CN112645702B - 一种宽频宽温高磁导率Mn-Zn铁氧体材料及其制备方法与应用 - Google Patents
一种宽频宽温高磁导率Mn-Zn铁氧体材料及其制备方法与应用 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 33
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000011701 zinc Substances 0.000 claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 7
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 6
- 239000011787 zinc oxide Substances 0.000 claims abstract description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 210000001161 mammalian embryo Anatomy 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 21
- 239000002994 raw material Substances 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 3
- 241000625836 Ochrolechia Species 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 2
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明属于铁氧体材料技术领域，特别公开了一种宽频宽温高磁导率Mn‑Zn铁氧体材料及其制备方法与应用。所述铁氧体材料，包括主成分和辅助成分；主成分包括51.5‑53.5mol％氧化铁、氧化锰24.5‑26.8mol％、余量为氧化锌；所述辅助成分相对于主成分的含量为：0～400ppm氧化铋、0～100ppm氧化硅、0～800ppm氧化钼和0～100ppm氧化铌，0～500ppm碳酸钙，所述辅助成分的含量均不为0。主成分和辅助成分配比合理，选择的辅助成分合适，含量适中，该锰‑锌铁氧体材料既具有宽频特性又具有高导磁率的特性。
Description
技术领域
本发明属于铁氧体材料技术领域，特别涉及一种宽频宽温高磁导率Mn-Zn铁氧体材料及其制备方法与应用。
背景技术
随着电子技术的快速发展，电子元件越来越向小型化、高频化发展，在要求高磁导率MnZn铁氧体除了必须具备高的磁导率外,还要求μi-f曲线要宽频且平坦，从而使材料能有较宽的频率和较高的磁导率，使材料具有较高的EMI滤波频率。本发明采用传统的氧化物陶瓷工艺制备MnZn铁氧体材料，通过对主配方、添加剂，搭配合宜的烧结工艺优化研究，开发出具有良好的宽频特性且高磁导MnZn铁氧体材料。
发明内容
为了克服上述现有技术的缺点与不足，本发明的首要目的在于提供一种宽频宽温高磁导率Mn-Zn铁氧体材料。
本发明另一目的在于提供所述宽频宽温高磁导率Mn-Zn铁氧体材料的制备方法。
本发明再一目的在于提供所述宽频宽温高磁导率Mn-Zn铁氧体材料在制备电子元件中的应用。
本发明的目的通过下述方案实现：
一种宽频宽温高磁导率Mn-Zn铁氧体材料，包括主成分和辅助成分；
所述主成分包括51.5-53.5mol％氧化铁、氧化锰24.5-26.8mol％、余量为氧化锌；所述辅助成分相对于主成分的含量为：0～400ppm氧化铋(Bi2O3)、0～100ppm氧化硅(SiO2)、0～800ppm氧化钼(MoO3)和0～100ppm氧化铌(Nb2O5)，0～500ppm碳酸钙(CaCO3)，所述辅助成分的含量均不为0。
优选地，所述辅助成分相对于主成分的含量包括240～270ppm碳酸钙、20～30ppm氧化硅、300～400ppm氧化铋、0～800ppm氧化钼和0～200ppm氧化铌，所述辅助成分的含量均不为0。
一种制备上述宽频宽温高磁导率Mn-Zn铁氧体材料的方法，包括以下步骤：
(1)按照配方依比例混合主成分，然后煅烧，得到煅烧粉末A；
(2)将得到的粉末A与辅助成分、水混合后进行球磨，得到浆料B，再加入PVA得到粉体；
(3)在步骤(2)所得粉体中加入硬脂酸锌，并以固定生胚密度的方式进行压实成型，得到生胚；
(4)将所得生胚进行烧结；依照烧结过程分为升温段、恒温段、降温段，制得最终产物。
步骤(1)所述煅烧的温度为800～900℃，优选为850℃；煅烧的时间为2～10h，优选为6h。
步骤(2)所述球磨的方式为湿式球磨，目标粒径为0.6～1.2μm；优选为0.9μm；依照粉末粒径大小调整研磨时间。
步骤(2)所述水与PVA、浆料B的重量比为2:1:5～12，优选为2:1:8。
步骤(3)所述硬脂酸锌按0.02％～0.05wt.％的比例添加。
步骤(3)所述固定生胚密度具体为3.4±0.2g/cm3。
步骤(4)所述升温段为从室温升至1300～1400℃，升温时间为4～8h；恒温段维持1300～1400℃在氧含量为1～4％中烧结6～12h；降温段从1300～1400℃降至室温，在平衡气氛中进行，速率为3～6℃/min。
所述宽频宽温高磁导率Mn-Zn铁氧体材料在制备电子元件中的应用。
本发明相对于现有技术，具有如下的优点及有益效果：
本发明的锰-锌铁氧体材料由于主成分和辅助成分配比合理，选择的辅助成分合适，含量适中，该锰-锌铁氧体材料既具有宽频特性又具有高导磁率之特性。
附图说明
图1为实施例3和对比例所得产物的起始磁导率随温度的变化。
图2为实施例1-3和对比例所得产物在不同频率的起始磁导率图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。本发明所述室温和未指明的温度为25-32℃。
实施例中所用试剂如无特殊说明均可从市场常规购得。
实施例中宽频宽温高磁导率Mn-Zn铁氧体材料的制备方法如下：
(1)将主成分中的各成分混合后在将其在温度为850℃下预烧6小时，得到粉体A；
(2)将步骤(1)所得粉体A、与辅助成分中各成分混合，得到球磨料B，在球磨料B中加入去离子水进行球磨，得到平均粒径为0.9μm的浆料B，在浆料B中加入聚乙烯醇溶液，搅拌，得到粉体B，所述聚乙烯醇溶液和浆料B的重量比为1：8。
(3)在步骤(2)所得粉体B中加入0.02～0.05％的硬脂酸锌，然后进行压制成型，得到生坯，固定生胚密度具体为3.4±0.2g/cm3。
(4)将步骤(3)所得生坯在特定曲线烧结：升温阶段：25℃～1380℃，在空气中升温6个小时；保温阶段：1380℃，氧含量2％，保温8个小时；降温阶段：1300℃～25℃，在平衡气氛中降温，速率为4.5℃/min，得到所述宽频宽温高磁导率Mn-Zn铁氧体材料。
实施例1
一种宽频宽温高磁导率Mn-Zn铁氧体材料，包括主成分和辅助成分；主原料的组分为含有51.5wt％的按Fe2O3计算的氧化铁，24.5wt％的按Mn3O4计算的氧化锰，其余为氧化锌；所述的辅助原料的组分相对于主成分为含有300ppm的按CaCO3计算的氧化钙，50ppm的按SiO2计算的氧化硅，350ppm的按Bi2O3计算的氧化铋，700ppm的按MoO3计算的氧化钼，10ppm的按Nb2O5计算的氧化铌。
实施例2
一种宽频宽温高磁导率Mn-Zn铁氧体材料，包括主成分和辅助成分；主原料的组分为含有52.5wt％的按Fe2O3计算的氧化铁，25.5wt的按Mn3O4计算的氧化锰，其余为氧化锌；所述的辅助原料的组分相对于主成分为含有400ppm的按CaCO3计算的氧化钙，25ppm的按SiO2计算的氧化硅，300ppm的按Bi2O3计算的氧化铋，600ppm的按MoO3计算的氧化钼，5ppm的按Nb2O5计算的氧化铌。
实施例3
一种宽频宽温高磁导率Mn-Zn铁氧体材料，包括主成分和辅助成分；主原料的组分为含有53.5wt％的按Fe2O3计算的氧化铁，26.8wt％的按Mn3O4计算的氧化锰，其余为氧化锌；所述的辅助原料的组分相对于主成分为含有500ppm的按CaCO3计算的氧化钙，10ppm的按SiO2计算的氧化硅，300ppm的按Bi2O3计算的氧化铋，600ppm的按MoO3计算的氧化钼，10ppm的按Nb2O5计算的氧化铌。
由本发明的实施例1至3和对比例得到的宽频高导磁率.高居礼温度锰-锌铁氧体材料经测试具有下表所示的技术效果。其中对比例为目前高导宽频材质行业的一般性能。
表1
本发明所得材料的起始磁导率大于13000(25℃)，而且在5℃～125℃范围内起始磁导率大于10000，如图1。另在10kHz～100kHz范围内起始磁导率大于13000μi；200kHz起始磁导率大于11000μi；截止频率大于850KHz，如图2，同时还具有材料磁滞常数ηB小于0.5×10<-6>/mT(-25℃，B1＝1.5mT，B2＝3mT)。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (9)
1.一种宽频宽温高磁导率Mn-Zn铁氧体材料，其特征在于包括主成分和辅助成分；
所述主成分包括53.5mol％氧化铁、氧化锰26.8mol％、余量为氧化锌；所述辅助成分相对于主成分的含量为：300ppm氧化铋、10ppm氧化硅、600ppm氧化钼和10ppm氧化铌，500ppm碳酸钙；
所述氧化铁具体地为Fe2O3；所述氧化锰具体地为Mn3O4。
2.一种制备权利要求1所述宽频宽温高磁导率Mn-Zn铁氧体材料的方法，其特征在于包括以下步骤：
(1)按照配方依比例混合主成分，然后煅烧，得到煅烧粉末A；
(2)将得到的粉末A与辅助成分、水混合后进行球磨，得到浆料B，再加入PVA得到粉体；
(3)在步骤(2)所得粉体中加入硬脂酸锌，并以固定生胚密度的方式进行压实成型，得到生胚；
(4)将所得生胚进行烧结；依照烧结过程分为升温段、恒温段、降温段，制得最终产物。
3.根据权利要求2所述的方法，其特征在于：步骤(1)所述煅烧的温度为800～900℃；煅烧的时间为2～10h。
4.根据权利要求2所述的方法，其特征在于：步骤(2)所述水与PVA、浆料B的重量比为2：1：5～12。
5.根据权利要求2所述的方法，其特征在于：步骤(2)所述球磨的方式为湿式球磨，目标粒径为0.6～1.2μm。
6.根据权利要求2所述的方法，其特征在于：步骤(3)所述硬脂酸锌按0.02％～0.05wt.％的比例添加。
7.根据权利要求2所述的方法，其特征在于：步骤(3)所述固定生胚密度具体为3.4±0.2g/cm3。
8.根据权利要求2所述的方法，其特征在于：步骤(4)所述升温段为从室温升至1300～1400℃，升温时间为4～8h；恒温段维持1300～1400℃在氧含量为1～4％中烧结6～12h；降温段从1300～1400℃降至室温，在平衡气氛中进行，速率为3～6℃/min。
9.根据权利要求1所述宽频宽温高磁导率Mn-Zn铁氧体材料在制备电子元件中的应用。
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