CN113024239A - 一种宽温超低损耗锰锌铁氧体材料及其制备方法 - Google Patents
一种宽温超低损耗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 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 15
- 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 15
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 28
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 10
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 15
- 238000005469 granulation Methods 0.000 claims description 11
- 230000003179 granulation Effects 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000654 additive Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000000465 moulding Methods 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000013473 artificial intelligence Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
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Abstract
本发明公开了一种宽温超低损耗锰锌铁氧体材料及其制备方法,所述材料的原料包括主成分和辅助成分;所述主成分含量以氧化物百分比计为:Fe2O3为50~52mol%、ZnO为10~12mol%、其余为MnO,主成分配方的总量为100%;按占主成分总重量计,辅助成分为:CaO 200~600ppm、ZrO2 200~400ppm、Co2O33000~10000ppm、SiO220~100ppm、Nb2O5200~400ppm、SnO2400ppm~800ppm或TiO2300~600ppm中的任意五种或以上组合;解决了现有技术的锰锌软磁铁氧体材料高低温损耗都高于310kW/m3等问题。
Description
技术领域
本发明属于软磁铁氧体材料制备技术领域,尤其涉及一种宽温超低损耗锰锌铁氧体材料及其制备方法。
背景技术
软磁铁氧体材料是电子元器件中的主要材料之一,是各种电子产品的主要配件,无论是消费家电产品,还是计算机、通讯设备、汽车等工业类产品。还广泛应用于5G通讯、人工智能、新能源汽车、物联网、绿色能源等新兴产业。
宽温低损耗锰锌软磁铁氧体材料主要用作电子设备中的开关电源,电子设备向小型化、轻量化发展也促使能量供应的开关电源向小型化、轻量化发展。要实现开关电源的小型化,轻量化、高效节能和可靠性。提高锰锌软磁铁氧体材料磁导率及降低宽温损耗是有效的方法。现有技术中发明专利公开号CN102097195A、CN102693803A、CN107200570A、CN111039667A等在宽温的范围内都实现了低功率损耗,但其高低温损耗都高于310kW/m3。
发明内容
本发明要解决的技术问题:提供一种宽温超低损耗锰锌铁氧体材料及其制备方法,以解决现有技术的锰锌软磁铁氧体材料在宽温的范围内都实现了低功率损耗,但其高低温损耗都高于310kW/m3等问题。
本发明技术方案:
一种宽温超低损耗锰锌铁氧体材料,所述材料的原料包括主成分和辅助成分;所述主成分含量以氧化物百分比计为:Fe2O3为50~52mol%、ZnO为10~12mol%、其余为MnO,主成分配方的总量为100%;按占主成分总重量计,辅助成分为:CaO 200~600ppm、ZrO2200~400ppm、Co2O33000~10000ppm、SiO220~100ppm、Nb2O5 200~400ppm、SnO2 400ppm~800ppm或TiO2300~600ppm中的任意五种或以上组合。
所述的一种宽温超低损耗锰锌铁氧体材料的制备方法,它包括:
步骤1、配料振磨混合:按照原料主成分配比称重,将各原料投入振磨机振磨混合,混料时间为0.5~1小时;
步骤2、预烧:对振磨处理后的粉料在空气窑中进行预烧;
步骤3、砂磨:预烧后的粉料,加入按比例称取的辅助成分用循环式砂磨机砂磨3~5小时,使粒径D50为1.0~1.5μm之间;
步骤4、喷雾造粒:用喷雾造粒机造粒;
步骤5、成型:采用全自动干压机进行成型,成型坯件尺寸为H25×15×7.5mm,成型压力为15~20Mpa;
步骤6、烧结:在氮气窑炉或钟罩炉中烧成,烧结最高温度1280~1340℃,烧结最高温度保温时间3~7小时,保温时氧气含量在2.8%~3.5%,然后在氮气保护气氛中冷却到室温,得到所要的软磁铁氧体材料。
步骤2所述预烧时,最高温度为850~900℃;最高温度保温时间为2~5小
时;预烧工艺见表1:
表1
造粒时,入口温度控制在280~320℃之间,出口温度为90~120℃。
本发明的有益效果:
本发明锰锌软磁铁氧体材料的制备,配方是基础、烧结是关键;低损耗铁氧体烧结的关键是晶粒化和致密化过程,本发明给出了烧结具体的关键技术及控制工艺,在900~1150℃列出了一个低氧气氛升温工艺,这样可以有效的使铁氧体致密化,1305℃或是1290℃保温阶段在一个平衡气氛中保温6到7小时,使晶粒长大形成磁芯损耗最小的晶粒尺寸。
配方和密度决定着材料的饱和磁通密度Bs(功率铁氧体磁芯通常工作于有直流偏置场的状态下,高Bs是为了保证磁芯具有高直流叠加特性的需要);而掺入有效的添加物及匹配适当的烧结工艺,对软磁铁氧体材料性能具有决定的意义。本发明在主配方、添加物和预烧工艺进行改进,特别在烧结工艺进行了深入的改进,通过对烧结温度及氧含量的精确控制;制备得到高低温损耗都小于310kW/m3的锰锌软磁铁氧体材料;解决了现有技术的锰锌软磁铁氧体材料在宽温的范围内都实现了低功率损耗,但其高低温损耗都高于310kW/m3等问题。
具体实施方式
一种宽温超低损耗锰锌铁氧体材料及其制备方法。由主成分和辅助成分组成,其中,主成分及含量以氧化物百分比计算为:Fe2O3为50~52mol%、ZnO为10~12mol%、其余为MnO,所述主成分配方的总量为100%;按占主成分总重量计的辅助成分为:CaO 200~600ppm、ZrO2 200~400ppm、Co2O33000~10000ppm、SiO220~100ppm、Nb2O5 200~400ppm、SnO2 400ppm~800ppm、TiO2300~600ppm中的任意五种或以上组合。
本发明中Fe2O3的含量最为关键,对于低损耗锰锌铁氧体来言,要Bs和Tc尽量高,损耗尽量低,提高Bs需要过铁配方,即摩尔比例要大于50%,但Fe2O3过多,则导致Fe2+离子增多,Fe2+与Fe3+之间的电子传递增多,材料损耗会加大,本发明在满足高Bs过铁配方的同时,严格避免引入过多的Fe2+,这是实现超低损耗的条件之一。
本发明通过掺入一定量的CaO与SiO2的复配添加剂,使之在晶界富聚,细化晶粒,增大材料的晶界电阻率,降低材料功耗;通过加入ZrO2、SnO2、TiO2或Nb2O5等添加剂来达到均匀化晶粒和提高密度的目的,抑制Fe2+的产生,进而降低损耗;加入Co2O3添加剂时,可使提高材料的温度稳定性和使用频率,降低损耗。
所述软磁铁氧体材料的具体制备过程为:
所述软磁铁氧体材料的具体制备过程为:
(1)配料振磨混合:按照所述原料主成分配比称重,将各原料投入振磨机振磨混合,混料时间为0.5~1小时;
(2)预烧:对振磨处理后的粉料在空气窑中进行预烧,最高温度为850~900℃,最高温度保温时间为2~5小时,具体预烧工艺见表1;
表1
(3)砂磨:预烧后的粉料,加入按比例称取的辅助成分用循环式砂磨机砂磨3~5小时,使粒径D50为1.0~1.5μm之间;
(4)喷雾造粒:用喷雾造粒机造粒,造粒时,入口温度控制在280~320℃之间,出口温度为90~120℃;
(5)成型:采用全自动干压机进行成型,成型坯件尺寸为H25×15×7.5mm,成型压力为15~20MPa。
(6)烧结:在氮气窑炉或钟罩炉中烧成,烧结最高温度1280~1340℃,烧结最高温度保温时间3~7小时,保温时氧气含量在2.8%~3.5%,然后在氮气保护气氛中冷却到室温,得到所要的软磁铁氧体材料;
本发明的软磁铁氧体特性如下表2:
实施例1
一种宽温超低损耗锰锌铁氧体材料及其制备方法。由主成分和辅助成分组成,其中,主成分及含量以氧化物百分比计算为:Fe2O3为50.55mol%、ZnO为11.05mol%、其余为MnO,所述主成分配方的总量为100%;按占主成分总重量计的辅助成分为:CaO 450ppm、ZrO2 250ppm、Co2O34000ppm、SiO230ppm、Nb2O5 300ppm、SnO2 550ppm。
所述软磁铁氧体材料的具体制备过程为:
所述软磁铁氧体材料的具体制备过程为:
(3)配料振磨混合:按照所述原料主成分配比称重,将各原料投入振磨机振磨混合,混料时间为0.8小时;
(4)预烧:对振磨处理后的粉料在空气窑中进行预烧,最高温度为870℃,最高温度保温时间为3小时,具体预烧工艺见表3;
表3
(3)砂磨:预烧后的粉料,加入按比例称取的辅助成分用循环式砂磨机砂磨3.5小时,使粒径D50为1.1μm之间;
(4)喷雾造粒:用喷雾造粒机造粒,造粒时,入口温度控制在300℃之间,出口温度为105℃;
(5)成型:采用全自动干压机进行成型,成型坯件尺寸为H25×15×7.5mm,成型压力为18MPa。
(7)烧结:在氮气窑炉或钟罩炉中烧成,烧结最高温度1305℃,烧结最高温度保温时间5.5小时,保温时氧气含量在3.2%,然后在氮气保护气氛中冷却到室温,得到所要的软磁铁氧体材料;具体烧结工艺见下表4
表4
本发明的实施例1软磁铁氧体特性如下表5:
表5
实施例2
一种宽温超低损耗锰锌铁氧体材料及其制备方法。由主成分和辅助成分组成,其中,主成分及含量以氧化物百分比计算为:Fe2O3为50.95mol%、ZnO为10.85mol%、其余为MnO,所述主成分配方的总量为100%;按占主成分总重量计的辅助成分为:CaO 400ppm、ZrO2 200ppm、Co2O33800ppm、SiO240ppm、Nb2O5 250ppm、SnO2250ppm、TiO2300ppm。
所述软磁铁氧体材料的具体制备过程为:
所述软磁铁氧体材料的具体制备过程为:
(5)配料振磨混合:按照所述原料主成分配比称重,将各原料投入振磨机振磨混合,混料时间为0.6小时;
(6)预烧:对振磨处理后的粉料在空气窑中进行预烧,最高温度为900℃,最高温度保温时间为2小时,具体预烧工艺见表6;
表6
(3)砂磨:预烧后的粉料,加入按比例称取的辅助成分用循环式砂磨机砂磨3小时,使粒径D50为1.25μm之间;
(4)喷雾造粒:用喷雾造粒机造粒,造粒时,入口温度控制在310℃之间,出口温度为100℃;
(5)成型:采用全自动干压机进行成型,成型坯件尺寸为H25×15×7.5mm,成型压力为17MPa。
(8)烧结:在氮气窑炉或钟罩炉中烧成,烧结最高温度1290℃,烧结最高温度保温时间6.5小时,保温时氧气含量在3.05%,然后在氮气保护气氛中冷却到室温,得到所要的软磁铁氧体材料;具体烧结工艺见下表7
表7
本发明的实施例2软磁铁氧体特性如下:
Claims (4)
1.一种宽温超低损耗锰锌铁氧体材料,其特征在于:所述材料的原料包括主成分和辅助成分;所述主成分含量以氧化物百分比计为:Fe2O3为50~52mol%、ZnO为10~12mol%、其余为MnO,主成分配方的总量为100%;按占主成分总重量计,辅助成分为:CaO 200~600ppm、ZrO2 200~400ppm、Co2O3 3000~10000ppm、SiO2 20~100ppm、Nb2O5 200~400ppm、SnO2400ppm~800ppm或TiO2 300~600ppm中的任意五种或以上组合。
2.如权利要求1所述的一种宽温超低损耗锰锌铁氧体材料的制备方法,它包括:
步骤1、配料振磨混合:按照原料主成分配比称重,将各原料投入振磨机振磨混合,混料时间为0.5~1小时;
步骤2、预烧:对振磨处理后的粉料在空气窑中进行预烧;
步骤3、砂磨:预烧后的粉料,加入按比例称取的辅助成分用循环式砂磨机砂磨3~5小时,使粒径D50为1.0~1.5μm之间;
步骤4、喷雾造粒:用喷雾造粒机造粒;
步骤5、成型:采用全自动干压机进行成型,成型坯件尺寸为H25×15×7.5mm,成型压力为15~20Mpa;
步骤6、烧结:在氮气窑炉或钟罩炉中烧成,烧结最高温度1280~1340℃,烧结最高温度保温时间3~7小时,保温时氧气含量在2.8%~3.5%,然后在氮气保护气氛中冷却到室温,得到所要的软磁铁氧体材料。
4.根据权利要求2所述的一种宽温超低损耗锰锌铁氧体材料的制备方法,其特征在于:造粒时,入口温度控制在280~320℃之间,出口温度为90~120℃。
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