CN1649039A - MnZn铁氧体的制造方法 - Google Patents
MnZn铁氧体的制造方法 Download PDFInfo
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- CN1649039A CN1649039A CNA2005100057636A CN200510005763A CN1649039A CN 1649039 A CN1649039 A CN 1649039A CN A2005100057636 A CNA2005100057636 A CN A2005100057636A CN 200510005763 A CN200510005763 A CN 200510005763A CN 1649039 A CN1649039 A CN 1649039A
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- mnzn
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- 238000004519 manufacturing process Methods 0.000 title claims description 29
- 229910000859 α-Fe Inorganic materials 0.000 title abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 46
- 230000004907 flux Effects 0.000 claims abstract description 41
- 238000004438 BET method Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 30
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 15
- 238000007493 shaping process Methods 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 10
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 238000012423 maintenance Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 238000010304 firing Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 238000009825 accumulation Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 230000007850 degeneration Effects 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910015621 MoO Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Abstract
本发明提供一种在数十kHz至数百kHz的频带区内损耗较低、且100℃左右的饱和磁通密度较高的MnZn铁氧体。在该MnZn铁氧体的制造方法中,具有将比表面积(根据BET法)为2.0~5.0m2/g、50%粒径为0.7~2.0μm的成形用粉末成形为预定形状的成形体的工序、以及烧成该成形体得到烧成体的工序。作为MnZn铁氧体,优选的主要成分为Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:4mol%或以下(但不含O)、余量实质上是MnO。
Description
技术领域
本发明涉及高温(100℃附近)下具有高饱和磁通密度、高导磁率、以及低损耗的MnZn铁氧体的制造方法。
背景技术
近年来,电子设备向小型、高输出功率方面发展,随之各种部件向高集成度、高速处理方面发展,这要求供给电力的电源线能够承载很大的电流。
而且要求电源线即使在高温下也能保持规定的性能,这是因为电源线往往暴露在来自于部件(例如CPU)等的发热环境中。并且电源线即使在汽车用电子电路那样高的使用环境温度条件下,也要求保持规定的性能。
因此,对于电源线所使用的变压器和电抗器也要求在高温下以大电流使用。
作为这些变压器和电抗器所使用的材料,有软磁金属材料和铁氧体材料。铁氧体材料被分类为MnZn系铁氧体和Ni系铁氧体。
与铁氧体相比,由于软磁金属材料的饱和磁通密度较高,因此具有即使通过更大的电流也不会引起磁饱和的优点。但是,软磁金属材料通常存在损耗高、价格贵、比重大、防锈性差等问题。
另一方面,铁氧体具有性能价格比优良、在数十kHz至数百kHz的频带中损耗较低的优点。另外,比Ni系铁氧体的饱和磁通密度高的MnZn系铁氧体一般应用于大电流用变压器以及扼流线圈。
例如在特公昭63-59241号公报中,除了MnO和ZnO以外,通过含有选自NiO、Li2O以及MgO中的至少1种而取得了150℃或以上温度的低损耗。但是,由于损耗显示最小的温度(以下称之为底部温度)为150℃或以上,因此在一般的变压器、电抗器用铁心所使用的温度范围(80~120℃)内,导致损耗和初始导磁率的退化,因而是不合适的。
另外,日本专利第3389170号公报公开了通过用NiO置换MnZn系铁氧体,其饱和磁通密度Bs在440mT或以上的直流重叠特性良好,能够在较宽的温度区使用。
此外,在特开2001-080952号公报中,通过在MnZn系铁氧体中添加CoO,获得了在20~100℃的宽温度区内电力损耗明显下降、以及温度变化相对缓和的效果。具体地说,得到了电力损耗的最小值为400kW/m3或以下、且电力损耗的最大值与最小值之差为150kW/m3或以下的特性。
此外,在特开平11-3813号公报中,通过使Fe2O3含量超过50mol%的MnZn系铁氧体的基本成分中同时含有NiO和CoO,即使在1MHz左右或以上的高频区仍表现出所谋求的低损耗。该MnZn系铁氧体具有下列的组成:含Fe2O3:52~68mol%、NiO:0.5~10mol%、ZnO:15mol%或以下、CoO:0.005~0.5mol%、以及余量实质上是MnO。
而且作为同时含有NiO和CoO的MnZn系铁氧体,还知道特开2000-286119号公报所公开的MnZn系铁氧体。该铁氧体的特征在于:相对于由Fe2O3:52~56mol%、ZnO:6~14mol%、NiO:4mol%或以下、CoO:0.01~0.6mol%、以及余量实质上为MnO所构成的基本成分,作为外加成分含有SiO2:0.0050~0.0500重量%以及CaO:0.0200~0.2000重量%,再以预定量含有从Ta2O5、ZrO2、Nb2O5、V2O5、K2O、TiO2、SnO2以及HfO2中选择的至少1种添加成分,并且在频率100kHz、最大磁通密度200mT的测定条件下,其损耗达到最低时的温度为50℃~85℃。
正如以上所说明的那样,同时含有NiO和CoO的MnZn系铁氧体,在损耗方面可能具备优良的特性。但是,特开平11-3813号公报所公开的MnZn系铁氧体,尽管在1MHz左右以上的高频带区域的损耗具有优良的特性,但对于数十kHz至数百kHz的频带,在应用方面并不合适。
另外,尽管在室温下的饱和磁通密度较高,但在一般的变压器、电抗器用铁心的使用温度区(80~120℃)内,如果饱和磁通密度下降,则也不能发挥所要求的变压器、电抗器用铁心的性能。
特开2000-286119号公报所公开的MnZn系铁氧体,尽管在数十kHz至数百kHz频带内的损耗具有优良的特性,但没有考量100℃左右的饱和磁通密度。
发明内容
本发明是基于上述的技术课题而完成的,其目的在于:提供数十kHz至数百kHz频带内的损耗较低、且100℃左右的饱和磁通密度较高的MnZn系铁氧体。
为此目的,本发明者经过反复研讨,结果发现:根据MnZn系铁氧体制造时所使用的原料粉末粒子(一次粒子)的特性的不同,损耗显示最低的温度(以下称之为底部温度)以及100℃左右的饱和磁通密度随之变化。本发明基于这一发现而提供一种MnZn系铁氧体的制造方法,其特征在于:该制造方法具有将比表面积(根据BET法测定)为2.0~5.0m2/g、50%粒径为0.7~2.0μm的成形用粉末成形为预定形状的成形体的工序、以及烧成该成形体得到烧成体的工序。成形用粉末通常在原料粉末经预烧后,将该预烧物粉碎而制得,但也可以包含次要成分用粉末。另外,所谓50%粒径是指将被测粉末的总体积设定为100%而求出累积曲线时,在该累积曲线上累积量为50%的那一点的粒径。
本发明的MnZn铁氧体,优选的主要成分为Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:4mol%或以下(但不包括0%)、以及余量实质上为MnO。
另外,在本发明中,成形用粉末的90%粒径优选为4.0μm或以下。并且所谓90%粒径是指将被测粉末的总体积设定为100%而求出累积曲线时,在该累积曲线上累积量为90%的那一点的粒径。
进而在本发明中,成形体的烧成优选在1250~1450℃的保持温度下进行。
在本发明中,作为第1次要成分,优选含有换算成SiO2为60~250ppm的Si、以及换算成CaCO3为700~2500ppm的Ca。另外,作为第2次要成分,优选含有CoO:500~4000ppm、Nb2O5:50~500ppm、ZrO2:50~1000ppm、Ta2O5:50~1000ppm、V2O5:50~1000ppm、HfO2:50~1000ppm、In2O5:50~2000ppm、MoO3:50~1000ppm、Bi2O3:50~1000ppm之中的1种、2种或更多种。
根据上述本发明的制造方法,能够得到由平均晶粒直径为5~35μm的烧成体构成的、100℃的饱和磁通密度为440mT或以上、损耗显示最小值的温度即底部温度为85~120℃、损耗的最小值(100kHz、200mT)为350kW/m3或以下的MnZn铁氧体。
根据本发明,能够提供数十kHz至数百kHz的频带内损耗较低、且100℃左右的饱和磁通密度较高的MnZn铁氧体。
附图说明
图1是表示实施例1制作的试样组成等的图表。
图2是表示实施例1制作的试样的磁特性等的图表。
图3是表示烧成温度1300℃时、比表面积与底部温度下的损耗的关系曲线。
图4是表示烧成温度1300℃时、50%粒径与底部温度下的损耗的关系曲线。
图5是表示烧成温度1300℃时、90%粒径与底部温度下的损耗的关系曲线。
图6是表示烧成温度1300℃时、比表面积与饱和磁通密度的关系曲线。
图7是表示烧成温度1300℃时、50%粒径与饱和磁通密度的关系曲线。
图8是表示烧成温度1300℃时、90%粒径与饱和磁通密度的关系曲线。
图9是表示烧成温度1325℃时、比表面积与底部温度下的损耗的关系曲线。
图10是表示烧成温度1325℃时、50%粒径与底部温度下的损耗的关系曲线。
图11是表示烧成温度1325℃时、90%粒径与底部温度下的损耗的关系曲线。
图12是表示烧成温度1325℃时、比表面积与饱和磁通密度的关系曲线。
图13是表示烧成温度1325℃时、50%粒径与饱和磁通密度的关系曲线。
图14是表示烧成温度1325℃时、90%粒径与饱和磁通密度的关系曲线。
图15是表示实施例2制作的试样的组成、磁特性等的图表。
图16是表示实施例3制作的试样的磁特性等的图表。
图17是表示实施例3制作的试样的磁特性等的图表。
具体实施方式
以下,就本发明进行更详细的说明。
首先,就成分的限定理由进行说明。
<Fe2O3>
当Fe2O3的含量较高时,高温区的饱和磁通密度提高,但另一方面,损耗存在退化的倾向。当Fe2O3的含量低于54mol%时,高温区的饱和磁通密度降低。另一方面,当Fe2O3的含量超过57mol%时,损耗的增加变得显著。因此,本发明将Fe2O3设定为54~57mol%。在该范围内,伴随着Fe2O3含量的增加,底部温度向低温侧移动,而当Fe2O3含量在54~57mol%的范围内时,能够保持磁特性或者尽可能地抑制磁特性的下降,同时将底部温度设定在85~120℃的范围内。优选的Fe2O3含量为54.5~56.5mol%,再优选的Fe2O3含量为54.5~55.5mol%。
<ZnO>
ZnO的含量也影响饱和磁通密度及损耗。当ZnO低于5mol%时,饱和磁通密度降低,同时损耗增大。而ZnO超过10mol%时,饱和磁通密度仍然降低,同时损耗也增大。因此,本发明将ZnO设定为5~10mol%。伴随ZnO含量的增加,底部温度向低温侧移动,但当ZnO含量在5~10mol%的范围内时,能够保持磁特性或者尽可能地抑制磁特性的降低,同时能够将底部温度设定在85~120℃的范围内。优选的ZnO含量为6~9mol%,再优选的ZnO含量为7~8mol%。
<NiO>
NiO使居里温度升高,由此能够使饱和磁通密度升高。但是,当NiO的含量超过4mol%时损耗增大。因此,本发明为得到饱和磁通密度得以改善而损耗较低这一效果,使NiO的含量在4mol%或以下(但不含0)的范围内。优选的NiO含量为0.2~4mol%,再优选的NiO含量为0.5~3mol%。
本发明的MnZn铁氧体,作为第1次要成分能够含有换算成SiO2为60~250ppm的Si、以及换算成CaCO3为700~2500ppm的Ca。Si和Ca由于在晶界偏析而形成高电阻层,有利于降低损耗,同时作为烧结助剂具有使烧结密度提高的效果。当Si按换算成SiO2计超过250ppm或Ca按换算成CaCO3计超过2500ppm时,因不连续的异常晶粒长大而引起的损耗的退化较大。于是本发明将Si按换算成SiO2计设定在250ppm或以下、将Ca按换算成CaCO3计设定在2500ppm或以下。另一方面,当Si按换算成SiO2计不足60ppm或Ca按换算成CaCO3计不足700ppm时,则不能充分得到上述效果,因此优选Si按换算成SiO2计含有60ppm或以上、Ca按换算成CaCO3计含有700ppm或以上。关于再优选的Si和Ca的含量,Si按换算成SiO2计为80~200ppm、Ca按换算成CaCO3计为1000~1800ppm;关于更优选的Si和Ca的含量,Si按换算成SiO2计为80~150ppm、Ca按换算成CaCO3计为1200~1700ppm。
此外,在复合添加Si和Ca的情况下,Si和Ca分别换算成SiO2和CaCO3,SiO2/CaCO3(重量比)设定在0.04~0.25、更优选设定在0.05~0.2的范围是有效的。
作为本发明的第2次要成分,能够含有CoO:500~4000ppm、Nb2O5:50~500ppm、ZrO2:50~1000ppm、Ta2O5:50~1000ppm、V2O5:50~1000ppm、HfO2:50~1000ppm、In2O5:50~2000ppm、MoO3:50~1000ppm、Bi2O3:50~1000ppm的1种、2种或以上。通过含有这些第2次要成分,能够谋求饱和磁通密度的升高和损耗的降低。优选的含量为CoO:600~2500ppm、Nb2O5:100~400ppm、In2O5:50~1000ppm、ZrO2、Ta2O5、V2O5、HfO2、MoO3、Bi2O3均为50~400ppm。再者,对于CoO、Nb2O5、In2O5,设定CoO:600~2000ppm、Nb2O5:80~300ppm、In2O5:50~400ppm是更为优选的。此外,在复合添加第2次要成分的情况下,总含量优选设定在5000ppm或以下,而且最优选将CoO用作第2次要成分。
作为本发明的第3次要成分,能够在SnO2:500~10000ppm以及TiO2:500~10000ppm的范围内含有1种或2种。SnO2和TiO2存在于晶粒内和晶界,具有使损耗降低的效果。但是,当SnO2和TiO2的含量超过10000ppm时,将因不连续异常晶粒长大而导致损耗的退化以及饱和磁通密度的降低。因此,本发明将SnO2和TiO2的上限值分别设定在10000ppm。另一方面,为了充分得到上述的降低损耗的效果,优选第3次要成分的含量为500ppm或以上。而且进一步优选的第3次要成分的含量为1000~8000ppm,更优选的第3次要成分的含量为1000~7000ppm。另外,在复合添加第3次要成分的情况下,总量优选设定为10000ppm或以下。
其次,针对本发明的MnZn铁氧体说明适宜的制造方法。
作为主要成分的原料,使用氧化物粉末或通过加热成为氧化物的化合物粉末。具体地说,能够使用Fe2O3粉末、Mn3O4粉末、ZnO粉末、以及NiO粉末等。
湿式混合主要成分的原料粉末以后进行预烧。预烧的保持温度在700~1000℃的范围内选择即可。气氛可以是N2气或大气。预烧的保持时间可以在0.5~5.0小时的范围内适当地进行选择。预烧后将预烧物进行粉碎。另外,本发明不局限于上述主要成分的原料,也可以将含有2种或以上金属的复合氧化物的粉末作为主要成分的原料。例如,通过氧化焙烧含有氯化铁、氯化锰的水溶液,可以得到含有Fe和Mn的复合氧化物的粉末。将该粉末与ZnO粉末混合作为主要成分的原料也是可以的。在这种情况下,预烧是不需要的。
同样地,作为次要成分的原料,也能使用氧化物粉末或通过加热成为氧化物的化合物粉末。具体地说,能够使用SiO2、CaCO3、Co3O4、Nb2O5、ZrO2、Ta2O5、HfO2、In2O5、SnO2、TiO2、MoO3、V2O5、Bi2O3等粉末。这些次要成分的原料粉末与预烧后被粉碎的主要成分粉末相混合。但是,将次要成分的原料粉末与主要成分的原料粉末混合后也可以预烧其混合粉末。
由主要成分以及次要成分构成的混合粉末,其比表面积(比表面积根据BET法测定,下同)设定为2.0~5.0m2/g、50%粒径为0.7~2.0μm。在此,比表面积不足2.0m2/g或超过5.0m2/g时损耗增大,而比表面积不足2.0m2/g时饱和磁通密度减小。另一方面, 50%粒径不足0.7μm或超过2.0μm时损耗增大,而50%粒径超过2.0μm时饱和磁通密度减小。优选的比表面积为2.5~4.0m2/g,优选的50%粒径为0.9~1.5μm。
为赋予供给成形的混合粉末以这样的特性,可以使用调整预烧后的粉碎条件或应用分级等公知的手段。
将预烧物粉碎后,为了顺利地进行成形工序,可以对预烧物粉末进行造粒。例如能够使用喷雾干燥器进行造粒。在混合粉末中少量添加适当的粘结材料例如聚乙烯醇(PVA),将其用喷雾干燥器进行喷雾和干燥。颗粒的粒径优选设定为80~200μm左右。
所得到的颗粒例如使用带有预定形状的模具的压力机成形为所希望的形状。然后,在随后的烧成工序中烧成该成形体。
在烧成工序,控制烧成温度和烧成气氛是必要的。
烧成在1250~1450℃的范围内保持规定时间即可。为了充分发挥本发明的MnZn铁氧体的效果,优选在1300~1400℃的范围内烧成成形体。
根据本发明的MnZn铁氧体材料,优选将平均晶粒直径设定在5~35μm的范围内。这是因为晶粒直径小于5μm时,磁滞损耗增大,另一方面,晶粒直径增大到超过35μm时,涡流损耗增大。优选的平均晶粒直径为8~30μm,更优选的平均晶粒直径为10~25μm。
像本发明那样,通过对烧成前的成形用粉末进行上述那样的特别定制,就能得到具有下列特性的MnZn铁氧体,即100℃的饱和磁通密度为440mT或以上,损耗显示最小值的温度即底部温度为85~120℃,损耗的最小值(测定条件:100kHz、200mT)为350kW/m3或以下。
实施例1
将作为主要成分原料的Fe2O3粉末、MnO粉末、ZnO粉末以及NiO粉末按照图1所示的组成进行湿式混合后,以图1所示的温度分别预烧2小时。
其次,将主要成分原料的预烧物与次要成分原料进行混合。作为次要成分原料,使用SiO2粉末、CaCO3粉末、Nb2O5粉末、ZrO2粉末以及Co3O4粉末。在主要成分原料的预烧物中添加次要成分的原料,边粉碎边混合。并测定粉碎后的混合粉末的比表面积(BET)、50%粒径以及90%粒径,其结果示于图1。
从图1可以确认:预烧温度越低且粉碎时间越长,则粉末的比表面积越大。
接着在得到的混合物中添加粘结剂,经颗粒化后成形,得到圆环形状的成形体。将得到的成形体按照图2所示的条件进行烧成,由此便得到铁氧体铁心。
另外,使用该铁氧体铁心测定初始导磁率(μi,测定温度:25℃、测定频率:100kHz)、25℃(RT)以及100℃的饱和磁通密度(Bs,测定磁场:1194A/m)、25~120℃的铁心损耗(Pcv,测定条件:100kHz、200mT)。其结果示于图2。
将比表面积(BET)、50%粒径以及90%粒径同底部温度(90℃)的损耗(Pcv at bottom)以及100℃的饱和磁通密度(Bs at 100℃)的关系经过整理的结果示于图3~图14。其中,图3~图8表示在1300℃烧成的试样的结果、图9~图14表示在1325℃烧成的试样的结果。
正如图3~图5、图9~图11所示那样,可知底部温度下的损耗伴随比表面积(BET)、50%粒径以及90%粒径的变化而变化,比表面积(BET)、50%粒径以及90%粒径无论是过大还是过小,其损耗均增大。即为了减小底部温度下的损耗,有必要控制比表面积(BET)、50%粒径以及90%粒径。
另一方面,正如图6~图8、图12~图14所示那样,比表面积(BET)越大、反之50%粒径以及90%粒径越小,则100℃的饱和磁通密度越能得到较高的值。
因此,为了兼备底部温度下的损耗以及100℃的饱和磁通密度这2个特性,优选比表面积(BET)在2.0~5.0m2/g、且50%粒径在0.7~2.0μm、进而90%粒径在4.0μm或以下的范围内。
实施例2
设定的组成以及烧成条件示于图15、而且作为第1次要成分只添加SiO2和CaCO3,除此以外与实施例1一样制作MnZn铁氧体,仍然与实施例1一样测定特性,其结果示于图15。另外,烧成前的粉末特性如下:
BET:2.5~4.0m2/g
50%粒径:0.7~1.5μm
90%粒径:1.0~4.0μm
而且图15中的Pcv表示在底部温度的损耗、B.Temp.表示底部温度。
正如图15所示那样,在Fe2O3少至53.5mol%的场合,饱和磁通密度(Bs)降低。另一方面,在Fe2O3多达57.5mol%时,损耗增大。
其次,在ZnO少至4.5mol%的场合,损耗增大,另一方面在ZnO多达11mol%的场合,饱和磁通密度(Bs)降低。
而且在NiO多达4.5mol%时,损耗增大。
从以上结果可知,本发明优选将Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:4mol%或以下(但不含0)、余量实质上是MnO作为主要成分。
实施例3
除了设定在图16和图17中的次要成分的种类以及含量以外,与实施例1一样制作MnZn铁氧体,仍然与实施例1一样测定特性,其结果示于图16和图17。烧成前的粉末特性如下:
BET:2.5~4.0m2/g
50%粒径:0.7~1.5μm
90%粒径:1.0~4.0μm
而且在图17中的Pcv at RT表示25℃的损耗、Pcv at 100℃表示于100℃的损耗、ΔPcv表示25℃的损耗-100℃的损耗。
正如图16所示那样,通过添加第2次要成分和第3次要成分,能够提高饱和磁通密度(Bs)且减小损耗。但是,过多地添加反而使饱和磁通密度(Bs)降低或者损耗增加,因此,在适宜的范围内添加是较为理想的。
另外,正如图17所示那样,通过适量添加CoO,能够降低底部温度下的损耗,同时使ΔPcv减小。
Claims (20)
1.一种MnZn铁氧体的制造方法,其特征在于:该制造方法具有将根据BET法测定的比表面积为2.0~5.0m2/g、50%粒径为0.7~2.0μm的成形用粉末成形为预定形状的成形体的工序、以及烧成所述成形体从而得到烧成体的工序。
2.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体的主要成分为Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:大于0mol%且不超过4mol%、以及余量实质上是MnO。
3.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述成形用粉末的所述比表面积为2.5~4.0m2/g。
4.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述成形用粉末的所述50%粒径为0.9~1.5μm。
5.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述成形用粉末的90%粒径为4.0μm或以下。
6.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述成形体的烧成在1250~1450℃的保持温度下进行。
7.根据权利要求2所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体含有换算成SiO2为60~250ppm的Si、以及换算成CaCO3为700~2500ppm的Ca作为第1次要成分。
8.根据权利要求2所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体含有CoO:500~4000ppm、Nb2O5:50~500ppm、ZrO2:50~1000ppm、Ta2O5:50~1000ppm、V2O5:50~1000ppm、HfO2:50~1000ppm、In2O5:50~2000ppm、MoO3:50~1000ppm、Bi2O3:50~1000ppm之中的1种、2种或更多种作为第2次要成分。
9.根据权利要求8所述的MnZn铁氧体的制造方法,其特征在于:所述烧结体至少含有CoO作为所述第2次要成分。
10.根据权利要求8所述的MnZn铁氧体的制造方法,其特征在于:所述烧结体含有CoO、Nb2O5以及ZrO2作为所述第2次要成分。
11.根据权利要求2所述的MnZn铁氧体的制造方法,其特征在于:所述烧结体含有SnO2:500~10000ppm以及TiO2:500~10000ppm之中的1种或2种作为所述第3次要成分。
12.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体的平均晶粒直径为5~35μm。
13.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体在100℃的饱和磁通密度为440mT或以上。
14.根据权利要求1所述的MnZn铁氧体的制造方法,其特征在于:所述烧结体的作为损耗显示最小值的温度的底部温度为85~120℃、且在100kHz、200mT的条件下测得的损耗的最小值为350kW/m3或以下。
15.根据权利要求14所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体在100kHz、200mT的条件下测得的损耗的最小值为320kW/m3或以下。
16.一种MnZn铁氧体的制造方法,其特征在于:该制造方法具有将根据BET法测定的比表面积为2.5~4.0m2/g、50%粒径为0.9~1.5μm、90%粒径为4.0μm或以下的成形用粉末成形为预定形状的成形体的工序、以及在1250~1450℃的保持温度下烧成所述成形体从而得到烧成体的工序。
17.一种MnZn铁氧体的制造方法,其具有将根据BET法测定的比表面积为2.0~5.0m2/g、50%粒径为0.7~2.0μm的成形用粉末成形为预定形状的成形体的工序、以及烧成所述成形体从而得到烧成体的工序,其中所述烧成体的平均晶粒直径为5~35μm、在100℃的饱和磁通密度为440mT或以上,作为损耗显示最小值的温度的底部温度为85~120℃、且在100kHz、200mT的条件下测得的损耗的最小值为320kW/m3或以下。
18.根据权利要求16所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体的主要成分为Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:大于0mol%且不超过4mol%、以及余量实质上是MnO;其中含有换算成SiO2为60~250ppm的Si、以及换算成CaCO3为700~2500ppm的Ca作为第1次要成分;含有CoO:500~4000ppm、Nb2O5:50~500ppm以及ZrO2:50~1000ppm作为第2次要成分。
19.根据权利要求17所述的MnZn铁氧体的制造方法,其特征在于:所述烧成体的主要成分为Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:大于0mol%且不超过4mol%、以及余量实质上是MnO;含有换算成SiO2为60~250ppm的Si、以及换算成CaCO3为700~2500ppm的Ca作为第1次要成分;含有CoO:500~4000ppm、Nb2O5:50~500ppm以及ZrO2:50~1000ppm作为第2次要成分。
20.一种MnZn铁氧体的制造方法,其具有将根据BET法测定的比表面积为2.5~4.0m2/g、50%粒径为0.9~1.5μm、90%粒径为4.0μm或以下的成形用粉末成形为预定形状的成形体的工序、在1250~1450℃的保持温度下烧成所述成形体从而得到烧成体的工序,其中所述烧成体的主要成分为Fe2O3:54~57mol%、ZnO:5~10mol%、NiO:大于0mol%且不超过4mol%、以及余量实质上是MnO;含有换算成SiO2为60~250ppm的Si、以及换算成CaCO3为700~2500ppm的Ca作为第1次要成分;含有CoO:500~4000ppm、Nb2O5:50~500ppm以及ZrO2:50~1000ppm作为第2次要成分;同时所述烧成体的平均晶粒直径为5~35μm,在100℃的饱和磁通密度为440mT或以上,作为损耗显示最小值的温度的底部温度为85~120℃、且在100kHz、200mT的条件下测得的损耗的最小值为320kW/m3或以下。
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EP (1) | EP1560229A3 (zh) |
JP (1) | JP4244193B2 (zh) |
KR (1) | KR100639770B1 (zh) |
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TW (1) | TWI303074B (zh) |
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- 2004-01-30 JP JP2004022453A patent/JP4244193B2/ja not_active Expired - Lifetime
-
2005
- 2005-01-03 TW TW094100084A patent/TWI303074B/zh not_active IP Right Cessation
- 2005-01-10 US US11/035,877 patent/US7294284B2/en not_active Expired - Fee Related
- 2005-01-25 CN CNA2005100057636A patent/CN1649039A/zh active Pending
- 2005-01-28 EP EP05001829A patent/EP1560229A3/en not_active Withdrawn
- 2005-01-29 KR KR1020050008327A patent/KR100639770B1/ko active IP Right Grant
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Also Published As
Publication number | Publication date |
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EP1560229A3 (en) | 2007-12-05 |
JP4244193B2 (ja) | 2009-03-25 |
EP1560229A2 (en) | 2005-08-03 |
HK1080212A1 (zh) | 2006-04-21 |
TW200525559A (en) | 2005-08-01 |
KR20060042892A (ko) | 2006-05-15 |
JP2005213100A (ja) | 2005-08-11 |
US20050167632A1 (en) | 2005-08-04 |
TWI303074B (en) | 2008-11-11 |
KR100639770B1 (ko) | 2006-10-31 |
US7294284B2 (en) | 2007-11-13 |
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