CN110517840A - 一种高频宽温低损耗MnZn铁氧体材料及其制备方法 - Google Patents

一种高频宽温低损耗MnZn铁氧体材料及其制备方法 Download PDF

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CN110517840A
CN110517840A CN201910737879.0A CN201910737879A CN110517840A CN 110517840 A CN110517840 A CN 110517840A CN 201910737879 A CN201910737879 A CN 201910737879A CN 110517840 A CN110517840 A CN 110517840A
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ferrite material
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韩奎
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Jingshi Magnetic Materials & Element Engineering Tech Research Co Ltd
Wuxi Spinel Magnetics Co Ltd
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Jingshi Magnetic Materials & Element Engineering Tech Research Co Ltd
Wuxi Spinel Magnetics Co Ltd
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Abstract

本发明公开了一种高频宽温低损耗MnZn铁氧体材料，所述铁氧体材料是四元系FeMnZnNi铁氧体材料，由主成份和辅助成份组成，其中主成份的组成为71～77.4mol％的Fe2O3，2～13.8mol％的ZnO，0.001～1mol％的Ni2O3，余量为Mn3O4；按主成份总重量计，辅助成份的组成为CaCO3：200～2000ppm、Nb2O5：0～500ppm、V2O5：0～500ppm、SnO2：0～1000ppm、TiO2：0～2000ppm、ZrO2：0～200ppm、Ta2O5：0～200ppm、GeO2：0～1000ppm、Co3O4：0～3000ppm、Bi2O3：0～1000ppm、SiO2：0～200ppm；还有其制备方法。该材料不含成本较高的In2O，通过有效控制配方、烧结工艺，所得材料可以达到：初始磁导率900+25％，25℃饱和磁通密度≥530mT，500kHz/50mT宽温下损耗≤80mW/cm3，1MHz/50mT宽温下损耗≤170mW/cm3，3MHz/30mT宽温下损耗≤570mW/cm3，5MHz/10mT宽温下损耗≤260mW/cm3，高频(500kHz～5MHz)、宽温(‑30～140℃)下的损耗、常高温的磁通密度有较大提升，扩大了温度使用区间，提高了在极寒地区的使用能力。

Description

一种高频宽温低损耗MnZn铁氧体材料及其制备方法
技术领域
本发明属于锰锌铁氧体技术领域，具体涉及一种高频宽温低损耗MnZn铁氧体材料及其制备方法。
背景技术
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的电源变压器材料，近些年市场对电子器件的高频化、小型化应用提出强烈需求，高Bs有利于电子产品的小型化，高频低损耗可有效降低器件的工作效率。
在专利方面，CN109095915A公开的MnZn铁氧体材料应用温度范围仅限3MHz～5MHz的频率区间和20℃～120℃的温度区间具有超低损耗，而且含有成本较高的In2O；CN107129291B公开的MnZn软磁铁氧体损耗偏高。
发明内容
本发明的第一个目的是为了克服上述缺陷，提供一种高频宽温低损耗MnZn铁氧体材料。
本发明的第二个目的是为了提供上述材料的制备方法。
本发明的目的通过以下技术方案来具体实现：
一种高频宽温低损耗MnZn铁氧体材料，所述铁氧体材料是四元系FeMnZnNi铁氧体材料，由主成份和辅助成份组成，其中主成份的组成为71～77.4mol％的Fe2O3，2～13.8mol％的ZnO，0.001～1mol％的Ni2O3，余量为Mn3O4；按主成份总重量计，辅助成份的组成为CaCO3：200～2000ppm、Nb2O5：0～500ppm、V2O5：0～500ppm、SnO2：0～1000ppm、TiO2：0～2000ppm、ZrO2：0～200ppm、Ta2O5：0～200ppm、GeO2：0～1000ppm、Co3O4：0～3000ppm、Bi2O3：0～1000ppm、SiO2：0～200ppm。
作为优选的，所述主成份中含有0.01～0.8mol％的Ni2O3。
进一步优选的，所述主成份中含有0.02～0.2mol％的Ni2O3。
上述高频宽温低损耗MnZn铁氧体材料的制备方法，括如下步骤：
(1)一次配料
按比例称量Fe2O3、Mn3O4、ZnO、Ni2O3主成分并混合均匀；
(2)一次烧结
将步骤(1)混合后的粉料放入预烧炉中，在900℃空气气氛下保温2h，随炉冷却得到一次烧结粉料；
(3)二次配料、砂磨
向步骤(2)的一次烧结粉料中添加CaCO3、Nb2O5、V2O5、SnO2、TiO2、ZrO2、Ta2O5、GeO2、Co3O4、Bi2O3、SiO2中的一种或多种辅助成分；然后将粉料放入行星磨，砂磨60min；
(4)喷雾造粒、成型
向步骤(3)的砂磨料中加入PVA、消泡剂，然后在喷雾塔中进行喷雾造粒；压制标准样环，标准样环生坯的压制密度为3.0～3.2g/cm3；
(5)二次烧结
烧结温度为1000～1200℃，在1％～6％的氧分压下保温4～10h；从保温段降至室温，按照平衡气氛曲线方程控制氧含量，降温速度为0.5～3℃/min。
本发明具有以下有益效果：
本发明提供的高频宽温低损耗MnZn铁氧体材料，不含成本较高的In2O，通过有效控制配方、烧结工艺，所得材料可以达到：初始磁导率900±25％，25℃饱和磁通密度≥530mT，500kHz/50mT宽温下损耗≤80mW/cm3，1MHz/50mT宽温下损耗≤170mW/cm3，3MHz/30mT宽温下损耗≤570mW/cm3，5MHz/10mT宽温下损耗≤260mW/cm3，高频(500kHz～5MHz)、宽温(-30～140℃)下的损耗、常高温的磁通密度有较大提升，扩大了温度使用区间，提高了在极寒地区的使用能力。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
本发明实施例中的原料均为市场可得产品。
实施例1
选用的主成分的含量以氧化物计为：Fe2O3：74.68mol％、ZnO：7.21mol％、Ni2O3:0.2mol％、余量Mn3O4，混合均匀。在900℃空气中预烧2h得到预烧料；向预烧料中加入按主成分总量计的副成分，副成分含量以氧化物计算为CaCO3：1000ppm、Nb2O5：300ppm、V2O5：300ppm、SnO2：500ppm、TiO2：800ppm、Ta2O5：200ppm、GeO2：200ppm、Co3O4：2000ppm、SiO2：150ppm，并加入适量的去离子水放入行星磨球磨1h，得到粒径0.7～1.2μm的粉体颗粒；将球磨后的料浆烘干后加入PVA、消泡剂造粒；压制标准样环生坯的压制密度为3.0～3.2g/cm3；放入钟罩炉中烧结，保温温度为1120℃，在1.0％氧含量中保温8h，随后按照平衡气氛曲线冷却出炉，降温速度为0.5～3℃/min，得到标准圆环供测试。测量采用日本岩崎8218-BH测试仪。
实施例1制备得到的MnZn软磁铁氧体材料性能如下
实施例2
选用的主成分的含量以氧化物计为：Fe2O3：73.73mol％、ZnO：7.26mol％、Ni2O3:0.9mol％、余量Mn3O4，其它辅助成分及制备工艺同实施例1。
实施例2制备得到的MnZn软磁铁氧体材料性能如下:
由实施例2可见过量的增加Ni2O3摩尔比会增加材料在500kHz～1MHz下损耗，在3MHz～5MHz下的损耗更高。
实施例3
选用的主成分的含量以氧化物计为：Fe2O3：74.2mol％、ZnO：8.2mol％、Ni2O3:0.07mol％、余量Mn3O4，混合均匀。在900℃空气中预烧2h得到预烧料；向预烧料中加入按主成分总量计的副成分，副成分含量以氧化物计算为CaCO3：1500ppm、Nb2O5：200ppm、V2O5：100ppm、TiO2：1100ppm、ZrO2：200ppm、Bi2O3：100ppm、GeO2：100ppm、Co3O4：2500ppm、SiO2：120ppm，并加入适量的去离子水放入行星磨球磨1h，得到粒径0.7～1.2μm的粉体颗粒；将球磨后的料浆烘干后加入PVA、消泡剂造粒；压制标准样环生坯的压制密度为3.0～3.2g/cm3；放入钟罩炉中烧结，保温温度为1150℃，在1.2％氧含量中保温6h，随后按照平衡气氛曲线冷却出炉，降温速度为0.5～3℃/min，得到标准圆环供测试。
实施例3制备得到的MnZn软磁铁氧体材料性能如下
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (4)

1.一种高频宽温低损耗MnZn铁氧体材料，其特征在于，所述铁氧体材料是四元系FeMnZnNi铁氧体材料，由主成份和辅助成份组成，其中主成份的组成为71～77.4mol％的Fe2O3，2～13.8mol％的ZnO，0.001～1mol％的Ni2O3，余量为Mn3O4；按主成份总重量计，辅助成份的组成为CaCO3：200～2000ppm、Nb2O5：0～500ppm、V2O5：0～500ppm、SnO2：0～1000ppm、TiO2：0～2000ppm、ZrO2：0～200ppm、Ta2O5：0～200ppm、GeO2：0～1000ppm、Co3O4：0～3000ppm、Bi2O3：0～1000ppm、SiO2：0～200ppm。
2.根据权利要求1所述的高频宽温低损耗MnZn铁氧体材料，其特征在于，所述主成份中含有0.01～0.8mol％的Ni2O3。
3.根据权利要求2所述的高频宽温低损耗MnZn铁氧体材料，其特征在于，所述主成份中含有0.02～0.2mol％的Ni2O3。
4.权利要求1-3任一项所述的高频宽温低损耗MnZn铁氧体材料的制备方法，其特征在于，包括如下步骤：
(1)一次配料
按比例称量Fe2O3、Mn3O4、ZnO、Ni2O3主成分并混合均匀；
(2)一次烧结
将步骤(1)混合后的粉料放入预烧炉中，在900℃空气气氛下保温2h，随炉冷却得到一次烧结粉料；
(3)二次配料、砂磨
向步骤(2)的一次烧结粉料中添加CaCO3、Nb2O5、V2O5、SnO2、TiO2、ZrO2、Ta2O5、GeO2、Co3O4、Bi2O3、SiO2中的一种或多种辅助成分；然后将粉料放入行星磨，砂磨60min；
(4)喷雾造粒、成型
向步骤(3)的砂磨料中加入PVA、消泡剂，然后在喷雾塔中进行喷雾造粒；压制标准样环，标准样环生坯的压制密度为3.0～3.2g/cm3；
(5)二次烧结
烧结温度为1000～1200℃，在1％～6％的氧分压下保温4～10h；从保温段降至室温，按照平衡气氛曲线方程控制氧含量，降温速度为0.5～3℃/min。
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