CN117383924A - 一种宽频高阻抗高磁导率锰锌软磁铁氧体及其制备方法 - Google Patents
一种宽频高阻抗高磁导率锰锌软磁铁氧体及其制备方法 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 title claims description 16
- 239000000463 material Substances 0.000 claims abstract description 38
- 238000000227 grinding Methods 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 17
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 13
- 238000000748 compression moulding Methods 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims description 36
- 230000035699 permeability Effects 0.000 claims description 26
- 239000004615 ingredient Substances 0.000 claims description 14
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- 238000007873 sieving Methods 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 239000000696 magnetic material Substances 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 24
- 239000011572 manganese Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 239000002075 main ingredient Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
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- 229910001004 magnetic alloy Inorganic materials 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
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- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 229910001035 Soft ferrite Inorganic materials 0.000 description 1
- FHKPLLOSJHHKNU-INIZCTEOSA-N [(3S)-3-[8-(1-ethyl-5-methylpyrazol-4-yl)-9-methylpurin-6-yl]oxypyrrolidin-1-yl]-(oxan-4-yl)methanone Chemical compound C(C)N1N=CC(=C1C)C=1N(C2=NC=NC(=C2N=1)O[C@@H]1CN(CC1)C(=O)C1CCOCC1)C FHKPLLOSJHHKNU-INIZCTEOSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于磁性材料技术领域，本发明提供了一种宽频高阻抗高磁导率锰锌软磁铁氧体及其制备方法，该材料包含主成分和辅助成分，主成分为Fe2O3、ZnO、Mn3O4，辅助成分包括：纳米CaCO3、纳米Bi2O3、纳米Nb2O5、SiO2。该材料的制备方法包括配料、混合、预烧、研磨、造粒、压制成型和放电等离子烧结，通过主成分、辅助成分和工艺方法的整体控制，制备得到的软磁铁氧体具备高阻抗、高磁导率的特性。
Description
技术领域
本发明属于磁性材料技术领域，具体涉及宽频高阻抗高磁导率软磁铁氧体及其制备方法。
背景技术
宽频、高阻抗、高磁导率锰锌铁氧体材料作为抗电磁干扰的主要材料，其用量近年来迅速增加。谐振电感作为常见的抗电磁干扰材料，主要应用在抑制电磁干扰、提高信号质量和稳定性等方面，不仅要求其具有高的初始磁导率、并在定频率范围内保持磁导率不变(宽频要求)和相应的阻抗特性要求。但是软磁铁氧体材料随着频率的增加会引起频散与吸收，频率升到一定值时材料的磁导率会急剧的下降。每种材质都存在着截止频率的问题，要使其在宽频范围中的高频段具有高阻抗高磁导率特性，尤其是谐振电感常用的 350KHz频率，就必须提高截止频率。故需要研究宽频高阻抗高磁导率软磁铁氧体及其制备方法。
现有技术例如公告号为CN1677579B的专利公开了一种宽频锰锌系高磁导率软磁铁氧体材料及其制备方法，所诉为软磁铁氧体粉料加入添加剂在1300℃氮气保护下进行烧结，获得了一种宽频高磁导率的材料，其核心是以低温烧结配合添加剂达到截止频率更高的目的，但其制备的样品磁导率较低，并不涉及通过不同的烧结方式，来达到高的磁粉烧结温度使其晶粒均匀长大，提供高的磁性能。公告号为CN102651264B的专利公开了一种烧结复合软磁材料及制备该材料的方法，其所诉材料为金属软磁、软磁铁氧体和低熔点的软磁合金所组成，其低熔点的软磁合金为机械破碎得到的颗粒粒径较大，且熔点在1000℃到1200℃，由上述成分组成材料配合放电等离子烧结技术得到该软磁材料， 但其并不涉及在单一软磁铁氧体粉末中加入低熔点物质纳米氧化铋，颗粒粒径为纳米级，熔点在817℃，配合放电等离子烧结技术在更低温度下形成液态相，晶粒生长过程加快，提高磁性能的问题。
为解决以上问题：我们通过合理的掺杂、砂磨及烧结工艺，提高材料磁导率，改善材料频率特性，制备得到一种宽频高阻抗高磁导率的锰锌软磁铁氧体。
发明内容
为了解决以上问题，本发明提供了一种宽频高阻抗高磁导率锰锌软磁铁氧体及其制备方法。本发明的具体技术方案为：一种宽频高阻抗高磁导率的锰锌铁氧体材料包含主成分和辅助成分，所述主成分按照摩尔比计，包括Fe2O3：50mol%～55mol%，ZnO：25mol%～28mol%，其余为Mn3O4；所述辅助成分包括：纳米CaCO3：300ppm～800ppm、纳米Bi2O3：200ppm～500ppm、纳米Nb2O5：100ppm～400ppm、SiO2：0ppm～200ppm。本发明通过对磁性材料配方的改善以及对制备工艺进行优化后，使得起始磁导率μi≥13000，且350kHz时，磁导率μi≥10000，截止频率fr≥450KHz，阻抗也得到了一定的提升。
上述宽频高阻抗高磁导率锰锌软磁铁氧体及其制备方法，包括如下步骤：
步骤1：按照主成分配比进行配料，Fe2O3：50mol%～55mol%，ZnO：25mol%～28mol%，其余为Mn3O4；
步骤2：将步骤1的配料进行湿法球磨混合；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为700℃～1000℃；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：300ppm～800ppm、纳米Bi2O3：200ppm～500ppm、纳米Nb2O5：100ppm～400ppm、SiO2：0ppm～200ppm，用珠磨机将其研磨，其中，可以用CuO或MoO3代替纳米Bi2O3作为辅助成分，CuO含量为0-400ppm，MoO3含量为100-500ppm；
步骤5：通过造粒、研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成环形生坯，密度为3.15 g/cm3～3.35g/cm3；
步骤7：烧结，采用放电等离子烧结技术，烧结温度在1300℃至1400℃，然后冷却至100℃出炉。
上述步骤2中，配料混合时间为10min～40min；
上述步骤3中，预烧升温速率为3℃/min～5℃/min，保温1h～3h；
上述步骤4中，纳米CaCO3：400ppm～600ppm、纳米Bi2O3：300ppm～400ppm、纳米Nb2O5：100ppm～200ppm、SiO2：0ppm～50ppm，珠磨机研磨时间在1小时到2小时之间；
上述步骤4中，若用CuO或MoO3代替纳米Bi2O3作为辅助成分，CuO含量为100ppm，MoO3含量为200ppm;
上述步骤5中，在步骤4得到的粉料中加入3wt％～20wt％聚乙烯醇，研磨过筛得到的颗粒尺寸在0.1mm到0.4mm之间；
上述步骤7中，烧结升温速率为20℃/min～50℃/min，保温10min～20min。
使用放电等离子烧结技术（sps）：放电等离子烧结是基于脉冲放电初期粉体间产生的火花放电现象（瞬间产生高温等离子体），通过瞬时高温场实现致密化的快速烧结工艺。本发明在辅助成分中含有低熔点杂质纳米Bi2O3，使原来的纯固相烧结变为有液相参与的烧结，而放电等离子烧结与传统烧结不同，它是利用脉冲大电流直接施加于模具和样品，产生体热，从而实现快速烧结，二者结合可以更好的形成大晶粒提高磁导率，纳米CaCO3等其他杂质可以使得晶粒均匀生长，通过配方与烧结的相互配合，达到改善材料微观组织，提高材料致密性的目的。
其具体性能提升为：在8mV，10kHz条件下，磁导率μi≥13000；100kHz条件下，磁导率μi≥12000；350kHz时，磁导率μi≥10000；截止频率fr≥450KHz；频率在100kHz时，阻抗系数ZN≥8Ω/mm；200kHz时，阻抗系数ZN≥18Ω/mm；350KHz时，阻抗系数ZN≥25Ω/mm；500kHz时，阻抗系数ZN≥35Ω/mm，100℃时饱和磁感应强度Bs≥250mT，居里温度Tc≥130℃。
具体实施方式
下面通过具体的实施案例，对本发明所制备的宽频高阻抗高磁导率软磁铁氧体及其制备方法进一步进行说明。
实施例1：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，Fe2O3：53.1mol%，ZnO：25.5mol%和其余的Mn3O4配料；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为850℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：600ppm、纳米Bi2O3：300ppm、纳米Nb2O5：200ppm、SiO2：100ppm，用珠磨机将其研磨80min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用放电等离子烧结技术（sps），烧结温度在1380℃，升温速率为50℃/min，保温20min，然后冷却至100℃出炉。
实施例2：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，采用和实施例1相同的主成分配方；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为900℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：800ppm、纳米Bi2O3：200ppm、纳米Nb2O5：200ppm、SiO2：150ppm，用珠磨机将其研磨80min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用放电等离子烧结技术（sps），烧结温度在1400℃，升温速率为50℃/min，保温20min，然后冷却至100℃出炉。
实施例3：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，Fe2O3：52.8mol%，ZnO：25.8mol%和其余的Mn3O4配料；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为850℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：600ppm、纳米Bi2O3：300ppm、纳米Nb2O5：200ppm、SiO2：100ppm，用珠磨机将其研磨80min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用放电等离子烧结技术（sps），烧结温度在1380℃，升温速率为50℃/min，保温20min，然后冷却至100℃出炉。
比较例1：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，Fe2O3：53.1mol%，ZnO：25.5mol%和其余的Mn3O4配料；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为850℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：600ppm、纳米Bi2O3：300ppm、纳米Nb2O5：200ppm、SiO2：100ppm，用珠磨机将其研磨80min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用钟罩炉进行烧结，烧结温度为1380℃，氧含量为4%，保温6h。
比较例2：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，采用和比较例1相同的主成分配方；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为900℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：800ppm、纳米Bi2O3：200ppm、纳米Nb2O5：200ppm、SiO2：150ppm，用珠磨机将其研磨90min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用钟罩炉进行烧结，烧结温度为1400℃，氧含量为5%，保温6h。
比较例3：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，Fe2O3：53.3mol%，ZnO：25.3mol%和其余的Mn3O4配料；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为850℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：600ppm、纳米Bi2O3：300ppm、纳米Nb2O5：200ppm、SiO2：100ppm，用珠磨机将其研磨90min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用钟罩炉进行烧结，烧结温度为1400℃，氧含量为4%，保温5h。
比较例4：一种宽频高阻抗高磁导率锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：
步骤1：按照主成分配比进行配料，采用和实施例1相同的主成分配方；
步骤2：将步骤1的配料进行湿法球磨混合，混合时间为20min；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为850℃，升温速率为5℃/min，保温2h；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：600ppm、纳米Nb2O5：200ppm、SiO2：100ppm，用珠磨机将其研磨80min；
步骤5：造粒，根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成尺寸为环形生坯，密度为3.2g/cm3；
步骤7：烧结，使用放电等离子烧结技术（sps），烧结温度在1380℃，升温速率为50℃/min，保温20min，然后冷却至100℃出炉。
实施例与比较例在不同频率下磁导率测试结果如下表1：
表1 实施例与比较例在不同频率下磁导率测试结果
| 频率f（Hz） | 10k | 100k | 200k | 350k |
| 实施例1 | 13780 | 14696 | 12738 | 10523 |
| 实施例2 | 13223 | 13823 | 12221 | 10097 |
| 实施例3 | 12794 | 13648 | 12043 | 9591 |
| 比较例1 | 11754 | 12400 | 11197 | 9161 |
| 比较例2 | 10548 | 11077 | 10372 | 8873 |
| 比较例3 | 10490 | 11132 | 9919 | 7992 |
| 比较例4 | 11279 | 11897 | 10891 | 9055 |
实施例与比较例在不同频率下阻抗系数测试结果如下表2：
表2 实施例与比较例在不同频率下阻抗系数测试结果
| 频率f（Hz） | 100k | 200k | 350k | 500k |
| 实施例1 | 12 | 24 | 31 | 43 |
| 实施例2 | 11 | 21 | 28 | 38 |
| 实施例3 | 12 | 23 | 30 | 41 |
| 比较例1 | 10 | 20 | 28 | 37 |
| 比较例2 | 8 | 17 | 24 | 34 |
| 比较例3 | 8 | 16 | 22 | 31 |
| 比较例4 | 9 | 19 | 28 | 38 |
通过对比实施例1与比较例1、实施例2与比较例2表明：实施例与比较例关键区别是是否采用放电等离子烧结工艺（sps），等离子烧结工艺相比于传统烧结，利用脉冲大电流直接施加于模具和样品，产生体热，辅助成分中含有低熔点杂质纳米Bi2O3，使原来的纯固相烧结变为有液相参与的烧结，二者结合从而实现快速烧结，可以更好的形成大晶粒提高磁导率，材料性能有了明显提升；通过对比实施例1与比较例4表明：低熔点杂质配合放电等离子烧结技术可以使得晶粒均匀生长，达到改善材料微观组织，提高材料磁性能的目的；通过对比实施例1与实施例3、比较例2与比较例3表明：烧结工艺相同时，不同的配方与预烧工艺，对材料的磁导率、频率特性及阻抗特性有极大影响。以上数据表明比较例起始磁导率相对较低都在12000以下，而实施例起始磁导率可达13000以上，并且在350KHz实施例磁导率远高于比较例，且对比阻抗系数，实施例相对比较例也有了明显的提高。
以上所述仅为本发明的一些实施方式，但本发明的保护范围并不局限于此。
Claims (7)
1.一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，包括以下步骤：
步骤1：按照主成分配比进行配料，Fe2O3：50mol%～55mol%，ZnO：25mol%～28mol%，其余为Mn3O4；
步骤2：将步骤1的配料进行湿法球磨混合；
步骤3：预烧，对步骤2中所得混合料烘干后进行预烧，预烧温度为700℃～1000℃；
步骤4：砂磨，将步骤3所得的预烧料中加入辅助成分：纳米CaCO3：300ppm～800ppm、纳米Bi2O3：200ppm～500ppm、纳米Nb2O5：100ppm～400ppm、SiO2：0ppm～200ppm，用珠磨机将其研磨，其中，可以用CuO或MoO3代替纳米Bi2O3作为辅助成分，CuO含量为0-400ppm，MoO3含量为100-500ppm；
步骤5：通过造粒、研磨过筛成一定尺寸的颗粒；
步骤6：压制成型，压制成环形生坯，密度为3.15 g/cm3～3.35g/cm3；
步骤7：烧结，采用放电等离子烧结技术，烧结温度在1300℃至1400℃，然后冷却至100℃出炉。
2.如权利要求1所述的一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，所述步骤2中，配料混合时间为10min～40min。
3.如权利要求1所述的一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，所述步骤3中，预烧升温速率为3℃/min～5℃/min，保温1h～3h。
4.如权利要求1所述的一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，所述步骤4中，纳米CaCO3：400ppm～600ppm、纳米Bi2O3：300ppm～400ppm、纳米Nb2O5：100ppm～200ppm、SiO2：0ppm～50ppm，珠磨机研磨时间在1小时到2小时之间。
5.如权利要求1所述的一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，所述步骤4中，若用CuO或MoO3代替所述纳米Bi2O3作为辅助成分，则CuO含量为100ppm，MoO3含量为200ppm。
6.如权利要求1所述的一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，所述步骤5中，在步骤4得到的粉料中加入3wt％～20wt％聚乙烯醇，研磨过筛得到的颗粒尺寸在0.1mm到0.4mm之间。
7.如权利要求1所述的一种宽频高阻抗高磁导率锰锌软磁铁氧体的制备方法，其特征在于，所述步骤7中，烧结升温速率为20℃/min～50℃/min，保温10min～20min。
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| CN112723873A (zh) * | 2021-02-05 | 2021-04-30 | 天通控股股份有限公司 | 一种宽频高阻抗高磁导率MnZn软磁铁氧体及其制备方法 |
| WO2023029255A1 (zh) * | 2021-09-03 | 2023-03-09 | 天通控股股份有限公司 | 一种汽车电子用宽温高磁导率锰锌软磁铁氧体及制备方法 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107473727A (zh) * | 2017-09-21 | 2017-12-15 | 郴州市久隆旺高科电子有限公司 | 一种宽频宽温高功率密度低损耗锰锌软磁铁氧体材料及其制备方法 |
| CN112723873A (zh) * | 2021-02-05 | 2021-04-30 | 天通控股股份有限公司 | 一种宽频高阻抗高磁导率MnZn软磁铁氧体及其制备方法 |
| WO2023029255A1 (zh) * | 2021-09-03 | 2023-03-09 | 天通控股股份有限公司 | 一种汽车电子用宽温高磁导率锰锌软磁铁氧体及制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 徐仲达;: "宽频高阻抗锰锌铁氧体材料工艺技术的探讨", 中国陶瓷工业, no. 05, 15 October 2016 (2016-10-15), pages 28 - 30 * |
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