CN111362685B - 一种高负温磁导率和低高温损耗的锰锌铁氧体及其制备方法 - Google Patents

一种高负温磁导率和低高温损耗的锰锌铁氧体及其制备方法 Download PDF

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CN111362685B
CN111362685B CN202010101797.XA CN202010101797A CN111362685B CN 111362685 B CN111362685 B CN 111362685B CN 202010101797 A CN202010101797 A CN 202010101797A CN 111362685 B CN111362685 B CN 111362685B
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sanding
manganese
zinc ferrite
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CN111362685A (zh
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吕东华
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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Priority to EP20919900.9A priority patent/EP4049987A4/en
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Abstract

本发明属于锰锌铁氧体材料技术领域。本发明公开了一种高负温磁导率和低高温损耗的锰锌铁氧体，其由Fe2O3、MnO和ZnO组成，同时还添加了由CaCO3、ZrO2、Co2O3和SnO2组成的添加剂。本发明通过Mn、Zn和Fe三种组分的合理调配及适当增加添加剂中Co含量获得了一种在‑20℃左右既具有高磁导率还具有低损耗并且在120～140℃仍具有低损耗的锰锌铁氧体材料；其在‑30～140℃温度范围内具有‑20℃左右及100℃左右两个损耗谷点，拓展了锰锌铁氧体材料的应用范围。

Description

一种高负温磁导率和低高温损耗的锰锌铁氧体及其制备方法
技术领域
本发明涉及锰锌铁氧体技术领域，尤其是涉及一种高负温磁导率和低高温损耗的锰锌铁氧体及其制备方法。
背景技术
随着时代的发展和社会的进步，节能减排和提高效率越来越被人们重视。同样的，对于磁性材料应用领域，降低损耗也是一种研究热点。现有技术中，日本TDK公司的PC47、PC45等铁氧体材料宣称具有较低的损耗，但是其都只是单点的低损耗，就目前来说尚不能满足当下的节能减排和提高效率的要求。TDK公司的PC95铁氧体材料相较于PC47和PC45具有更宽的低损耗温度区间，但是其也仅仅只是在25～100℃温度范围内具有较低的损耗；同样的，飞磁公司生产的3C97等材料也仅在60～140℃温度范围内具有较低的损耗；国内其他厂家的一些产品也是类似情况，如天通公司的TPW33和安磁的JPP97等铁氧体材料，但这些铁氧体材料也仅仅只能在高温区间具有较低的损耗，而对于低温甚至零下温度区间的磁导率则无法兼顾。
发明内容
为解决上述问题，本发明提供了一种既在-20℃左右温度范围具有高磁导率同时在120～140℃温度范围具有低损耗的锰锌铁氧体材料，满足电子元件在极端恶劣环境下的工作要求。
本发明还公开了一种上述锰锌铁氧体的制备方法。
为实现上述目的，本发明采用的技术方案如下：
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.35～52.45mol％，MnO的摩尔百分添加量为37.6～37.9mol％，ZnO的摩尔百分添加量为9.65～10.05mol％。
作为优选，还包含以下原料组成的添加剂，添加剂中，以预烧料(主料经过预烧后得到的粉料)的总重量计，CaCO3的重量百分添加量为0.06～0.10wt％，ZrO2的重量百分添加量为0.015～0.04wt％，Co2O3为的重量百分添加量为0.3～0.45wt％，SnO2的重量百分添加量为0.1～0.2wt％。
作为优选，添加剂在主料经混合预烧后制得预烧料后添加。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后进行预烧处理，制得预烧料；
c)向预烧料中加入添加剂并进行二次砂磨，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后压制成型制得标环，标环经过烧结制得锰锌铁氧体。
作为优选，粘结剂水溶液为浓度7～8wt％的聚乙烯醇溶液，粘结剂水溶液的添加量一次砂磨料浆中的粘结剂水溶液添加量为主料重量的8～12wt％，所述二次砂磨料浆中的粘结剂水溶液添加量为预烧料重量的8～12wt％。
作为优选，步骤a)中，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：(5～7)：(0.5～0.6)，砂磨时间为50～70分钟。
作为优选，步骤c)中，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：(5～7)：(0.4～0.5)，砂磨时间为120～160分钟。
作为优选，步骤b)中，预烧温度为900～920℃。
作为优选，步骤d)中，压制成型时压力为7～9MPa。
作为优选，步骤d)中，烧结温度为1280～1320℃。
现有的技术认为Co2O3含量提高的会降低-20℃的磁导率，而且不利于降低120～140℃的损耗，因为Co2O3含量高，会使谷点往低温方向移动。
本发明认为-20℃磁导率的高低与Co2O3含量高低没有必然的联系，影响-20℃磁导率的高低的核心因素是材料的磁晶各向异性常数K1。K1值小的磁导率高，K1值大的磁导率低；同时适当提高Co2O3含量，有利于降低120℃--140℃；本发明提供一种高Co2O3含量提高-20℃磁导率同时降低120℃--140℃损耗的方法，这与传统的高Co2O3含量会降低-20℃磁导率，提高120℃---140℃损耗的认知是完全不同的。
本发明的核心创新点在于，本发明可以提供损耗温度曲线具有双谷点的锰锌铁氧材料及其制备方法。具体来说就是要充分运用好材料的谷点，在谷点确定的情况下，加入适当高的Co2O3的量，来降低-20℃、120℃和140℃的磁晶各向异性常数K1。这里要充分说明一下所谓的谷点，与现有技术上的谷点有所区别，现有技术的谷点是指25℃--120℃范围内的损耗最低点，本发明的谷点除了现有技术上的所谓的谷点，还要增加-20℃左右的谷点。
因此，本发明具有以下有益效果：本发明通过Mn、Zn和Fe三种组分的合理调配及适当增加添加剂中Co含量获得了一种在-20℃左右既具有高磁导率还具有低损耗并且在120～140℃仍具有低损耗的锰锌铁氧体材料；其在-30～140℃温度范围内具有-20℃左右及100℃左右两个损耗谷点，拓展了锰锌铁氧体材料的应用范围。
附图说明
图1为本发明实施例1中制得的锰锌铁氧体材料-30℃～140℃温度范围内的损耗Pcv曲线。
具体实施方式
下面结合具体实施方式对本发明的技术方案作进一步的说明。
显然，所描述的实施例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它实施例，都属于本发明保护的范围。
在本发明中，若非特指，所有的设备和原料均可从市场上购得或是本行业常用的，下述实施例中的方法，如无特别说明，均为本领域常规方法。
实施例1
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.35mol％，MnO的摩尔百分添加量为37.6mol％，ZnO的摩尔百分添加量为10.05mol％；
还包含以下原料组成的添加剂，添加剂中，以预烧料的总重量计，CaCO3的重量百分添加量为0.08wt％，ZrO2的重量百分添加量为0.02wt％，Co2O3为的重量百分添加量为0.4wt％，SnO2的重量百分添加量为0.1wt％。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.55，砂磨时间为60分钟，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后在900℃进行预烧处理，制得预烧料；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为主料重量的10wt％；
c)向预烧料中加入添加剂并进行二次砂磨，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.45，砂磨时间为120分钟，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后在成型压力为8MPa下压制成型制得标环，标环在1300℃温度下经过烧结制得锰锌铁氧体；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为预烧料重量的10wt％。
实施例2
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.45mol％，MnO的摩尔百分添加量为37.9mol％，ZnO的摩尔百分添加量为9.65mol％；
还包含以下原料组成的添加剂，添加剂中，以预烧料的总重量计，CaCO3的重量百分添加量为0.08wt％，ZrO2的重量百分添加量为0.02wt％，Co2O3为的重量百分添加量为0.44wt％，SnO2的重量百分添加量为0.1wt％。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.55，砂磨时间为60分钟，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后在920℃进行预烧处理，制得预烧料；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为主料重量的10wt％；
c)向预烧料中加入添加剂并进行二次砂磨，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.45，砂磨时间为140分钟，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后在成型压力为8MPa下压制成型制得标环，标环在1300℃温度下经过烧结制得锰锌铁氧体；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为预烧料重量的10wt％。
实施例3
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.45mol％，MnO的摩尔百分添加量为37.8mol％，ZnO的摩尔百分添加量为9.75mol％；
还包含以下原料组成的添加剂，添加剂中，以预烧料的总重量计，CaCO3的重量百分添加量为0.06wt％，ZrO2的重量百分添加量为0.015wt％，Co2O3为的重量百分添加量为0.3wt％，SnO2的重量百分添加量为0.15wt％。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：5：0.5，砂磨时间为70分钟，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后在910℃进行预烧处理，制得预烧料；粘结剂水溶液为浓度7wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为主料重量的12wt％；
c)向预烧料中加入添加剂并进行二次砂磨，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：5：0.4，砂磨时间为160分钟，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后在成型压力为7MPa下压制成型制得标环，标环在1280℃温度下经过烧结制得锰锌铁氧体；粘结剂水溶液为浓度7wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为预烧料重量的12wt％。
实施例4
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.43mol％，MnO的摩尔百分添加量为37.65mol％，ZnO的摩尔百分添加量为9.92mol％；
还包含以下原料组成的添加剂，添加剂中，以预烧料的总重量计，CaCO3的重量百分添加量为0.07wt％，ZrO2的重量百分添加量为0.025wt％，Co2O3为的重量百分添加量为0.45wt％，SnO2的重量百分添加量为0.2wt％。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：7：0.6，砂磨时间为50分钟，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后在920℃进行预烧处理，制得预烧料；粘结剂水溶液为浓度8wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为主料重量的8wt％；
c)向预烧料中加入添加剂并进行二次砂磨，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：7：0.5，砂磨时间为120分钟，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后在成型压力为9MPa下压制成型制得标环，标环在1310℃温度下经过烧结制得锰锌铁氧体；粘结剂水溶液为浓度8wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为预烧料重量的8wt％。
实施例5
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.40mol％，MnO的摩尔百分添加量为37.90mol％，ZnO的摩尔百分添加量为9.70mol％；
还包含以下原料组成的添加剂，添加剂中，以预烧料的总重量计，CaCO3的重量百分添加量为0.10wt％，ZrO2的重量百分添加量为0.04wt％，Co2O3为的重量百分添加量为0.35wt％，SnO2的重量百分添加量为0.13wt％。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.55，砂磨时间为60分钟，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后在910℃进行预烧处理，制得预烧料；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为主料重量的10wt％；
c)向预烧料中加入添加剂并进行二次砂磨，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.45，砂磨时间为140分钟，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后在成型压力为8MPa下压制成型制得标环，标环在1300℃温度下经过烧结制得锰锌铁氧体；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为预烧料重量的10wt％。
实施例6
一种高负温磁导率和低高温损耗的锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.38mol％，MnO的摩尔百分添加量为37.85mol％，ZnO的摩尔百分添加量为9.77mol％；
还包含以下原料组成的添加剂，添加剂中，以预烧料的总重量计，CaCO3的重量百分添加量为0.09wt％，ZrO2的重量百分添加量为0.03wt％，Co2O3为的重量百分添加量为0.39wt％，SnO2的重量百分添加量为0.18wt％。
一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，包括以下步骤：
a)将主料中的各组分混合后进行一次砂磨，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.55，砂磨时间为60分钟，砂磨后制得砂磨料浆；
b)向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后在900℃进行预烧处理，制得预烧料；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为主料重量的10wt％；
c)向预烧料中加入添加剂并进行二次砂磨，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：6：0.45，砂磨时间为150分钟，砂磨后制得二次砂磨料浆；
d)向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后在成型压力为8MPa下压制成型制得标环，标环在1300℃温度下经过烧结制得锰锌铁氧体；粘结剂水溶液为浓度7.5wt％的聚乙烯醇溶液，粘结剂水溶液的添加量为预烧料重量的10wt％。
对比例1
锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.75mol％，MnO的摩尔百分添加量为37.2mol％，ZnO的摩尔百分添加量为10.05mol％。
本对比例中，锰锌铁氧体的添加剂及制备方法同实施例1。
对比例2
锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.25mol％，MnO的摩尔百分添加量为38.00mol％，ZnO的摩尔百分添加量为9.75mol％。
本对比例中，锰锌铁氧体的添加剂及制备方法同实施例1。
对比例3
锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.44mol％，MnO的摩尔百分添加量为37.96mol％，ZnO的摩尔百分添加量为9.60mol％。
本对比例中，锰锌铁氧体的添加剂及制备方法同实施例1。
对比例4
锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.35mol％，MnO的摩尔百分添加量为37.55mol％，ZnO的摩尔百分添加量为10.10mol％。
本对比例中，锰锌铁氧体的添加剂及制备方法同实施例1。
对比例5
锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.25mol％，MnO的摩尔百分添加量为37.75mol％，ZnO的摩尔百分添加量为10.00mol％。
本对比例中，锰锌铁氧体的添加剂及制备方法同实施例1。
对比例6
锰锌铁氧体，包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.55mol％，MnO的摩尔百分添加量为37.70mol％，ZnO的摩尔百分添加量为9.75mol％。
本对比例中，锰锌铁氧体的添加剂及制备方法同实施例1。
对比例7
锰锌铁氧体，其主料及制备方法同实施例1。
其添加剂如下：
以预烧料的总重量计，CaCO3的重量百分添加量为0.08wt％，ZrO2的重量百分添加量为0.02wt％，Co2O3为的重量百分添加量为0.20wt％，SnO2的重量百分添加量为0.1wt％。
对比例8
锰锌铁氧体，其主料及制备方法同实施例1。
其添加剂如下：
以预烧料的总重量计，CaCO3的重量百分添加量为0.08wt％，ZrO2的重量百分添加量为0.02wt％，Co2O3为的重量百分添加量为0.50wt％，SnO2的重量百分添加量为0.1wt％。
性能检测：
对上述各实施例及对比例中获得的锰锌铁氧体材料进行性能检测，其中检测项目包括-20℃下的磁导率μi，120℃及140℃下的损耗Pcv(100kHz 200mT)，如下表1所示。
并根据实际条件绘制实施例1中制得锰锌铁氧体材料-30℃～140℃温度范围内的损耗Pcv曲线，如图1所示。
表1
Figure BDA0002387109120000081
从表1可以得出，
1.对比例1中Fe2O3含量过高，并且MnO的含量偏低，导致其高温损耗偏高，-20℃磁导率远低于实施例中的样品；
2.对比例2中Fe2O3含量偏低，并且MnO的含量过高，导致其高温损耗偏高，-20℃磁导率远低于实施例中的样品，但略高于对比例1中样品；
3.对比例3中MnO含量过高，并且ZnO的含量偏低，导致其高温损耗偏高，-20℃磁导率远低于实施例中的样品；
4.对比例4中MnO含量偏低，并且ZnO的含量过高，导致其高温损耗偏高，-20℃磁导率远低于实施例中的样品，且低于对比例3中样品；
5.对比例5中Fe2O3的含量偏低，其高温损耗远高于实施例中制得的样品，同时-20℃磁导率也较低；
6.对比例6中Fe2O3的含量过高，其高温损耗远高于实施例中制得的样品，同时-20℃磁导率也较低，甚至低于对比例5中制得的样品；
7.对比例7中Co2O3含量偏低，导致高温损耗偏高，-20℃磁导率低；
8.对比例8中Co2O3含量过高，导致高温损耗偏高，-20℃磁导率严重降低，甚至低于对比例7中制得的样品。
应当理解的是，对于本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。

Claims (8)

1.一种高负温磁导率和低高温损耗的锰锌铁氧体，其特征在于包含以下原料组成的主料：
Fe2O3的摩尔百分添加量为52.35～52.45mol%，MnO的摩尔百分添加量为37.6～37.9mol%，ZnO的摩尔百分添加量为9.65～10.05mol%；
添加剂中，以主料经过预烧后得到粉料即预烧料的总重量计，CaCO3的重量百分添加量为0.06～0.10wt%，ZrO2的重量百分添加量为0.015～0.04wt%，Co2O3为的重量百分添加量为0.3～0.45wt%，SnO2的重量百分添加量为0.1～0.2wt%；
所述添加剂在主料经混合预烧制得预烧料后添加。
2.一种根据权利要求1所述的高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于包括以下步骤：
a）将主料中的各组分混合后进行一次砂磨，砂磨后制得砂磨料浆；
b）向砂磨料浆中加入粘结剂水溶液混匀并进行喷雾造粒，之后进行预烧处理，制得预烧料；
c）向预烧料中加入添加剂并进行二次砂磨，砂磨后制得二次砂磨料浆；
d）向二次砂磨料浆中加入粘结剂水溶液混匀并喷雾造粒，然后压制成型制得标环，标环经过烧结制得锰锌铁氧体。
3.根据权利要求2所述的一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于：
所述粘结剂水溶液为浓度7～8wt%的聚乙烯醇溶液，所述一次砂磨料浆中的粘结剂水溶液添加量为主料重量的8～12wt%，所述二次砂磨料浆中的粘结剂水溶液添加量为预烧料重量的8～12wt%。
4.根据权利要求2所述的一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于：
所述步骤a）中，一次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：（5～7）：（0.5～0.6），砂磨时间为50～70分钟。
5.根据权利要求2所述的一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于：
所述步骤c）中，二次砂磨中采用去离子水作为砂磨介质，料球水的重量比为1：（5～7）：（0.4～0.5），砂磨时间为120～160分钟。
6.根据权利要求2所述的一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于：
所述步骤b）中，预烧温度为900～920℃。
7.根据权利要求2所述的一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于：
所述步骤d）中，压制成型时压力为7～9MPa。
8.根据权利要求2所述的一种高负温磁导率和低高温损耗的锰锌铁氧体的制备方法，其特征在于：
所述步骤d）中，烧结温度为1280～1310℃。
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