CN107140967A - 一种MgMnZn系铁氧体及其制备工艺 - Google Patents

一种MgMnZn系铁氧体及其制备工艺 Download PDF

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CN107140967A
CN107140967A CN201710397989.8A CN201710397989A CN107140967A CN 107140967 A CN107140967 A CN 107140967A CN 201710397989 A CN201710397989 A CN 201710397989A CN 107140967 A CN107140967 A CN 107140967A
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mgmnzn
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陈丽莎
章志明
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Abstract

本发明公开了一种MgMnZn系铁氧体，其特征在于：所述MgMnZn系铁氧体，按质量份计算，是用5～18份氧化镁、9～21份氧化锌，50～70份氧化铁、0.01～1份氧化镍、5～10份碳酸镁和5～10份碳酸锰制备而成。本发明的MgMnZn系铁氧体提高了材料的上限使用频率，拓宽了材料的吸波频率的范围。

Description

一种MgMnZn系铁氧体及其制备工艺
技术领域
本发明涉及一种MgMnZn系铁氧体及其制备工艺，特别是一种用于制作抗干扰磁芯的 MgMnZn 系铁氧体及其制备工艺。
背景技术
现在的电子信息设备需要抗电磁干扰的频率范围是1MHz到1000MHz，而目前常用的MgZn铁氧体、NiZn铁氧体、MnZn铁氧体、CuZn铁氧体，由于铁氧体中金属离子种类的不同，对电磁波的吸收各有优势但在使用频率或阻抗方面也存在相应的不足。如MnZn铁氧体的特点是高，一般在2000～15000，其缺点是和在临界频率fc以上迅速下降，因而抑制电磁干扰的频率范围较窄。此外，其表面电阻率低，因此常用的MnZn主要使用于30M以下频率，常用的是1M以下频率； NiZn铁氧体常用的使用频率在200M以下，经掺CuO后制成的NiCuZn铁氧体可以使用到1GHz，但其阻抗值不高。NiZn铁氧体通过掺杂等方法改性，品种很多，从几十到2000。一般在临界频率fc以上和下降得比锰锌铁氧体慢一些，表面电阻率高。而Mg铁氧体能在更高的频率下使用。因此，需要设计一种宽频带抗电磁干扰复合体系材料，从而有效拓宽吸收噪音电磁波的频率范围。
发明内容
本发明的目的在于，提供一种MgMnZn系铁氧体及其制备工艺，从而有效拓宽吸收噪音电磁波的频率范围。
本发明的技术方案：一种MgMnZn系铁氧体，其特征在于：所述MgMnZn系铁氧体，按质量份计算，是用5～18份氧化镁、9～21份氧化锌，50～70份氧化铁、0.01～1份氧化镍、5～10份碳酸镁和5～10份碳酸锰制备而成。
前述的MgMnZn系铁氧体，所述氧化镍为纳米级氧化镍。
前述的MgMnZn系铁氧体，所述铁氧体的气孔率为1.9％～2.1％，居里点大于120℃，电阻率大于107欧姆•厘米，在1khz，25℃时的初始磁导率为600±25％，在H＝1600A/m的磁场中，25℃时的饱和磁通密度大于2600m/A，在200MHz、300MHz、500MHz中阻抗值都分别大于200。
前述的MgMnZn系铁氧体的制备工艺，所述MgMnZn系铁氧体是按以下步骤制备的：
A、将氧化镁、氧化镍和90%的氧化铁、氧化锌和碳酸锰依次加入到混料机中进行混合后，升温至960℃下预烧30分钟，得到经预烧的粉料，为A品；
B、在A品中添加10%的氧化铁、氧化锌和碳酸镁后，进行二次粉碎，加入粘合剂混合，采用喷雾造粒法得到平均直径为0.1～0.8mm的颗粒，为B品；
C、将B品烘干后压制成型，并进行修整得到成型体，为C品；
D、将C品在1250～1350℃下烧结2～3小时，降温，即得。
前述的MgMnZn系铁氧体的制备方法， A步骤中的混合后升温过程中，在升温的温度在100℃至450℃之间是缓慢升温。
与现有技术相比，本发明根据单一铁氧体材料对不同频率的噪音电磁波的吸收频率范围和单一材料的铁磁共振频率不同的原理，利用不同铁氧体的铁磁共振频率不同，形成的抗电磁干扰的频率范围不一样的特点，将MgZn铁氧体、NiZn铁氧体、MnZn铁氧体、CuZn铁氧体成分的材料进行复合形成复合铁氧体材料，通过大量的实验找到了合理的成分比例和适宜此材料形成的工艺技术。复合铁氧体材料中能够使铁氧体在烧结过程中析出微晶，在块状材料内部形成微小颗粒，同时阻止晶粒的长大，达到在材料内部既有纳米晶，又有亚微米晶和亚米晶，即同一种材料内部由不同结构大小的晶粒组成，它们的铁磁共振频率点不一样，如此可以吸收不同的噪音的电磁波，满足了信号连接线对噪音电磁波的吸收的要求。这样就提高材料的上限使用频率，拓宽了材料的吸波频率的范围。
此外，本发明的制备工艺在配料时改变传统一次加入原材料的工艺，采用两步添加原材料，在二次粉碎时添加少量剩余的Fe2O3、ZnO和MgCO3加入，使MgZn更有效地均匀地分布在MnZn铁氧体的表面，使材料在1MHz600MHz之间的阻抗值提高2%以上，同时采用低温预烧（预烧温度960℃）工艺，既节约了能源，同时增加了烧结后产品的密度。
具体实施方式
下面实施例对本发明作进一步的说明，但并不作为对本发明限制的依据。
实施例：
将10g氧化镁、0.5g氧化镍和54g的氧化铁、12g氧化锌和5g碳酸锰依次加入到混料机中进行混合后，升温至960℃下预烧30分钟，其中，在升温的温度在100℃至450℃之间是缓慢升温，得到经预烧的粉料，为A品；
在A品中添加6g氧化铁、2g氧化锌和5g碳酸镁后，进行二次粉碎，加入粘合剂混合，采用喷雾造粒法得到平均直径为0.1～0.8mm的颗粒，为B品；
将B品烘干后压制成型，并进行修整得到成型体，为C品；
将C品在1250～1350℃下烧结2～3小时，降温，即得本发明的 MgMnZn 系铁氧体。
本发明根据单一铁氧体材料对不同频率的噪音电磁波的吸收频率范围和单一材料的铁磁共振频率不同的原理，利用不同铁氧体的铁磁共振频率不同，形成的抗电磁干扰的频率范围不一样的特点，将MgZn铁氧体、NiZn铁氧体、MnZn铁氧体、CuZn铁氧体成分的材料进行复合形成复合铁氧体材料，通过大量的实验找到了合理的成分比例和适宜此材料形成的工艺技术。我们发现，复合铁氧体材料中能够使铁氧体在烧结过程中析出微晶，在块状材料内部形成微小颗粒，同时阻止晶粒的长大，达到在材料内部既有纳米晶，又有亚微米晶和亚米晶，即同一种材料内部由不同结构大小的晶粒组成，它们的铁磁共振频率点不一样，如此可以吸收不同的噪音的电磁波，满足了信号连接线对噪音电磁波的吸收的要求。这样就提高材料的上限使用频率，拓宽了材料的吸波频率的范围。
此材料有效地拓宽了抗电磁干扰的频率范围并形成多个铁磁共振频率点，其在200MHz、300MHz、500MHz中阻抗值都分别大于200。
目前采用的铁氧体干法制造工艺是根据配方进行配料（将主要原材料和微量元素都在此工艺进行添加），再经过混合、预烧、二次粉碎，然后造粒、成型、烧结、检验。如按传统工艺，原材料一次性加入，在预烧的过程中，由于原材料均匀的混合，工艺烧结曲线采用缓慢加热，保温时间加长，使形成的MnZn铁氧体是完整的铁氧体晶粒，这样在材料中的铁氧体结构和化学成分基本上是一致的，其晶粒大小基本一致，能为铁氧体提供很好的磁性能，但这种结构在高频状态下不能体现很好的磁性能，其主要的原因是阻抗值低，不能用于高频。
本发明采用两步添加原材料，使在MnZn铁氧体的颗粒上形成了MgZn铁氧体，MgZn铁氧体具有很高的阻值，同时，在铁氧体颗粒与颗粒之间还存在一定的尖隙和大小不均匀的MgZn铁氧体颗粒，这种结构有利于铁氧体向高频方向扩展，从而使本铁氧体材料可以用于很宽的频带。具体的过程是在配料时将主要原材料Fe2O3（部分）、ZnO（部分）、MgO（部分）、MnCO3、NiO在此工艺添加，采用低温预烧（预烧温度960℃），使其在预烧的过程中，使这些配好的原材料尽量形成尖晶石结构的铁氧体。在粉碎时，将少量剩余的Fe2O3、ZnO和MgCO3加入，这样没有经过预烧的材料形成的铁氧体将填充于预烧的铁氧体晶粒之间，同时，没有经过预烧的材料在反应过程中MnCO3进行分解，形成MnO+CO2，由于CO2的溢出，在材料中形成微小的气孔，这样就形成了材料内部成分不均匀的颗粒和气孔，从而达到了提高材料的阻抗值、拓宽吸收频率的范围、提高铁磁共振频率的目的。

Claims (5)

1.一种MgMnZn系铁氧体，其特征在于：所述MgMnZn系铁氧体，按质量份计算，是用5～18份氧化镁、9～21份氧化锌，50～70份氧化铁、0.01～1份氧化镍、5～10份碳酸镁和5～10份碳酸锰制备而成。
2.根据权利要求1所述的MgMnZn系铁氧体，其特征在于：所述氧化镍为纳米级氧化镍。
3.根据权利要求1所述的MgMnZn系铁氧体，其特征在于：所述铁氧体的气孔率为1.9％～2.1％，居里点大于120℃，电阻率大于107欧姆•厘米，在1khz，25℃时的初始磁导率为600±25％，在H＝1600A/m的磁场中，25℃时的饱和磁通密度大于2600m/A，在200MHz、300MHz、500MHz中阻抗值都分别大于200。
4.根据权利要求1、2或3所述的MgMnZn系铁氧体的制备工艺，其特征在于，所述MgMnZn系铁氧体是按以下步骤制备的：
A、将氧化镁、氧化镍和90%的氧化铁、氧化锌和碳酸锰依次加入到混料机中进行混合后，升温至960℃下预烧30分钟，得到经预烧的粉料，为A品；
B、在A品中添加10%的氧化铁、氧化锌和碳酸镁后，进行二次粉碎，加入粘合剂混合，采用喷雾造粒法得到平均直径为0.1～0.8mm的颗粒，为B品；
C、将B品烘干后压制成型，并进行修整得到成型体，为C品；
D、将C品在1250～1350℃下烧结2～3小时，降温，即得。
5.根据权利要求4所述的MgMnZn系铁氧体的制备方法，其特征在于：A步骤中的混合后升温过程中，在升温的温度在100℃至450℃之间是缓慢升温。
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CN109095914A (zh) * 2018-11-01 2018-12-28 沅陵辰州磁电高科有限公司 镁锰锌软磁材料
CN114014643A (zh) * 2021-10-12 2022-02-08 江西瑞吉磁电子科技有限公司 一种抗干扰、耐高压磁芯材料及其制备方法

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