CN113277841B - 超高频软磁铁氧体材料及磁芯的制备方法 - Google Patents

超高频软磁铁氧体材料及磁芯的制备方法 Download PDF

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CN113277841B
CN113277841B CN202110589898.0A CN202110589898A CN113277841B CN 113277841 B CN113277841 B CN 113277841B CN 202110589898 A CN202110589898 A CN 202110589898A CN 113277841 B CN113277841 B CN 113277841B
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soft magnetic
presintering
ferrite material
magnetic ferrite
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CN113277841A (zh
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黄刚
李崇华
廖继红
卢明超
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China Magnetic Electronic Technology Co ltd
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Abstract

本发明涉及软磁铁氧体技术领域，公开了超高频软磁铁氧体材料及磁芯的制备方法，所述主体成分按摩尔份数计，包括有：Fe2O367～69mol；BaCO323～25mol；片状Co3O47～9mol；相对所述主成分总量，各添加剂成分的重量百分比分别为：Na2CO3 100～400PPM；SrCO3100～800PPM；Sm2O330～100PPM；TiZn 100～300PPM；Li2CO3100～300PPM，本发明具有较高磁导率、低损耗、高频率的优点。

Description

超高频软磁铁氧体材料及磁芯的制备方法
技术领域
本发明涉及软磁铁氧体技术领域，特别涉及超高频软磁铁氧体材料及磁芯的制备方法。
背景技术
在实现了电阻、电容、半导体和光电器件集成化后，如何使得软磁材料应用在超高频段并实现磁性电子器件的集成，已经成为制约电子信息技术高频化和集成化的瓶颈。其主要原因就是，用于电感器、变压器的磁性材料在高频时磁导率下降，因此进一步提高磁导率、提高和加宽工作频率、降低损耗、满足宽温区间和微型化是未来的发展目标。
发明内容
本发明的目的是提供超高频软磁铁氧体材料及磁芯的制备方法，旨在解决超高频下磁导率低、损耗高的问题。
本发明的上述技术目的是通过以下技术方案得以实现的：
一种超高频软磁铁氧体材料，铁氧体粉料包括主体成分和添加剂成分，其中，
所述主体成分按摩尔份数计，包括有：
Fe2O3 67~69 mol；
BaCO3 23~25 mol；
片状Co3O4 7~9 mol；
相对所述主成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 100~400PPM；
SrCO3 100~800PPM；
Sm2O3 30~100PPM；
TiZn 100~300PPM；
Li2CO3 100~300PPM；
纳米SiO2 50~100PPM。
在以上技术方案的基础上，优选的，所述纳米SiO2的颗粒尺寸范围为50~100nm。
本发明提供一种超高频软磁铁氧体磁芯，采用上述的超高频软磁铁氧体材料制备而成。
在其中一实施例中，所述超高频软磁铁氧体磁芯的晶粒尺寸为3μm-4μm，起始磁导率μi达到35以上，高温100℃、1GHz、30mT 条件下功率损耗在400kW/m3以下，100℃Bs值在380mT以上。
一种超高频软磁铁氧体磁芯的制备方法，包括以下步骤：
S1，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各主成分，再将各主成分混合，经湿式球磨、烘干、预烧、研磨得到M型和Y型钡铁氧体磁粉；
S2，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、模压、烧结，即得。
在其中一实施例中，所述S1步骤中，在预烧工序之前加入助熔剂。
在其中一实施例中，所述S1和S2步骤中，湿式球磨工序使用超硬锆球。
在其中一实施例中，所述S3步骤中，所用粘结剂为PPS树脂。
在其中一实施例中，所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
上述任一项所述的超高频软磁铁氧体材料在以高频开关电源为代表的电子元器件、超高频(GHz)频段的抗电磁干扰元件、可在高频工作的电感器、变压器。
与现有技术相比，本发明的有益效果在于：
1.平面型六角结构铁氧体适合应用于超高频的情况，尤其是Z型六角铁氧体材料，其中Co2Z 六角铁氧体材料根据前人研究其应用频率范围明显向高频方向移动。碱金属的碳酸盐对Co2Z 材料的共振频率有明显的提高作用，加入Na2CO3可使Co2Z 材料的频带得到显著扩展，避免Co2Z 材料实际达到的共振频率与理论值差距较大；Sm3+为稀土元素，低熔点的Sm2O3产生了液相烧结，有助于提高密度，与Sr（Sr取代Ba+）复合使用，所得截止频率较高，其磁导率在两者之间，再与Li+和TiZn（Zn低熔点，促进液相烧结，可促进晶粒长大并趋于完整，晶界变薄，气孔率降低，从而使畴壁位移和畴壁转动的阻力下降，从而可使起始磁导率上升，但使截止频率下降；Li+取代Co+，可使磁导率大幅提高）联合使用，使起始磁导率提高，而使截止频率也保持在较高水平，同时可掺杂SiO2进一步使磁导率提高，同时Li+或TiZn使之为单向Z型铁氧体，几种添加剂成分综合作用，获得具有较高磁导率、低损耗、高频率以及高品质因数的Co2Z 材料；
2.采用纳米级尺度的SiO2粉体代替原微米尺寸的粉体，有利于更好地控制晶粒尺寸即材料的显微结构，进而可以制备出密度高、晶粒细小均匀的纳米材料，从而可满足近年来电子产品向超薄微型化发展而对软磁铁氧体提出了更小体积、更高功效的要求；
3.采用两步法，使晶粒尺寸增大，同时气孔率下降，烧结密度增大，从而使磁矩增大，从而使饱和磁感应强度（Bs）增大，同时两步法可对用于产生的Z型钡铁氧体材料的M型和Y型钡铁氧体磁粉的量直接进行控制，使其按在一定比例下发生相转变，从而获得纯度高的单向六角Z型钡铁氧体材料，一定程度上克服Co2Z 材料成相温度高、范围窄的问题；
4.PPS树脂填充通过选择填充物质和填充量，可以获得超高频软磁材料，同时不仅改善了磁导率的频率特性还改善了磁导率的温度特性；湿式球磨工序使用超硬锆球，可防止使用球磨罐和钢球中的含铁的物质将会进入到粉料中，导致粉料中铁含量变大；使用的Co3O4为片状粉料，有利于主晶相转变为Z相。
5.Ba在高温下易挥发，加入助熔剂CuO-Bi2O3（5.0wt%CuO和5.0wt%Bi2O3）可促进液相烧结，可降低预烧温度，从而防止其消耗，同时较低的预烧温度使预烧料具有较高的反应活性，从而使其在烧结步骤中进行固相反应。
6.最终产品的晶粒尺寸为3μm-4μm，起始磁导率μi达到900以上，高温100℃、5MHz、30mT 条件下功率损耗在250kW/m3以下，100℃Bs值在390mT以上。
具体实施方式
下面将结合具体实施例对本发明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的一部分实施例，而不是全部的实施例。基于本发明的实施例，本领域普通技术人员在没有作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
本实施例提供一种超高频软磁铁氧体材料，
所述主体成分按摩尔份数计，包括有：
Fe2O3 67 mol
BaCO3 25 mol
片状Co3O4 7 mol
相对所述主成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 400PPM
SrCO3 100PPM
Sm2O3 100PPM
TiZn 100PPM
Li2CO3 100PPM
纳米SiO2 100PPM
所述纳米SiO2的尺寸为50-100nm。
一种超高频软磁铁氧体磁芯的制备方法，包括以下步骤：
S1，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各主成分，再将各主成分混合，经湿式球磨、烘干、预烧、研磨得到M型和Y型钡铁氧体磁粉；
S2，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、模压、烧结，即得。
所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
所述S1步骤中，在预烧工序之前加入助熔剂，所述S1和S2步骤中，湿式球磨工序使用超硬锆球，所述S3步骤中，所用粘结剂为PPS树脂。
实施例2
所述主体成分按摩尔份数计，包括有：
Fe2O3 69 mol
BaCO3 23 mol
片状Co3O4 9 mol
相对所述主成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 100PPM
SrCO3 800PPM
Sm2O3 30PPM
TiZn 300PPM
Li2CO3 300PPM
纳米SiO2 50PPM
所述纳米SiO2的尺寸为50-100nm。
一种超高频软磁铁氧体磁芯的制备方法，包括以下步骤：
S1，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各主成分，再将各主成分混合，经湿式球磨、烘干、预烧、研磨得到M型和Y型钡铁氧体磁粉；
S2，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、模压、烧结，即得。
所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
所述S1步骤中，在预烧工序之前加入助熔剂，所述S1和S2步骤中，湿式球磨工序使用超硬锆球，所述S3步骤中，所用粘结剂为PPS树脂。
实施例3
所述主体成分按摩尔份数计，包括有：
Fe2O3 68 mol
BaCO3 24 mol
片状Co3O4 8 mol
相对所述主成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 300PPM
SrCO3 600PPM
Sm2O3 50PPM
TiZn 200PPM
Li2CO3 200PPM
纳米SiO2 70PPM
所述纳米SiO2的尺寸为50-100nm。
一种超高频软磁铁氧体磁芯的制备方法，包括以下步骤：
S1，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各主成分，再将各主成分混合，经湿式球磨、烘干、预烧、研磨得到M型和Y型钡铁氧体磁粉；
S2，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、模压、烧结，即得。
所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
所述S1步骤中，在预烧工序之前加入助熔剂，所述S1和S2步骤中，湿式球磨工序使用超硬锆球，所述S3步骤中，所用粘结剂为PPS树脂。
实施例4
所述主体成分按摩尔份数计，包括有：
Fe2O3 69 mol
BaCO3 23 mol
片状Co3O4 8 mol
相对所述主成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 350PPM
SrCO3 500PPM
Sm2O3 40PPM
TiZn 150PPM
Li2CO3 150PPM
纳米SiO2 60PPM
所述纳米SiO2的尺寸为50-100nm。
一种超高频软磁铁氧体磁芯的制备方法，包括以下步骤：
S1，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各主成分，再将各主成分混合，经湿式球磨、烘干、预烧、研磨得到M型和Y型钡铁氧体磁粉；
S2，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、模压、烧结，即得。
所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
所述S1步骤中，在预烧工序之前加入助熔剂，所述S1和S2步骤中，湿式球磨工序使用超硬锆球，所述S3步骤中，所用粘结剂为PPS树脂。
实施例5
所述主体成分按摩尔份数计，包括有：
Fe2O3 67 mol
BaCO3 25 mol
片状Co3O4 8 mol
上述成分为分析纯级，各主成分的配比总计为100mol%
相对所述主成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 250PPM
SrCO3 700PPM
Sm2O3 70PPM
TiZn 250PPM
Li2CO3 250PPM
纳米SiO2 80PPM
所述纳米SiO2的尺寸为50-100nm。
一种超高频软磁铁氧体磁芯的制备方法，包括以下步骤：
S1，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各主成分，再将各主成分混合，经湿式球磨、烘干、预烧、研磨得到M型和Y型钡铁氧体磁粉；
S2，根据上述任一项所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、模压、烧结，即得。
所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
所述S1步骤中，在预烧工序之前加入助熔剂，所述S1和S2步骤中，湿式球磨工序使用超硬锆球，所述S3步骤中，所用粘结剂为PPS树脂。
对各实施例得到的磁芯进行测试，得到以下结果：
表1性能测试统计表
Figure DEST_PATH_IMAGE001
可以看出，最终产品的晶粒尺寸为3μm-4μm，起始磁导率μi达到900以上，高温100℃、5MHz、30mT 条件下功率损耗在250kW/m3以下，100℃Bs值在390mT以上。
需要说明的是，本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。
上述描述仅是对本发明较佳实施例的描述，并非对本发明范围的任何限定，本发明领域的普通技术人员根据上述揭示内容做的任何变更、修饰，均属于权利要求书的保护范围。

Claims (8)

1.一种超高频软磁铁氧体材料，其特征在于：铁氧体粉料包括主体成分和添加剂成分，其中，
所述主体成分按摩尔份数计，包括有：
Fe2O3 67~69 mol；
BaCO3 23~25 mol；
片状Co3O4 7~9 mol；
相对所述主体成分总量，各添加剂成分的重量百分比分别为：
Na2CO3 100~400PPM；
SrCO3 100~800PPM；
Sm2O3 30~100PPM；
TiZn 100~300PPM；
Li2CO3 100~300PPM；
纳米SiO2 50~100PPM；
采用所述铁氧体粉料制备磁芯的方法，包括以下步骤：
S1，根据以上所述的超高频软磁铁氧体材料的用量称量各主体成分，再将各主体成分混合，经湿式球磨、烘干、预烧、研磨、过筛得到M型和Y型钡铁氧体磁粉；
S2，根据以上所述的超高频软磁铁氧体材料的用量称量各添加剂成分，对步骤S1得到的M型和Y型钡铁氧体磁粉按1：1 称量并与添加剂成分混合，经湿式球磨、烘干、预烧；
S3，加入粘结剂，经研磨、过筛、模压、烧结，即得。
2.根据权利要求1所述的超高频软磁铁氧体材料，其特征在于：所述纳米SiO2的颗粒尺寸范围为50~100nm。
3.根据权利要求1所述的超高频软磁铁氧体材料，其特征在于：最终产品的晶粒尺寸为3μm-4μm，起始磁导率μi达到900以上，高温100℃、5MHz、30mT 条件下功率损耗在250kW/m3以下，100℃Bs值在390mT以上。
4.根据权利要求1所述的超高频软磁铁氧体材料，其特征在于：所述S1步骤中，在预烧工序之前加入助熔剂，所述助熔剂为CuO-Bi2O3。
5.根据权利要求1所述的超高频软磁铁氧体材料，其特征在于：所述S1和S2步骤中，湿式球磨工序使用超硬锆球。
6.根据权利要求1所述的超高频软磁铁氧体材料，其特征在于：所述S3步骤中，所用粘结剂为PPS树脂。
7.根据权利要求4所述的超高频软磁铁氧体材料，其特征在于：所述S1步骤中的工艺参数为：湿式球磨时间2h，在氧气中预烧，预烧温度为950℃，升温速率为1℃/min，预烧时间为3 h；所述S2步骤中的工艺参数为：湿式球磨时间为2h，在氧气中预烧，预烧温度为950℃，预烧时间为3 h；所述S3步骤中的工艺参数为：烧结温度为1250℃，降温速率为1℃/min，烧结时间为2h。
8.根据权利要求1所述的超高频软磁铁氧体材料在以高频开关电源为代表的电子元器件、超高频频段的抗电磁干扰元件、可在高频工作的电感器、变压器的应用。
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