CN104934181B - 一种软磁MnZn系功率铁氧体 - Google Patents

一种软磁MnZn系功率铁氧体 Download PDF

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CN104934181B
CN104934181B CN201510193299.1A CN201510193299A CN104934181B CN 104934181 B CN104934181 B CN 104934181B CN 201510193299 A CN201510193299 A CN 201510193299A CN 104934181 B CN104934181 B CN 104934181B
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soft magnetism
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mnzn
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CN104934181A (zh
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赵旭
顾小建
卢飞翔
张雪强
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

本发明公开了一种软磁MnZn系功率铁氧体，旨在提供一种饱和磁通密度高、损耗低的软磁MnZn系功率铁氧体。它包括主成分和副成分，所述的主成分包括Fe2O3、MnO、ZnO和NiO，以主成分的总量计算，Fe2O3占53.0‑55.0mol％，ZnO占3.0‑7.0mol％，NiO占0‑1.0mol％，MnO为余量，所述的副成分包括CoO、SiO2、CaCO3、Nb2O5和ZrO2。本发明的有益效果是：100℃的饱和磁通密度Bs大于460mT，100℃的磁芯损耗Pcv小于320kW/m3；因为其具有如此优良的性能，在产品的实际应用上，可以使器件进一步小型化，并且由于非常低的损耗，器件的工作效率还可以进一步提高。

Description

一种软磁MnZn系功率铁氧体
技术领域
本发明涉及铁氧体相关技术领域，尤其是指一种软磁MnZn系功率铁氧体。
背景技术
MnZn铁氧体广泛应用于电子、通讯领域作为电源变压器材料。传统开关电源的输出功率与材料直接相关的参数就是材料的饱和磁通密度。高饱和磁通密度的材料可以使开关电源更加小型化、薄型化。材料的功率损耗会影响电能的转化效率，越低功率损耗，器件的转化效率越高。
近年来，行业对高饱和磁通密度低损耗的铁氧体材料进行了各种研究，如中国发明专利公开CN102063989、CN101483092、CN101552073、CN102194561等对主成分进行了研究，获得了很好的性能，但是其100℃的饱和磁通密度Bs都没有办法做到460mT以上。中国发明专利公开CN101290827达到了100℃饱和磁通密度Bs在460mT，但是其工艺并不是传统的软磁铁氧体工艺，批量生产困难。中国发明专利公开CN103964832获得了100℃饱和磁通密度Bs在470mT以上的成就，但是其主成分中使用了1-4mol％的NiO，由于Ni的成本非常高，其材料降低了市场竞争力。
发明内容
本发明是为了克服现有技术中存在饱和磁通密度低、损耗大的不足，提供了一种饱和磁通密度高、损耗低的软磁MnZn系功率铁氧体。
为了实现上述目的，本发明采用以下技术方案：
一种软磁MnZn系功率铁氧体，包括主成分和副成分，所述的主成分包括Fe2O3、MnO、ZnO和NiO，以主成分的总量计算，Fe2O3占53.0-55.0mol％，ZnO占3.0-7.0mol％，NiO占0-1.0mol％，MnO为余量，所述的副成分包括CoO、SiO2、CaCO3、Nb2O5和ZrO2。
其中：NiO的含量范围中包含0。本发明中，可以使用传统工艺进行批量生产，采用特有的组分配方和作为副成分的掺杂元素相互配合，经过研磨、压制、烧结而得。其中，主成分配方力求更合理地为掺杂提供有利的基础，在此基础上，进而以独到的掺杂促进更好地液相烧结、更细化晶粒，生长出更为均匀细化的晶粒分布，同时控制晶界气孔率，形成较高烧结密度，最终生成更为合理的软磁微观结构，从而获得饱和磁通密度高、损耗低的软磁MnZn系功率铁氧体。
作为优选，所述的副成分包括第一副成分和第二副成分，所述的第一副成分为CoO，以主成分的总量计算为基础，CoO的含量为0-0.15wt％。其中：CoO的含量范围中包含0。
作为优选，所述的第二副成分为SiO2、CaCO3、Nb2O5和ZrO2，以主成分的总量计算为基础，SiO2为0.005-0.015wt％、CaCO3为0.03-0.15wt％、Nb2O5为0.05-0.4wt％、ZrO2为0.05-0.4wt％。
作为优选，在1194A/m的测试条件下，25℃时所述软磁MnZn系功率铁氧体的饱和磁通密度Bs大于550mT，100℃时所述软磁MnZn系功率铁氧体的饱和磁通密度Bs大于460mT。
作为优选，在100kHz、200mT的测试条件下，25℃时所述的软磁MnZn系功率铁氧体功率损耗Pcv小于750kW/m3，100℃时所述的软磁MnZn系功率铁氧体功率损耗Pcv小于320kW/m3。
本发明的有益效果是：100℃的饱和磁通密度Bs大于460mT，100℃的磁芯损耗Pcv小于320kW/m3；因为其具有如此优良的性能，在产品的实际应用上，可以使器件进一步小型化，并且由于非常低的损耗，器件的工作效率还可以进一步提高。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
由于本发明可以使用传统工艺进行批量生产，故以下实施案例均采用统一的生产工艺进行生产，仅配方有所区别，具体制备工艺如下：
1.配料
按照各实施例与对比例配比，分别以Fe2O3、MnO、ZnO形式计算比例，称取Fe2O3、Mn3O4、ZnO三种原料，然后在砂磨机中加入去离子水进行混合和破碎，时间40分钟。循环混合10分钟后进行喷雾造粒。
2.预烧
将喷雾料放入预烧炉中，在850℃下进行预烧，时间3个小时。
3.二次砂磨
在预烧料中加入以下重量百分比的辅助成分：CaCO3：0.08wt％，SiO2：0.05wt％，Nb2O5：0.02wt％，ZrO2：0.02wt％。其中：CoO和NiO按照各实施例与对比例称取。然后将粉料放入砂磨机中加入去离子水进行二次砂磨，砂磨时间90分钟。
4.喷雾造粒和成型
在二次砂磨料中加入约0.08wt％的PVA，以及0.004wt％的消泡剂，然后在喷雾塔中进行喷雾造粒成50-200μm的颗粒。将不同实施例与对比例的颗粒成型成密度为3.00-3.15g/cm3的H25*15*8mm标准样环毛坯。
5.烧结
在一定的氧气和氮气比例下升温，在1300℃的温度条件下烧结5小时，烧结时的氧气分压为5％，然后在一定的氧气和氮气的比例下冷却到室温。
6.测试
将烧结好的样环用日本岩崎公司的SY8218仪器进行功耗Pcv及饱和磁通密度Bs的测试。测试条件分别为：在100kHz，200mT的条件下测试Pcv；在50Hz，1194A/m的条件下测试Bs。
以下是为了更好的说明本发明而列举的实施例，但是本发明并不限于这些实施例。
实施例1
Fe2O3＝54.8mol％、ZnO＝3mol％、MnO＝42.2mol％、NiO＝0.0mol％、CoO＝0.08wt％。
实施例2
Fe2O3＝54.4mol％、ZnO＝4mol％、MnO＝41.6mol％、NiO＝0.0mol％、CoO＝0.08wt％。
实施例3
Fe2O3＝54.0mol％、ZnO＝5mol％、MnO＝41.0mol％、NiO＝0.0mol％、CoO＝0.08wt％。
实施例4
Fe2O3＝53.6mol％、ZnO＝6mol％、MnO＝40.4mol％、NiO＝0.0mol％、CoO＝0.08wt％。
实施例5
Fe2O3＝53.2mol％、ZnO＝7mol％、MnO＝39.8mol％、NiO＝0.0mol％、CoO＝0.08wt％。
对比例1
Fe2O3＝55.2mol％、ZnO＝2mol％、MnO＝42.8mol％、NiO＝0.0mol％、CoO＝0.08wt％。
对比例2
Fe2O3＝52.8mol％、ZnO＝8mol％、MnO＝39.2mol％、NiO＝0.0mol％、CoO＝0.08wt％。
实施例6
Fe2O3＝54.0mol％、ZnO＝6mol％、MnO＝39.0mol％、NiO＝1.0mol％、CoO＝0.08wt％。
对比例3
Fe2O3＝54.4mol％、ZnO＝6mol％、MnO＝37.6mol％、NiO＝2.0mol％、CoO＝0.08wt％。
实施例7
Fe2O3＝53.8mol％、ZnO＝6mol％、MnO＝40.2mol％、NiO＝0.0mol％、CoO＝0.0wt％。
实施例8
Fe2O3＝53.4mol％、ZnO＝6mol％、MnO＝40.6mol％、NiO＝0.0mol％、CoO＝0.15wt％。
对比例4
Fe2O3＝53.0mol％、ZnO＝6mol％、MnO＝41.0mol％、NiO＝0.0mol％、CoO＝0.20wt％。
根据以上各实施例与对比例的配方进行制备软磁MnZn系功率铁氧体，并压环烧结测试性能，测试结果见表1。
表1
从表1中的各项数据分析可得：(1)实施例1-5和对比例1、2相比较，当ZnO的含量低于3mol％时，软磁MnZn系功率铁氧体的功率损耗上升；当ZnO的含量高于7mol％时，软磁MnZn系功率铁氧体的饱和磁通密度降低；(2)实施例4、6和对比例3相比较，当NiO的含量高于1mol％时，软磁MnZn系功率铁氧体在100℃时的功率损耗上升；(3)实施例4、7、8和对比例4相比较，当CoO的含量高于0.15wt％时，软磁MnZn系功率铁氧体的饱和磁通密度降低；软磁MnZn系功率铁氧体在100℃时的功率损耗上升。由表1各项性能逐项对比可见：在1194A/m测试条件下，本发明的软磁MnZn系功率铁氧体在25℃时的饱和磁通密度Bs大于550mT，在100℃时的饱和磁通密度Bs大于460mT；本发明的软磁MnZn系功率铁氧体在100kHz、200mT测试条件下，25℃时的功率损耗Pcv小于750kW/m3，100℃时的功率损耗Pcv小于320kW/m3。由此可见，本发明的软磁MnZn系功率铁氧体同时具备了高饱和磁通密度Bs和低损耗Pcv，具有非常好的市场前景。

Claims (2)

1.一种软磁MnZn系功率铁氧体，其特征是，包括主成分和副成分，所述的主成分包括Fe2O3、MnO、ZnO和NiO，以主成分的总量计算，Fe2O3占53.0-55.0mol％，ZnO占3.0-4.0mol％，NiO占0mol％，MnO为余量，所述的副成分包括CoO、SiO2、CaCO3、Nb2O5和ZrO2，所述的副成分包括第一副成分和第二副成分，所述的第一副成分为CoO，以主成分的总量计算为基础，CoO的含量为0-0.15wt％，在1194A/m的测试条件下，25℃时所述软磁MnZn系功率铁氧体的饱和磁通密度Bs大于550mT，100℃时所述软磁MnZn系功率铁氧体的饱和磁通密度Bs大于460mT；在100kHz、200mT的测试条件下，25℃时所述的软磁MnZn系功率铁氧体功率损耗Pcv小于750kW/m3，100℃时所述的软磁MnZn系功率铁氧体功率损耗Pcv小于320kW/m3。
2.根据权利要求1所述的一种软磁MnZn系功率铁氧体，其特征是，所述的第二副成分为SiO2、CaCO3、Nb2O5和ZrO2，以主成分的总量计算为基础，SiO2为0.005-0.015wt％、CaCO3为0.03-0.15wt％、Nb2O5为0.05-0.4wt％、ZrO2为0.05-0.4wt％。
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