CN106478087A - 一种高频低功耗MnZn铁氧体材料及其制备方法 - Google Patents
一种高频低功耗MnZn铁氧体材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 52
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000470 constituent Substances 0.000 claims abstract description 31
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 14
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 12
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 230000035699 permeability Effects 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000011573 trace mineral Substances 0.000 description 4
- 235000013619 trace mineral Nutrition 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910002974 CaO–SiO2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：52.9‑55.3mol％Fe2O3，7‑10mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.03‑0.35wt％CaCO3、0.005‑0.01wt％SiO2、0.02‑0.1wt％TiO2、0.02‑0.08wt％Bi2O3、0.02‑0.07wt％Nb2O5、0.01‑0.08wt％MoO3中的4种以上。制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别小于380mw/cm3和395mw/cm3，磁导率为1500±25％。
Description
技术领域
本发明涉及软磁铁氧体技术领域，具体涉及一种高频低功耗MnZn铁氧体材料及其制备方法。
背景技术
MnZn铁氧体材料是一种具有高磁导率、高电阻率和低损耗特性的材料，在网络通讯、轨道交通等领域，尤其是在开关电源领域，具有非常广泛的应用。开关电源被广泛应用于工业、民用及军事电子设备的各个领域，是现代电子设备的重要组成部分。电子产品向小型化方向发展的技术趋势，要求开关电源体积小、重量轻、可靠性高，而其核心部件主变压器的体积和重量，是构成开关电源体积和重量的主要部分。根据变压器工作的原理，输出电压与频率成正比(Vm＝KfBmAN)，因此要缩小体积和重量就要提高开关电源工作频率，而制约这一目标实现的关键技术之一就是开关电源用铁氧体材料的高频低损耗技术。随着现代信息产业技术的迅猛发展以及电子设备制造技术的不断更新和完善，磁性元器件市场对高性能开关电源用高频低功耗材料的需求量将越来越大。
MnZn铁氧体材料的电磁性能主要是由材料配方和制备工艺所决定的，该材料配方的一般形式为Mn(1-x)ZnxMyFe2O4，其中，M代表所添加的微量元素，y为添加量，x为锌的含量，理论和实践表明，通过合理的配方和优良的制造工艺，并添加适量的微量元素，可以对铁氧体材料有关电磁性能进行改进。例如，软磁高频功率铁氧体材料的一个重要参数就是在高频下的功率损耗要尽可能的低，适量地添加微量元素可以在铁氧体的晶界处产生高电阻层，进而提高铁氧体材料的整体电阻率，有效降低材料在高频下的涡流损耗，从而获得性能优良的高频低功耗MnZn铁氧体材料。
发明内容
本发明针对现有技术的不足，提供了一种高频低功耗MnZn铁氧体材料及其制备方法。
本发明的目的是通过如下技术方案实现的：
一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：52.9-55.3mol％Fe2O3，7-10mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.03-0.35wt％CaCO3、0.005-0.01wt％SiO2、0.02-0.1wt％TiO2、0.02-0.08wt％Bi2O3、0.02-0.07wt％Nb2O5、0.01-0.08wt％MoO3中的4种以上。
所述MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别小于380mw/cm3和395mw/cm3，磁导率为1500±25％。
一种高频低功耗MnZn铁氧体材料的制备方法，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在800-950℃下预烧2-3h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的7-10％；
5)将环状毛坯置于air/N2气氛烧结炉，在1200-1300℃、氧分压1-5％条件下烧结3-5h，得高频低功耗MnZn铁氧体材料。
根据传统铁磁学理论，铁氧体损耗主要包括磁滞损耗、涡流损耗和剩余损耗三部分。当频率超过200kHz时，涡流损耗超过磁滞损耗在总损耗中占主导地位，成为高频损耗的最主要部分。因此，在保持较低磁滞损耗和剩余损耗的同时尽可能降低涡流损耗是高频低损耗铁氧体材料制备的关键。众所周知，涡流损耗不仅与材料电阻率ρ有关，还与材料的平均晶粒尺寸d有关，即Pe∝d2/ρ。降低涡流损耗的有效方法是添加适量的微量元素，在晶界形成高电阻层，以提高晶界电阻率以及晶粒内的电阻率。目前，国内外普遍采用的方法是用CaO-SiO2作添加剂，因其富集于晶界，能够形成高电阻晶界层，达到降低高频涡流损耗的目的。普通功率铁氧体的烧结温度一般为1300-1400℃，其工作频率低于500KHz。本发明的有益效果：
1.本发明制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别小于380mw/cm3和395mw/cm3，磁导率为1500±25％，节能性好，具有广阔的市场应用前景。
2.本发明的主成分和辅助成分选用和配比合理，制备方法简单易行，常规生产设备即可生产。
具体实施方式
以下结合具体实施方式对本发明作进一步的说明。
实施例1
一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：54.5mol％Fe2O3，7.5mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.06wt％CaCO3、0.005wt％SiO2、0.06wt％TiO2、0.025wt％Bi2O3。
一种高频低功耗MnZn铁氧体材料的制备方法，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在900℃下预烧2.5h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的8％；
5)将环状毛坯置于air/N2气氛烧结炉，在1210℃、氧分压3％条件下烧结4h，得高频低功耗MnZn铁氧体材料。
制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别为355mw/cm3和376mw/cm3，起始磁导率为1450。
实施例2
一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：53.3mol％Fe2O3，8.1mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.055wt％CaCO3、0.007wt％SiO2、0.1wt％TiO2、0.035wt％Bi2O3、0.045wt％Nb2O5。
一种高频低功耗MnZn铁氧体材料的制备方法，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在930℃下预烧2.5h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的8％；
5)将环状毛坯置于air/N2气氛烧结炉，在1270℃、氧分压3％条件下烧结4h，得高频低功耗MnZn铁氧体材料。
制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别为347mw/cm3和371mw/cm3，起始磁导率为1380。
实施例3
一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：52.9mol％Fe2O3，10mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.03wt％CaCO3、0.01wt％SiO2、0.08wt％TiO2、0.08wt％Bi2O3、0.02wt％Nb2O5、0.08wt％MoO3。
一种高频低功耗MnZn铁氧体材料的制备方法，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在800℃下预烧2h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的7％；
5)将环状毛坯置于air/N2气氛烧结炉，在1300℃、氧分压1％条件下烧结5h，得高频低功耗MnZn铁氧体材料。
制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别为372mw/cm3和383mw/cm3，起始磁导率为1410。
实施例4
一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：54.0mol％Fe2O3，9mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.20wt％CaCO3、0.009wt％SiO2、0.02wt％TiO2、0.05wt％Nb2O5、0.01wt％MoO3。
一种高频低功耗MnZn铁氧体材料的制备方法，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在850℃下预烧3h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的9％；
5)将环状毛坯置于air/N2气氛烧结炉，在1200℃、氧分压4％条件下烧结3h，得高频低功耗MnZn铁氧体材料。
制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别为366mw/cm3和391mw/cm3，起始磁导率为1470。
实施例5
一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，主成分为：55.3mol％Fe2O3，7mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.35wt％CaCO3、0.008wt％SiO2、0.04wt％TiO2、0.02wt％Bi2O3、0.07wt％Nb2O5、0.04wt％MoO3。
一种高频低功耗MnZn铁氧体材料的制备方法，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在950℃下预烧2.5h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的10％；
5)将环状毛坯置于air/N2气氛烧结炉，在1250℃、氧分压2％条件下烧结4h，得高频低功耗MnZn铁氧体材料。
制备的高频低功耗MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别为361mw/cm3和379mw/cm3，起始磁导率为1370。
Claims (3)
1.一种高频低功耗MnZn铁氧体材料，由主成分和辅助成分制备得到的，其特征在于，主成分为：52.9-55.3mol％Fe2O3，7-10mol％ZnO，余量为Mn3O4；按主成分总重量计，辅助成分为0.03-0.35wt％CaCO3、0.005-0.01wt％SiO2、0.02-0.1wt％TiO2、0.02-0.08wt％Bi2O3、0.02-0.07wt％Nb2O5、0.01-0.08wt％MoO3中的4种以上。
2.根据权利要求1所述的高频低功耗MnZn铁氧体材料，其特征在于，所述MnZn铁氧体材料在1MHz×50mT条件下，在60℃和80℃的功耗分别小于380mw/cm3和395mw/cm3，起始磁导率为1500±25％。
3.一种权利要求1所述的高频低功耗MnZn铁氧体材料的制备方法，其特征在于，是由以下步骤制备得到的：
1)按比例称取主成分原料，混合均匀，得粉料；
2)将粉料在800-950℃下预烧2-3h；
3)将辅助成分加至预烧后的粉料中，球磨至粒径为1.0-1.5μm；
4)将球磨后的粉料加入有机粘合剂PVA混匀，造粒，压制成型，制得环状毛坯；
所述有机粘合剂PVA的加入量为粉料重量的7-10％；
5)将环状毛坯置于air/N2气氛烧结炉，在1200-1300℃、氧分压1-5％条件下烧结3-5h，得高频低功耗MnZn铁氧体材料。
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