CN111892395A - 一种高频高阻抗锰锌铁氧体材料及其制备方法 - Google Patents
一种高频高阻抗锰锌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 57
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 21
- 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 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 42
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 24
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 21
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 11
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical group O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 3
- 208000032365 Electromagnetic interference Diseases 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910003962 NiZn Inorganic materials 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011361 granulated particle Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000004883 computer application Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明涉及软磁铁氧体技术领域,尤其是一种高频高阻抗锰锌铁氧体材料及其制备方法,其主成份以氧化物计算由Fe2O3:48~49.7mol%,MnO:29~33mol%,ZnO:19~21mol%,Co2O3:0.03~0.08mol%组成;按主成分重量计的副成分包括Nb2O5:0.01~0.05wt%、CaCO3:0.02~0.05wt%,SnO2:0.01~0.08wt%、Bi2O3:0.01~0.06wt%,MoO3:0.01~0.05wt%中的至少三种。该高频高阻抗锰锌铁氧体材料的制备方法采用的工艺步骤是:配料、预烧、砂磨、造粒、成型、烧结。与现有技术相比,本材料具有高频高阻抗、高居里温度、价格低廉等优良特性,可以满足电子设备对EMI的高需求。
Description
技术领域
本发明涉及软磁铁氧体领域,具体领域为一种锰锌铁氧体材料。
背景技术
在电子信息时代,随着卫星通信、移动通信、计算机应用等的高速发展,电磁干扰(EMI)在军事和民用电子信息领域的影响越来越严重,对公共环境和人身安全以及信息保密造成了很大的危害。解决或降低电磁污染和提高电子设备抗EMI能力的有效办法是采用电磁兼容(EMC)设计,其中需用到大量抗EMI材料,即高阻抗材料。随着各国有关电磁兼容法律法规的健全,特别是车载电子的滤波需求,频率提升到100MHz,100MHz高频抗EMI材料铁氧体磁芯的需求量与日俱增。
高导材料因为具有较高的起始磁导率,被广泛应用在EMI中,但其应用频率主要集中在1MHz以下,25MHz和100MHz下阻抗较低,难以满足未来的需求发展。目前高频EMI主要使用的是NiZn材料,但其磁导率难以达到2500以上,并且其价格昂贵,居里温度和饱和磁通密度都较低。
为了应对EMI对材料越来越高的特性需求,需要综合材料的特性:高磁导率、高居里温度、高频高阻抗、高饱和磁通密度等。
发明内容
为了解决上述技术难题,本发明提供一种磁导率3000的高频高阻抗锰锌铁氧体材料及其制备方法。
为实现上述目的,本发明提供如下技术方案:
一种高频高阻抗锰锌铁氧体材料,由主成分和副成分组成,所述主成份以氧化物计算,由Fe2O3:48~49.7mol%,MnO:29~33mol%,ZnO:19~21mol%,Co2O3:0.03~0.08mol%组成;按主成分重量计的副成分包括Nb2O5:0.01~0.05wt%、CaCO3:0.02~0.05wt%,SnO2:0.01~0.08wt%、Bi2O3:0.01~0.06wt%,MoO3:0.01~0.05wt%中的至少三种。
进一步的,所述主成分由Fe2O3:49~49.7mol%,MnO:29~32mol%,ZnO:19~20mol%,Co2O3:0.05~0.08mol%组成。
该高频高阻抗锰锌铁氧体材料的制备方法,包括以下步骤:
1)配料:按照主成分Fe2O3、MnO、ZnO、Co2O3的比例进行称量并混合砂磨,砂磨时间15min~30min;
2)预烧:将混合后的粉料进行预烧,预烧温度850℃~1050℃;
3)砂磨:将副组分加入预烧料进行二次混合处理,砂磨时间为40~70min,粒径为1.3μm~2.0μm;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯T25*15*7.5;
6)烧结:将毛坯在推板窑炉中烧结,烧结温度1270-1300℃。
进一步的,步骤6)中所述的烧结温度为1280~1300℃。
与现有技术相比,本发明的有益效果是:
本发明通过成分的选择,优化烧结工艺,制得的锰锌铁氧体材料的起始磁导率可达到3000,居里温度在130℃以上,25MHz阻抗(线径0.5mm*长度165mm,1Ts)达到50Ω,100MHz阻抗达到120Ω,具有较高的高频阻抗,并且可以在推板窑烧结,成本低。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种高频高阻抗锰锌铁氧体材料,由主成分和副成分组成,所述主成分为Fe2O3:48.5mol%,MnO:31mol%,ZnO:20mol%,Co2O3:0.05mol%,副成分为Nb2O5:0.02wt%、CaCO3:0.03wt%、SnO2:0.04wt%,以上副成分按Fe2O3、MnO、ZnO、Co2O3总重量百分比进行计算。
其制备方法包括如下步骤:
1)配料:按照主成分Fe2O3、MnO、ZnO、Co2O3的比例进行称量并混合砂磨,砂磨时间为15min;
2)预烧:将混合后的粉料进行预烧,预烧温度为900℃,保温2h;
3)砂磨:将副组分加入预烧料中进行二次混合处理,砂磨时间为40min,粒径为2.0μm;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯T25*15*7.5;
6)烧结:将毛坯在推板窑炉中进行烧结,烧结温度为1300℃。
实施例2
一种高频高阻抗锰锌铁氧,由主成分和副成分组成,主成分为Fe2O3:49.5mol%,MnO:30.6mol%,ZnO:19.5mol%,Co2O3:0.04mol%;副成分为Nb2O5:0.03wt%、SnO2:0.04wt%,MoO3:0.02wt%,以上副成分按Fe2O3、ZnO、MnO、Co2O3总重量百分比进行计算。
其制备方法包括如下步骤:
1)配料:按照主成分Fe2O3、MnO、ZnO、Co2O3的比例进行称量并混合砂磨,砂磨时间为20min;
2)预烧:将混合后的粉料进行预烧,预烧温度为900℃,保温2h;
3)砂磨:将副组分加入预烧料进行二次混合处理,砂磨时间为50min,粒径为1.7μm;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯T25*15*7.5;
6)烧结:将毛坯推板窑炉中进行烧结,烧结温度为1300℃。
实施例3
一种高频高阻抗锰锌铁氧体材料,由主成分和副成分组成,主成分为Fe2O3:49.7mol%,MnO:29.6mol%,ZnO:20mol%,Co2O3:0.07mol%;副成分为CaCO3:0.02wt%,Bi2O3:0.02wt%,SnO2:0.05wt%,MoO3:0.03wt%,以上副成分按Fe2O3、ZnO、MnO、Co2O3总重量百分比进行计算。
其制备方法包括如下步骤:
1)配料:按照主成分Fe2O3、MnO、ZnO、Co2O3的比例进行称量并混合砂磨,砂磨时间为15min;
2)预烧:将混合后的粉料进行预烧,预烧温度为1000℃,保温2h;
3)砂磨:将副组分加入预烧料中先振磨后再进行二次混合处理,砂磨时间为60min;粒径为1.45μm;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯T25*15*7.5;
6)烧结:将毛坯推板窑炉中进行烧结,烧结温度为1280℃。
实施例4
一种高频高阻抗锰锌铁氧体材料,由主成分和副成分组成,主成分为Fe2O3:49mol%,MnO:30.5mol%,ZnO:19.0mol%,Co2O3:0.05mol%;副成分为Nb2O5:0.04wt%,CaCO3:0.02wt%,SnO2:0.05wt%,MoO3:0.03wt%,以上副成分按Fe2O3、MnO、ZnO、Co2O3总重量百分比进行计算。
其制备方法包括如下步骤:
1)配料:按照主成分Fe2O3、MnO、ZnO、Co2O3的比例进行称量并混合砂磨,砂磨时间为15min;
2)预烧:将混合后的粉料进行预烧,预烧温度为1000℃,保温2h;
3)砂磨:将副组分加入预烧料中进行二次混合处理,砂磨时间为70min,粒径为1.30μm;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯T25*15*7.5;
6)烧结:将毛坯推板窑炉中进行烧结,烧结温度为1300℃。
为突出本发明的有益效果,还进行了以下对比例实验。
对比例1
一种锰锌铁氧体材料,主成分选择Fe2O3:47.0mol%,MnO:35mol%,ZnO:18.0mol%;副成分选择Nb2O5:0.04wt%、CaCO3:0.05wt%、SnO2:0.04wt%,Co2O3:0.05wt%,以上副成分按Fe2O3、ZnO、MnO的总重量百分比进行计算。
其制备方法包括如下步骤:
1)配料:按照主成分Fe2O3、ZnO、MnO的比例进行称量并混合砂磨,砂磨时间为15min;
2)预烧:将混合后的粉料进行预烧,预烧温度为900℃,保温2h;
3)砂磨:将副组分加入预烧料中进行二次混合处理,砂磨时间为60min;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯,
6)烧结:将毛坯在推板窑炉中烧结,烧结温度为1300℃。
对比例2
一种锰锌铁氧体材料,主成分为Fe2O3:49.5mol%,MnO:30.5mol%,ZnO:19.0mol%,副成分为Nb2O5:0.05wt%,CaCO3:0.02wt%,SnO2:0.04wt%,MoO3:0.03wt%,以上副成分按Fe2O3、ZnO、MnO总重量百分比进行计算。
其制备方法包括如下步骤:
1)配料:按照主配方Fe2O3、ZnO、MnO的比例进行称量并混合砂磨,砂磨时间为15min;
2)预烧:将混合后的粉料进行预烧,预烧温度为1000℃,保温2h;
3)砂磨:将副组分加入预烧料中进行二次混合处理,砂磨时间为70min;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯;
6)烧结:将毛坯在推板窑炉中进行烧结,烧结温度为1320℃。
将实施例1-4和对比例1-2制备的标准样环性能测试结果对比如下表。
以上结果显示:本发明的锰锌铁氧体材料具有高频高阻抗特性,适应电子、通讯领域对滤波器材料需求,并且具有较高的饱和磁通密度等优势。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (8)
1.一种高频高阻抗锰锌铁氧体材料,其特征在于:由主成分和副成分组成,所述主成份以氧化物计算,由Fe2O3:48~49.7mol%,MnO:29~33mol%,ZnO:19~21mol%,Co2O3:0.03~0.08mol%组成;按主成分重量计的副成分包括Nb2O5:0.01~0.05wt%、CaCO3:0.02~0.05wt%,SnO2:0.01~0.08wt%、Bi2O3:0.01~0.06wt%,MoO3:0.01~0.05wt%中的至少三种。
2.根据权利要求1所述的高频高阻抗锰锌铁氧体材料,其特征在于:所述主成分由Fe2O3:49~49.7mol%,MnO:29~32mol%,ZnO:19~20mol%,Co2O3:0.05~0.08mol%组成。
3.根据权利要求1所述的高频高阻抗锰锌铁氧体材料,其特征在于:所述主成分为Fe2O3:48.5mol%,MnO:31mol%,ZnO:20mol%,Co2O3:0.05mol%;所述副成分为Nb2O5:0.02wt%、CaCO3:0.03wt%、SnO2:0.04wt%,以上副成分按Fe2O3、MnO、ZnO、Co2O3总重量百分比进行计算。
4.根据权利要求1所述的高频高阻抗锰锌铁氧体材料,其特征在于:所述主成分为Fe2O3:49.5mol%,MnO:30.6mol%,ZnO:19.5mol%,Co2O3:0.04mol%;所述副成分为Nb2O5:0.03wt%、SnO2:0.04wt%,MoO3:0.02wt%,以上副成分按Fe2O3、MnO、ZnO、Co2O3总重量百分比进行计算。
5.根据权利要求2所述的高频高阻抗锰锌铁氧体材料,其特征在于:所述主成分为Fe2O3:49.7mol%,MnO:29.6mol%,ZnO:20mol%,Co2O3:0.07mol%;所述副成分为CaCO3:0.02wt%,Bi2O3:0.02wt%,SnO2:0.05wt%,MoO3:0.03wt%,以上副成分按Fe2O3、ZnO、MnO、Co2O3总重量百分比进行计算。
6.根据权利要求2所述的高频高阻抗锰锌铁氧体材料,其特征在于:所述主成分为Fe2O3:49mol%,MnO:30.5mol%,ZnO:19.0mol%,Co2O3:0.05mol%;所述副成分为Nb2O5:0.04wt%、CaCO3:0.02wt%、SnO2:0.05wt%、MoO3:0.03wt%,以上副成分按Fe2O3、MnO、ZnO、Co2O3总重量百分比进行计算。
7.权利要求1-6任一所述的高频高阻抗锰锌铁氧体材料的制备方法,其特征在于,包括以下步骤:
1)配料:按照主成分Fe2O3、MnO、ZnO、Co2O3的比例进行称量并混合砂磨,砂磨时间15min~30min;
2)预烧:将混合后的粉料进行预烧,预烧温度850℃~1050℃;
3)砂磨:将副组分加入预烧料进行二次混合处理,砂磨时间为40~70min,粒径1.3μm~2.0μm;
4)造粒:将砂磨后的料浆烘干后进行造粒;
5)成型:将造粒好的颗粒进行压制得到需要的毛坯T25*15*7.5;
6)烧结:将毛坯在推板窑炉中烧结,烧结温度1270-1300℃。
8.根据权利要求7所述的高频高阻抗锰锌铁氧体材料的制备方法,其特征在于:步骤6)中所述的烧结温度为1280~1300℃。
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