CN106830913B - 一种高频低损耗高饱和磁通密度软磁铁氧体材料及其制备方法 - Google Patents

一种高频低损耗高饱和磁通密度软磁铁氧体材料及其制备方法 Download PDF

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CN106830913B
CN106830913B CN201710172937.0A CN201710172937A CN106830913B CN 106830913 B CN106830913 B CN 106830913B CN 201710172937 A CN201710172937 A CN 201710172937A CN 106830913 B CN106830913 B CN 106830913B
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张强原
邢冰冰
李小龙
沈晓燕
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Tiantong Kaili Technology Co ltd
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Abstract

本发明了公开了一种高频低损耗高饱和磁通密度软磁铁氧体材料及其制备方法，铁氧体材料由主成分和副成分组成，所述主成分以各自氧化物计算分别为Fe2O3:54.5～55.5mol%，ZnO：3.5～6mol%，Co2O3：0.10～0.25mol%，其余为MnO；所述副成分包括Nb2O5、CaCO3、V2O5、ZrO2和Ta2O5中的一种或几种。其制备方法包括配料、砂磨、预烧、砂磨、热处理、造粒、成型、烧结。本发明在主成分中添加Co2O3，并控制主成分、副成分的组成含量，优化烧结工艺，使软磁铁氧体材料同时具备高频低损耗、高磁通密度的性能。

Description

一种高频低损耗高饱和磁通密度软磁铁氧体材料及其制备 方法
技术领域
本发明涉及软磁铁氧体材料及其制备方法，具体涉及一种高频低损耗高饱和磁通密度软磁铁氧体材料及其制备方法。
背景技术
目前，软磁铁氧体是一种具有高磁导率、高电阻率和低损耗特性的材料，因而在变压器、电感器、开关电源、通讯设备、计算机电子整流设备中得到广泛应用；MnZn铁氧体作为一种重要的软磁铁氧体材料，被广泛应用在电子、通讯领域，主要用作能量存储和转换。随着功率转换用电子设备小型化、高效化、高能量密度化的发展，一方面要求功率转换用软磁铁氧体材料的频率越来越高，并且在高的工作频率下具有低的损耗，目前开关电源的频率已发展到1MHZ,而更高频率5MHz是未来市场发展方向；另一方面则要求软磁铁氧体材料具有高的饱和磁通密度来提高变压器的抗直流叠加能力，提高能量存储。
MnZn铁氧体磁心损耗可分为三部分：磁滞损耗(Ph)、涡流损耗(Pe)、剩余损耗(Pr)，对于MnZn铁氧体来说，在较高的频率下，涡流损耗和剩余损耗占据主要部分，降低MnZn铁氧体的高频损耗主要从以下方面入手：调整配方，加入添加剂和优化工艺；公开号CN1038333344A专利文献公开了一种高频低损耗铁氧体及其制备方法，通过把Fe2O3的含量固定在54～57mol%，ZnO含量限制在0～5mol%，实现高频低损耗，但是只涉及到损耗，并未提高饱和磁通密度特性。因此开发一种具有高频低损耗、高饱和磁通密度的MnZn铁氧体材料是迫切需要解决的问题。
发明内容
本发明所要解决的技术问题是提供一种高频低损耗高饱和磁通密度软磁铁氧体材料及其制备方法，在主成分中添加Co2O3，并控制主成分、副成分的组成含量，优化烧结工艺，使软磁铁氧体材料同时具备高频低损耗、高磁通密度的性能。
本发明解决技术问题所采用的技术方案是：一种高频低损耗高饱和磁通密度软磁铁氧体材料，由主成分和副成分组成，所述主成分为四元系，分别为Fe2O3 :54.5～55.5mol%，ZnO ：3.5～6mol%，Co2O3: 0.10～0.25mol%，其余为MnO；所述副成分包括Nb2O5 :0.01～0.03wt%、CaCO3 :0.04～0.20wt%、V2O5 :0.01～0.05wt%、ZrO2 :0～0.01wt%、Ta2O5 :0～0.05wt%中的一种或几种。
一种上所述的高频低损耗高饱和磁通密度软磁铁氧体材料的制备方法，包括如下步骤：
1) 配料：采用四元系配方，按照主配方Fe2O3、ZnO、Co2O3和MnO的比例进行称量并混合砂磨；
2）预烧：将混合后的粉料进行预烧；
3）砂磨：将添加剂加入预烧料中先振磨后再进行二次混合处理,砂磨时间为40～90min，粒径为0.1～1.0um；
4）热处理：将砂磨后的料浆进行600～900℃的热处理；
5）造粒：将砂磨后的料浆烘干后进行造粒；
6）成型：将造粒好的颗粒进行压制得到需要的毛坯；
7）烧结：将毛坯在窑炉中采用平衡氧分压进行烧结，在升温段800～1100℃下氧含量为0.1～0.5%，烧结温度为1180℃～1300℃。
作为一种优选，步骤2)中所述的预烧温度为700～1000℃，保温1～2h。
作为一种优选，步骤4)中所述的热处理温度为700～850℃，热处理时间3～5h，处理后粒径为0.3～1.1um，粒径分布0.2～2.0um占居90%以上。
作为一种优选，步骤6）中所述的烧结温度为1200～1300℃，平衡氧含量为2.0～4.0%,保温时间为3～5h。
本发明的有益效果是: 通过控制主成分、副成分的组成及含量，优化烧结工艺，所制备的高频铁氧体磁心在1MHz 50mT下100℃功耗小于100kW/m3，5MHz 10mT下100℃的功耗小于100kW/m3，100℃下的饱和磁通密度达到450mT，使软磁铁氧体材料同时具备高频低损耗、高磁通密度的性能。
具体实施方式
实施例1：一种高频低损耗高饱和磁通密度软磁铁氧体材料，由主成分和副成分组成，所述主成分为四元系，分别为Fe2O3:54.96mol%，ZnO：5.66mol% ，Co2O3：0.10mol%，其余为MnO；副成分Nb2O5:0.02wt%、CaCO3:0.10wt%、V2O5:0.03wt%、ZrO2:0.01wt%，以上副成分按Fe2O3 、ZnO、MnO、Co2O3的总重量百分比进行计算。
一种制作实施例1所述的高频低损耗高饱和磁通密度软磁铁氧体材料的制备方法，包括如下步骤：
1) 配料：采用四元系配方，按照主配方Fe2O3、ZnO、Co2O3和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850℃，保温2h；
3）砂磨：将添加剂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0.5um；
4）热处理：将砂磨后的料浆进行700℃的热处理，热处理时间5h，处理后粒径为0.7um，粒径分布0.2～2.0um占居90%以上。
5）造粒：将砂磨后的料浆烘干后进行造粒；
6）成型：将造粒好的颗粒进行压制得到需要的毛坯，
7）烧结：将毛坯在窑炉中采用平衡氧分压进行烧结，在升温段800～1100℃下氧含量为0.1%，烧结温度为1240℃，平衡氧含量为3.5%,保温时间为4h；
实施例2：一种高频低损耗高饱和磁通密度软磁铁氧体材料，由主成分和副成分组成，所述主成分为四元系，分别为Fe2O3:55.36mol%，ZnO：4.00mol% ，Co2O3：0.20mol%，其余为MnO；副成分Nb2O5:0.02wt%、CaCO3:0.05wt%、V2O5:0.03wt%、ZrO2:0.01wt%，以上副成分按Fe2O3 、ZnO、MnO、Co2O3的总重量百分比进行计算。
一种制作实施例2所述的高频低损耗高饱和磁通密度软磁铁氧体材料的制备方法，包括如下步骤：
1) 配料：采用四元系配方，按照主配方Fe2O3、ZnO、Co2O3和MnO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：将添加剂加入预烧料中先振磨后再进行二次混合处理,砂磨时间为50min，粒径为0.7um；
4）热处理：将砂磨后的料浆进行850℃的热处理，热处理时间3h，处理后粒径为0.9um，粒径分布0.2～2.0um占居90%以上。
5）造粒：将砂磨后的料浆烘干后进行造粒；
6）成型：将造粒好的颗粒进行压制得到需要的毛坯；
7）烧结：将毛坯在窑炉中采用平衡氧分压进行烧结，在升温段800～1100℃下氧含量为0.3%，烧结温度为1260℃，平衡氧含量为4.0%,保温时间为5h；
实施例3：一种高频低损耗高饱和磁通密度软磁铁氧体材料，由主成分和副成分组成，所述主成分为四元系，分别为Fe2O3:55.40mol%，ZnO：3.77mol% ，Co2O3：0.20mol%，其余为MnO；副成分Nb2O5:0.02wt%、CaCO3:0.10wt%、V2O5:0.03wt%、Ta2O5:0.03wt%，以上副成分按Fe2O3 、ZnO、MnO、Co2O3的总重量百分比进行计算。
一种制作实施例3所述的高频低损耗高饱和磁通密度软磁铁氧体材料的制备方法，包括如下步骤：
1) 配料：采用四元系配方，按照主配方Fe2O3、ZnO、Co2O3和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750℃，保温2h；
3）砂磨：将添加剂加入预烧料中先振磨后再进行二次混合处理,砂磨时间为80min，粒径为0.2um；
4）热处理：将砂磨后的料浆进行700℃的热处理，热处理时间3h，处理后粒径为0.4um，粒径分布0.2～2.0um占居90%以上。
5）造粒：将砂磨后的料浆烘干后进行造粒；
6）成型：将造粒好的颗粒进行压制得到需要的毛坯；
7）烧结：将毛坯在窑炉中采用平衡氧分压进行烧结，在升温段800～1100℃下氧含量为0.2%，烧结温度为1230℃，平衡氧含量为3.2%,保温时间为4h
实施例4：一种高频低损耗高饱和磁通密度软磁铁氧体材料，由主成分和副成分组成，所述主成分为四元系，分别为Fe2O3:55.11mol%，ZnO：3.14mol% ，Co2O3：0.25mol%，其余为MnO；副成分Nb2O5:0.02wt%、CaCO3:0.15wt%、V2O5:0.03wt%、ZrO2:0.005wt%、Ta2O5:0.02wt%，以上副成分按Fe2O3 、ZnO、MnO、Co2O3的总重量百分比进行计算。
一种制作实施例4所述的高频低损耗高饱和磁通密度软磁铁氧体材料的制备方法，包括如下步骤：
1) 配料：采用四元系配方，按照主配方Fe2O3、ZnO、Co2O3和MnO的比例进行称量并混合砂磨，砂磨时间为30min；
2）预烧：将混合后的粉料进行预烧，预烧温度为960℃，保温1h；
3）砂磨：将添加剂加入预烧料中先振磨后再进行二次混合处理,砂磨时间为90min，粒径为0.3um；
4）热处理：将砂磨后的料浆进行800℃的热处理，热处理时间3h，处理后粒径为0.5um，粒径分布0.2～2.0um占居90%以上。
5）造粒：将砂磨后的料浆烘干后进行造粒；
6）成型：将造粒好的颗粒进行压制得到需要的毛坯；
7）烧结：将毛坯在窑炉中采用平衡氧分压进行烧结，在升温段800～1100℃下氧含量为0.4%，烧结温度为1200℃，平衡氧含量为2.0%,保温时间为5h。
以上四个实施例制备的标准样环性能测试结果如下：
Figure 885540DEST_PATH_IMAGE001
以上所述是本发明的优选实施例，应当指出，对于本领域技术人员来说，在不脱离本发明制备方法的前提下，还可以作出润饰，这些润饰也视为本发明的保护范围。

Claims (4)

1.一种高频低损耗高饱和磁通密度软磁铁氧体材料，由主成分和副成分组成，其特征在于:所述主成分为四元系，分别为Fe2O3 :54.5～55.5mol%，ZnO ：3.5～6mol%，Co2O3: 0.10～0.25mol%，其余为MnO；所述副成分包括Nb2O5 :0.01～0.03wt%、CaCO3 :0.04～0.20wt%、V2O5 :0.01～0.05wt%、ZrO2 :0～0.01wt%、Ta2O5 :0～0.05wt%中的一种或几种；其制备方法包括如下步骤：
1) 配料：采用四元系配方，按照主配方Fe2O3、ZnO、Co2O3和MnO的比例进行称量并混合砂磨；
2）预烧：将混合后的粉料进行预烧；
3）砂磨：将添加剂加入预烧料中先振磨后再进行二次混合处理,砂磨时间为40～90min，粒径为0.1～1.0um；
4）热处理：将砂磨后的料浆进行600～900℃的热处理；
5）造粒：将砂磨后的料浆烘干后进行造粒；
6）成型：将造粒好的颗粒进行压制得到需要的毛坯；
7）烧结：将毛坯在窑炉中采用平衡氧分压进行烧结，在升温段800～1100℃下氧含量为0.1～0.5%，烧结温度为1180℃～1300℃。
2.根据权利要求1所述的高频低损耗高饱和磁通密度软磁铁氧体材料，其特征在于：步骤2)中所述的预烧温度为700～1000℃，保温1～2h。
3.根据权利要求1所述的高频低损耗高饱和磁通密度软磁铁氧体材料，其特征在于：步骤4)中所述的热处理温度为700～850℃，热处理时间3～5h，处理后粒径为0.3～1.1um，粒径分布0.2～2.0um占 据 90%以上。
4.根据权利要求1所述的高频低损耗高饱和磁通密度软磁铁氧体材料，其特征在于：步骤6）中所述的烧结温度为1200～1260℃，平衡氧含量为2.0～4.0%,保温时间为3～5h。
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