种为TiO2、添加量为0.5质量%所获得的微粉(30%)、和(2)制造粗粉时的摩尔比为氧化铁5.9∶碳酸锶1、在电炉中1230℃下煅烧所获得的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得实施例7的铁氧体粉末。
实施例7的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(实施例8)
秤量实施例1中(1)制造微粉时的摩尔比为氧化铁5.5∶碳酸锶1、所添加的过渡金属氧化物种为TiO2+ZnO、添加量为0.1质量%+0.1质量%=0.2质量%所获得的微粉(30%)、和(2)制造粗粉时的摩尔比为氧化铁5.9∶碳酸锶1、在电炉中1230℃下煅烧所获得的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得实施例8的铁氧体粉末。
实施例8的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(实施例9)
秤量实施例1中(1)制造微粉时的摩尔比为氧化铁5.5∶碳酸锶1、所添加的过渡金属氧化物种为TiO2+ZnO、添加量为1.0质量%+1.0质量%=2.0质量%所获得的微粉(30%)、和(2)制造粗粉时的摩尔比为氧化铁5.9∶碳酸锶1、在电炉中1230℃下煅烧所得的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得实施例9的铁氧体粉末。
实施例9的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(实施例10)
秤量实施例1中(1)制造微粉时的摩尔比为氧化铁5.5∶碳酸锶1、所添加的过渡金属氧化物种为TiO2+ZrO2、添加量为1.0质量%+1.0质量%=2.0质量%所得的微粉(30%)、和(2)制造粗粉时的摩尔比为氧化铁5.9∶碳酸锶1、在电炉中1230℃下煅烧所得的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得实施例10的铁氧体粉末。
实施例10的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(比较例1)
实施例1中(1)制造微粉时不添加ZrO2,除此之外,与实施例1同样地操作,获得比较例1的铁氧体粉末和粘结磁体。
比较例1的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
接下来,使用上述所得铁氧体粉末,与实施例1同样地,获得比较例1的圆柱状各向异性粘结磁体。
并且,将该比较例1的磁体用BH示踪剂进行测定,显示为SQ(Area)0.878、Hk/iHc0.772。该结果记载于一览表即表1中。
(比较例2)
秤量实施例1中(1)制造微粉时不添加ZrO2而得到的微粉(30%)、和(2)中所得到的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得比较例2的铁氧体粉末。
比较例2的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
(比较例3)
实施例1中(3)制造混合粉(铁氧体粉末)时,秤量(1)中得到的微粉(80%)、和(2)中得到的粗粉(20%),将其充分地混合,除此之外,与实施例1同样地操作,获得比较例2的铁氧体粉末。
比较例3的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中。
(比较例4)
实施例1中(1)制造微粉时ZrO2添加量为10质量%,除此之外,与实施例1同样地操作,获得比较例4的铁氧体粉末。
比较例4的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中。
(比较例5)
秤量实施例1中(1)制造微粉时的摩时比为氧化铁5.5∶碳酸锶1、不添加ZrO2所得的微粉(30%)、和(2)制造粗粉时的摩尔比为氧化铁5.9∶碳酸锶1、在电炉中1230℃下煅烧所得的粗粉(70%),将其充分地混合,除此之外,与实施例1同样地操作,获得比较例5的铁氧体粉末。
比较例5的铁氧体粉末的平均粒径、比表面积、压缩密度、σs、SFD的测定值记载于表1中,该铁氧体粉末的粒度分布记载于表2中。
[表1]
[表2]
(总结)
由表1、2的结果可知,为平均粒径0.20μm以上且不到5.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体粉,其中,通过激光衍射式粒度分布测定装置求得的该磁铅石型铁氧体粉的粒度分布中,粒径1μm以下的颗粒的比例为20质量%以上,或者为含有平均粒径为0.20μm以上且不到1.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体的微粉;和,平均粒径为1.00μm以上且不到5.00μm的磁铅石型铁氧体的粗粉,所述磁铅石型铁氧体的微粉的配合量为15质量%以上、40质量%以下的、实施例1~10的铁氧体粉末,具有与不具有含有过渡金属氧化物的技术方案的比较例1、2、5的铁氧体粉末几乎同样的粉末物性。
然而,当比较实施例1~10的铁氧体粉末、和比较例1~5的铁氧体粉末的磁特性时,σs、SFD均是实施例1~10的铁氧体粉末比较优异。
进而可知,当比较实施例1的粘结磁体、和比较例1的粘结磁体的磁特性时,SQ、Hk/iHc均是实施例1的粘结磁体比较优异,为高取向和高磁力品。
Claims (6)
1.一种粘结磁体用铁氧体粉末,其特征在于,其为平均粒径在0.20μm以上且不到5.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体粉,其中,
通过激光衍射式粒度分布测定装置求得的该磁铅石型铁氧体粉的粒度分布中,粒径1μm以下的颗粒的比例为20质量%以上。
2.一种粘结磁体用铁氧体粉末,其特征在于,其含有:平均粒径在0.20μm以上且不到1.00μm的范围、且含有选自Zr、Ti、Zn、Co、Mn和Ni所组成的组中的至少1种以上过渡金属的氧化物的磁铅石型铁氧体的微粉;和,平均粒径在1.00μm以上且不到5.00μm的范围的磁铅石型铁氧体的粗粉,
所述磁铅石型铁氧体的微粉的配合量为15质量%以上、40质量%以下。
3.根据权利要求2所述的粘结磁体用铁氧体粉末,其特征在于,所述含有过渡金属的氧化物的磁铅石型铁氧体的微粉含有0.01质量%以上、3质量%以下的Zr氧化物和/或Ti氧化物。
4.根据权利要求2所述的粘结磁体用铁氧体粉末,其特征在于,所述含有过渡金属的氧化物的磁铅石型铁氧体的微粉含有0.01质量%以上、3质量%以下的Ti氧化物和Zn氧化物。
5.一种粘结磁体用铁氧体粉末的制造方法,其特征在于,具有以下工序:
准备含有过渡金属氧化物的磁铅石型铁氧体,并将其制成平均粒径在0.20μm以上且不到1.00μm的范围的微粉的工序;
准备磁铅石型铁氧体,并将其制成平均粒径在1.00μm以上且不到5.00μm的范围的粗粉的工序;
将该微粉和该粗粉混合,制造具有微粉的配合量为15质量%以上、40质量%以下、剩余部分为粗粉的混合比率的铁氧体粉末的工序。
6.一种粘结磁体,其特征在于,其使用权利要求1~4的任一项所述的粘结磁体用铁氧体粉末作为磁性粉。
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- 2008-09-25 JP JP2008246834A patent/JP5578777B2/ja active Active
- 2008-09-26 WO PCT/JP2008/067472 patent/WO2009041606A1/ja active Application Filing
- 2008-09-26 KR KR1020107009282A patent/KR101515251B1/ko active IP Right Grant
- 2008-09-26 CN CN2008801086801A patent/CN101808943B/zh not_active Expired - Fee Related
- 2008-09-26 EP EP08833553.4A patent/EP2204352B1/en not_active Not-in-force
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CN107004479A (zh) * | 2015-02-23 | 2017-08-01 | 同和电子科技有限公司 | 粘结磁体用铁氧体粉末及其制造方法以及铁氧体系粘结磁体 |
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CN112640008A (zh) * | 2018-08-28 | 2021-04-09 | 富士胶片株式会社 | 磁铅石型六方晶铁氧体的粉体及其制造方法及电波吸收体 |
CN112640008B (zh) * | 2018-08-28 | 2023-11-28 | 富士胶片株式会社 | 磁铅石型六方晶铁氧体的粉体及其制造方法及电波吸收体 |
CN112805795A (zh) * | 2018-10-10 | 2021-05-14 | 味之素株式会社 | 磁性糊料 |
US12014854B2 (en) | 2018-10-10 | 2024-06-18 | Ajinomoto Co., Inc. | Magnetic paste |
CN110828091A (zh) * | 2019-11-21 | 2020-02-21 | 广东华南半导体光电研究院有限公司 | 一种环保型磁体的制备方法 |
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US20100295643A1 (en) | 2010-11-25 |
WO2009041606A1 (ja) | 2009-04-02 |
JP5578777B2 (ja) | 2014-08-27 |
EP2204352B1 (en) | 2018-01-03 |
JP2009099969A (ja) | 2009-05-07 |
CN101808943B (zh) | 2013-06-26 |
EP2204352A4 (en) | 2013-05-15 |
KR101515251B1 (ko) | 2015-04-24 |
EP2204352A1 (en) | 2010-07-07 |
KR20100063133A (ko) | 2010-06-10 |
US8337714B2 (en) | 2012-12-25 |
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