CN116283262A - 一种耐高温高磁导率高阻抗MnZn铁氧体材料及其制备方法和应用 - Google Patents
一种耐高温高磁导率高阻抗MnZn铁氧体材料及其制备方法和应用 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 89
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 239000008187 granular material Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 4
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- 239000004576 sand Substances 0.000 description 15
- 238000000227 grinding Methods 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000003801 milling Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
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- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910004762 CaSiO Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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Abstract
本发明提供了一种耐高温高磁导率高阻抗MnZn铁氧体材料及其制备方法和应用,属于铁氧体材料技术领域。本发明提供的MnZn铁氧体材料具有较高的初始磁导率,高居里温度,在100KHz~1MHz范围内具有较高的阻抗特性。以外径25mm、内径15mm、高度10mm的环状磁芯测试,初始磁导率>7000,居里温度>190℃,频率提高到300KHz左右初始磁导率才开始衰减;在2匝绕组、0.1V电压下测试,100KHz阻抗>15Ω,500KHz阻抗>50Ω,阻抗特性优异。因而在高温下也具有较高的磁导率和阻抗特性,可以适应高温工作环境,起到稳定的滤波或抗电磁干扰效果,适合用作高温条件下工作的滤波器件电感材料。
Description
技术领域
本发明涉及铁氧体材料技术领域,尤其涉及一种耐高温高磁导率高阻抗MnZn铁氧体材料及其制备方法和应用。
背景技术
高导MnZn铁氧体材料具有高初始磁导率、高电阻率、高阻抗和低损耗因数的特点,广泛应用于制作宽带变压器、扼流圈电感、抗电磁干扰共模线圈等,使用这类材料制作的电子元器件具有较高的阻抗特性和良好的抗电磁干扰能力,应用领域涉及家用电器、数字通信、航空航天和汽车电子。随着现代技术的发展,高导MnZn铁氧体应用环境越来越复杂,对其工作特性要求也越来越高,航空航天、汽车电子等领域电子设备工作温度普遍较高,然而常规高导MnZn铁氧体材料居里温度普遍较低,一般在140℃以下,难以满足高温环境的使用要求。
发明内容
本发明的目的在于提供一种耐高温高磁导率高阻抗MnZn铁氧体材料及其制备方法和应用,所述MnZn铁氧体材料具有耐高温、高磁导率和高阻抗特性。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种耐高温高磁导率高阻抗MnZn铁氧体材料,包括主成分和辅助成分,以所述主成分的总量为100mol%计,所述主成分包括以下摩尔百分比的制备原料:Fe2O3:53~56mol%,ZnO:12.5~15.5mol%,余量为Mn3O4;所述辅助成分在主成分中的质量含量为:CaCO3100~400ppm,SiO250~150ppm,Bi2O3100~500ppm,Nb2O5100~300ppm,ZrO250~200ppm,Co2O3300~1000ppm,CuO 500~3000ppm。
本发明提供了上述技术方案所述耐高温高磁导率高阻抗MnZn铁氧体材料的制备方法,包括以下步骤:
将Fe2O3、ZnO、Mn3O4与水进行湿式混合,得到混合料;
将所述混合料进行预烧,得到铁氧体预烧料;
将所述铁氧体预烧料与辅助成分混合,依次进行砂磨和造粒,得到颗粒料;
将所述颗粒料依次进行压制和烧结,得到耐高温高磁导率高阻抗MnZn铁氧体材料。
优选的,所述水的质量为Fe2O3、ZnO和Mn3O4总质量的50%,所述湿式混合的时间为60~120min。
优选的,所述预烧的温度为800~1000℃,时间为60~120min。
优选的,所述预烧的气氛为空气气氛。
优选的,所述砂磨的介质为水,所述砂磨的时间为60~120min。
优选的,进行所述砂磨50~100min后,向所得砂磨物料中加入PVA溶胶,所述PVA溶胶的质量为铁氧体预烧料质量的1%。
优选的,所述烧结包括:第一阶段,以1~3.5℃/min的升温速度升温至300℃,在300℃保温0.3~2h;第二阶段,以0.5~1℃/min的升温速度升温至800℃后,降低氧分压至5~10%;第三阶段,保持氧分压为5~10%,以4~6℃/min的升温速度升温至1350~1430℃,保持氧分压为1~10%保温4~8h。
优选的,完成所述烧结后,还包括:以3~6℃/min的降温速度降至室温。
本发明提供了上述技术方案所述耐高温高磁导率高阻抗MnZn铁氧体材料或上述技术方案所述制备方法制备得到的耐高温高磁导率高阻抗MnZn铁氧体材料在航空航天或汽车电子领域中的应用。
本发明提供了一种耐高温高磁导率高阻抗MnZn铁氧体材料,本发明利用主成分中ZnO提高铁氧体材料的居里温度,进而提高耐高温特性;利用辅助成分提高宽温磁导率和阻抗特性;Bi2O3掺杂到MnZn铁氧体中,促进铁氧体化反应进行,提高晶粒大小和烧结密度,进而提高磁导率;Co2O3掺杂到MnZn铁氧体中可以降低宽温磁晶各向异性,从而提高铁氧体材料的磁导率,并改善宽温特性。CaCO3、SiO2属于高熔点氧化物,掺杂到MnZn铁氧体后,烧结过程中Ca和Si会向晶界偏析,形成高电阻率的CaSiO3,从而提高晶界电阻率,改善材料的频率和阻抗特性;Nb2O5和ZrO2属于高熔点氧化物,掺杂入铁氧体中主要分布在晶界上,进一步提高晶界电阻率;SiO2、CaO、Nb2O5、ZrO2复配掺杂可以在铁氧体晶界形成多种复合氧化物,实现协同改善铁氧体材料的阻抗作用;CuO能与Fe2O3、MnO、ZnO形成低熔点共熔物,从而降低铁氧体材料烧结温度,提高晶粒大小,改善磁导率特性。因而本发明提供的MnZn铁氧体材料具有较高的初始磁导率,高居里温度,在100KHz~1MHz范围内具有较高的阻抗特性。以外径25mm、内径15mm、高度10mm的环状磁芯测试,初始磁导率>7000,居里温度>190℃,频率提高到300KHz左右初始磁导率才开始衰减;在2匝绕组、0.1V电压下测试,100KHz阻抗>15Ω,500KHz阻抗>50Ω,阻抗特性优异。因而在高温下也具有较高的磁导率和阻抗特性,可以适应高温工作环境,起到稳定的滤波或抗电磁干扰效果,适合用作高温条件下工作的滤波器件电感材料。
具体实施方式
本发明提供了一种耐高温高磁导率高阻抗MnZn铁氧体材料,包括主成分和辅助成分,以所述主成分的总量为100mol%计,所述主成分包括以下摩尔百分比的制备原料:Fe2O3:53~56mol%,ZnO:12.5~15.5mol%,余量为Mn3O4;所述辅助成分在主成分中的质量含量为:CaCO3100~400ppm,SiO250~150ppm,Bi2O3100~500ppm,Nb2O5100~300ppm,ZrO250~200ppm,Co2O3300~1000ppm,CuO 500~3000ppm。
在本发明中,若无特殊说明,所需制备原料均为本领域技术人员熟知的市售商品。
本发明提供的耐高温高磁导率高阻抗MnZn铁氧体材料包括主成分;以所述主成分的总量为100mol%计,所述主成分包括以下摩尔百分比的制备原料:Fe2O3:53~56mol%,ZnO:12.5~15.5mol%,余量为Mn3O4。
在本发明中,所述Fe2O3的摩尔百分比更优选为54~55mol%,所述ZnO的摩尔百分比优选为13~15mol%。
ZnO的占比越低,其对应的居里温度也越高,但ZnO高的同时会降低整体的宽温磁导率,本发明通过控制ZnO占比为12.5~15.5mol%,使得铁氧体材料的居里温度达到190℃以上。
本发明提供的耐高温高磁导率高阻抗MnZn铁氧体材料包括辅助成分,所述辅助成分在主成分中的质量含量为:CaCO3100~400ppm,SiO250~150ppm,Bi2O3100~500ppm,Nb2O5100~300ppm,ZrO250~200ppm,Co2O3300~1000ppm,CuO 500~3000ppm;更优选为Bi2O3300ppm,CuO 1000ppm。
本发明中,Bi2O3属于低熔点(825℃)氧化物,掺杂到MnZn铁氧体中,在较低的温度下即可形成液相,促进铁氧体化反应进行,提高晶粒大小和烧结密度,进而提高磁导率。
MnZn铁氧体材料具有负的磁晶各向异性,而Co2O3是具有正的磁晶各向异性的氧化物,Co2O3掺杂到MnZn铁氧体中可以降低宽温磁晶各向异性,从而提高铁氧体材料的磁导率,并改善宽温特性。
CaCO3、SiO2属于高熔点氧化物,掺杂到MnZn铁氧体后,烧结过程中Ca和Si会向晶界偏析,形成高电阻率的CaSiO3,从而提高晶界电阻率,改善材料的频率和阻抗特性。Nb2O5和ZrO2属于高熔点氧化物,掺杂入铁氧体中主要分布在晶界上,进一步提高晶界电阻率。SiO2、CaO、Nb2O5、ZrO2复配掺杂可以在铁氧体晶界形成多种复合氧化物,实现协同改善铁氧体材料的阻抗作用。CuO能与Fe2O3、MnO、ZnO形成低熔点共熔物,从而降低铁氧体材料烧结温度,提高晶粒大小,改善磁导率特性。
本发明提供了上述技术方案所述耐高温高磁导率高阻抗MnZn铁氧体材料的制备方法,包括以下步骤:
将Fe2O3、ZnO、Mn3O4与水进行湿式混合,得到混合料;
将所述混合料进行预烧,得到铁氧体预烧料;
将所述铁氧体预烧料与辅助成分混合,依次进行砂磨和造粒,得到颗粒料;
将所述颗粒料依次进行压制和烧结,得到耐高温高磁导率高阻抗MnZn铁氧体材料。
本发明将Fe2O3、ZnO、Mn3O4与水进行湿式混合,得到混合料。
本发明优选在砂磨机中进行湿式混合;所述水的质量优选为Fe2O3、ZnO和Mn3O4总质量的50%,所述湿式混合的时间优选为60~120min。
完成所述湿式混合后,本发明优选将所得物料进行干燥,得到混合料;本发明对所述干燥没有特殊的限定,按照本领域熟知的过程进行即可。
得到混合料后,本发明将所述混合料进行预烧,得到铁氧体预烧料。
本发明优选将所述混合料置于承烧板上,放入马弗炉中进行预烧;所述预烧的温度优选为800~1000℃,更优选为900℃;时间优选为60~120min,更优选为90min;所述预烧的气氛优选为空气气氛。
本发明通过预烧使部分原料Fe2O3、Mn3O4和ZnO发生铁氧体化反应,形成ZnFe2O4和MnFe2O4,避免后续粉料二次烧结过程中收缩过大而导致毛坯开裂。
得到铁氧体预烧料后,本发明将所述铁氧体预烧料与辅助成分混合,依次进行砂磨和造粒,得到颗粒料。
本发明优选将辅助成分与铁氧体预烧料放入篮式砂磨机中,进行砂磨;所述砂磨的介质优选为水,所述砂磨的时间优选为60~120min。
进行所述砂磨50~100min后,本发明优选向所得砂磨物料中加入PVA溶胶,所述PVA溶胶的质量为铁氧体预烧料质量的1%。本发明对所述造粒没有特殊的限定,按照本领域熟知的过程进行即可。
得到颗粒料后,本发明将所述颗粒料依次进行压制和烧结,得到耐高温高磁导率高阻抗MnZn铁氧体材料。
本发明对所述压制的过程没有特殊的限定,按照本领域熟知的过程进行即可;所述压制后,所得毛坯的密度优选为2.6±0.1g/cm3。
本发明对所述压制后坯体的形状没有特殊的限定,根据实际需求调整即可;在本发明的实施例中,具体是将颗粒料压制成外径25mm、内径15mm、高度10mm的环状毛坯。
本发明优选在气氛保护钟罩炉中进行烧结。
在本发明中,所述烧结优选包括:第一阶段,以1~3.5℃/min的升温速度升温至300℃,在300℃保温0.3~2h;第二阶段,以0.5~1℃/min的升温速度升温至800℃后,降低氧分压至5~10%;第三阶段,保持氧分压为5~10%,以4~6℃/min的升温速度升温至1350~1430℃(更优选为1400℃),保持氧分压为1~10%(更优选为3%)保温4~8h,更优选为6h。
本发明通过第一阶段的烧结使毛坯中的有机物充分燃烧、挥发。
在所述第二阶段中,升温至800℃后,本发明优选关闭炉门,向炉膛内充入氮气,降低氧分压至5~10%。
完成所述烧结后,本发明优选还包括:以3~6℃/min的降温速度降至室温,得到耐高温高磁导率高阻抗MnZn铁氧体材料。
本发明提供了上述技术方案所述耐高温高磁导率高阻抗MnZn铁氧体材料或上述技术方案所述制备方法制备得到的耐高温高磁导率高阻抗MnZn铁氧体材料在航空航天或汽车电子领域中的应用。本发明对所述应用的方法没有特殊的限定,按照本领域熟知的方法应用即可。
下面将结合本发明中的实施例,对本发明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
(1)按照摩尔百分比:Fe2O353mol%,ZnO 15.0mol%,Mn3O432mol%,准确称取Fe2O3、ZnO和Mn3O4,在砂磨机中进行湿式混合,加水量为原料总质量的50%,混合时间120min,干燥,得到混合料;
(4)将所述混合料置于承烧板上,放入马弗炉中预烧,预烧温度900℃,预烧时间120min,气氛为空气气氛,得到铁氧体预烧料;
(5)向铁氧体预烧料中加入辅助成分,CaCO3400ppm,SiO250ppm,Bi2O3500ppm,Nb2O5100ppm,ZrO2200ppm,Co2O31000ppm,CuO 500ppm;辅助成分与铁氧体预烧料一起放入篮式砂磨机中,砂磨介质为水,砂磨时间120min,砂磨50min后向所得砂磨物料中加入铁氧体预烧料质量1%的PVA溶胶,进行造粒,得到颗粒料;
(4)将所述颗粒料压制成外径25mm,内径15mm,高度10mm的环状毛坯,毛坯密度2.6g/cm3;
(5)将压制的毛坯在气氛保护钟罩炉中进行烧结,具体烧结过程为:以1℃/min的速度升温到300℃,在300℃保温2h;然后以0.5℃升温速度升温到800℃,关闭炉门,向炉膛内充入氮气,将氧分压降低至5%;再将升温速度提高至4℃/min,升温到1430℃,升温段氧分压保持在5%,保温过程氧分压保持在3%,保温时间4h,在所得平衡气氛中以3℃/min速度冷却到室温,得到MnZn铁氧体材料,外径25mm、内径15mm、高度10mm的环状磁芯。
实施例2
(1)按照摩尔百分比:Fe2O3:56mol%,ZnO:13mol%,Mn3O4:31mol%,准确称取Fe2O3、ZnO和Mn3O4,在砂磨机中进行湿式混合,加水量为原料总重量的50%,混合时间120min,干燥,得到混合料;
(6)将所述混合料置于承烧板上,放入马弗炉中预烧,预烧温度800℃,预烧时间90min,气氛为空气气氛,得到铁氧体预烧料;
(7)向所述铁氧体预烧料中加入辅助成分,CaCO3400ppm,SiO2:150ppm,Bi2O3:300ppm,Nb2O5:300ppm,ZrO2:50ppm,Co2O3:300ppm,CuO 1000ppm,将辅助成分与预烧料一起放入篮式砂磨机中,砂磨介质为水,砂磨时间120min,砂磨100min后加入铁氧体预烧料质量1%的PVA溶胶,进行造粒,得到颗粒料;
(4)将所述颗粒料压制成外径25mm,内径15mm,高度10mm的环状毛坯,毛坯密度2.6±0.1g/cm3;
(5)将压制的毛坯在气氛保护钟罩炉中进行烧结,具体烧结过程为:以3.5℃/min的速度升温到300℃,在300℃保温2h;然后以0.5℃升温速度升温到800℃,关闭炉门,向炉膛内充入氮气,将氧分压降低至5%;再将升温速度提高至4℃/min,升温到1400℃,升温段氧分压保持在5%,保温过程氧分压在1%,保温时间6h,在所得平衡气氛中以3℃/min速度冷却到室温,得到MnZn铁氧体材料,外径25mm、内径15mm、高度10mm的环状磁芯。
性能测试
1)对实施例1~2制备的MnZn铁氧体材料进行性能测试,软磁铁氧体材料初始磁导率测试国标-GBT-35690-2017;软磁铁氧体材料阻抗测试国标-GBT-3658-2008,在2匝绕组、0.1V电压下测试;软磁铁氧体材料居里温度测试标准-GB/T-6553-2014;每个实施例的样品平行测试5个样品,分别编号为样环1~5,所得结果见表1~2。
表1 实施例1制备的MnZn铁氧体材料的性能数据
表2 实施例2制备的MnZn铁氧体材料的性能数据
由表1~2可知,本发明制备的MnZn铁氧体材料具有耐高温、高磁导率和高阻抗特性。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种耐高温高磁导率高阻抗MnZn铁氧体材料,其特征在于,包括主成分和辅助成分,以所述主成分的总量为100mol%计,所述主成分包括以下摩尔百分比的制备原料:Fe2O3:53~56mol%,ZnO:12.5~15.5mol%,余量为Mn3O4;所述辅助成分在主成分中的质量含量为:CaCO3100~400ppm,Si O250~150ppm,Bi2O3100~500ppm,Nb2O5100~300ppm,ZrO250~200pp m,Co2O3300~1000ppm,CuO500~3000ppm。
2.权利要求1所述耐高温高磁导率高阻抗MnZn铁氧体材料的制备方法,其特征在于,包括以下步骤:
将Fe2O3、ZnO、Mn3O4与水进行湿式混合,得到混合料;
将所述混合料进行预烧,得到铁氧体预烧料;
将所述铁氧体预烧料与辅助成分混合,依次进行砂磨和造粒,得到颗粒料;
将所述颗粒料依次进行压制和烧结,得到耐高温高磁导率高阻抗MnZn铁氧体材料。
3.根据权利要求2所述的制备方法,其特征在于,所述水的质量为Fe2O3、ZnO和Mn3O4总质量的50%,所述湿式混合的时间为60~120min。
4.根据权利要求2所述的制备方法,其特征在于,所述预烧的温度为800~1000℃,时间为60~120min。
5.根据权利要求2或4所述的制备方法,其特征在于,所述预烧的气氛为空气气氛。
6.根据权利要求2所述的制备方法,其特征在于,所述砂磨的介质为水,所述砂磨的时间为60~120min。
7.根据权利要求6所述的制备方法,其特征在于,进行所述砂磨50~100min后,向所得砂磨物料中加入PVA溶胶,所述PVA溶胶的质量为铁氧体预烧料质量的1%。
8.根据权利要求2所述的制备方法,其特征在于,所述烧结包括:第一阶段,以1~3.5℃/min的升温速度升温至300℃,在300℃保温0.3~2h;第二阶段,以0.5~1℃/min的升温速度升温至800℃后,降低氧分压至5~10%;第三阶段,保持氧分压为5~10%,以4~6℃/min的升温速度升温至1350~1430℃,保持氧分压为1~10%保温4~8h。
9.根据权利要求2或8所述的制备方法,其特征在于,完成所述烧结后,还包括:以3~6℃/min的降温速度降至室温。
10.权利要求1所述耐高温高磁导率高阻抗MnZn铁氧体材料或权利要求2~9任一项所述制备方法制备得到的耐高温高磁导率高阻抗MnZn铁氧体材料在航空航天或汽车电子领域中的应用。
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