CN109320230B - 一种具有四高特性的锰锌软磁铁氧体材料的制备方法 - Google Patents

一种具有四高特性的锰锌软磁铁氧体材料的制备方法 Download PDF

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CN109320230B
CN109320230B CN201811181735.3A CN201811181735A CN109320230B CN 109320230 B CN109320230 B CN 109320230B CN 201811181735 A CN201811181735 A CN 201811181735A CN 109320230 B CN109320230 B CN 109320230B
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周海波
张泂
沈军刚
刘浩松
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Nanjing Zhongdian Panda Magnetic Electrical Technology Co ltd
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Abstract

本发明涉及一种具有四高特性的锰锌软磁铁氧体材料的制备方法，包括以下步骤：配主料，配辅料，主料混合预烧，主辅料混合后二次球磨，喷雾干燥制成颗粒料，按客户要求压制毛坯、气氛控制烧结，即得到合格磁心产品，本发明通过合理调配主成分，同时通过加入超细粉碎的辅料，达到提高结晶均匀性以及有效增大晶粒的作用，使得磁心成分的均匀分布、气孔减少、烧结密度高，从而具有高磁导率、高居里温度、高磁通密度、同时在0.5kHz到1MHz的宽频范围内感量稳定性高的特性。

Description

一种具有四高特性的锰锌软磁铁氧体材料的制备方法
技术领域
本发明涉及软磁铁氧体领域，具体涉及一种具有四高特性的锰锌软磁铁氧体材料的制备方法。
背景技术
锰锌软磁铁氧体属于软磁铁氧体中的一大类，目前被广泛用于滤波器、电感器、变压器、功率转换器等电子领域。由于现在对于锰锌软磁铁氧体材料应用条件的苛刻要求，因此需要锰锌软磁铁氧体材料具有高导磁率、高居里温度、高饱和磁通密度、同时在尽量宽的频率范围内能保持导磁率的稳定性，但实际情况由于配方中各种组份的互相牵制影响的作用，很难在各个方面都达到最满意的参数。
发明内容
为了解决以上问题，克服现有工艺条件的局限，本发明提供了一种具有高导磁率、高居里温度、高饱和磁通密度、高频谱稳定性的锰锌软磁铁氧体材料的制备方法。
为实现上述目的，本发明提供的技术方案是：
一种具有四高特性的锰锌软磁铁氧体材料的制备方法，包括以下步骤：
1)配主料：取Fe2O3、MnO和ZnO配主料，其摩尔比为(51.5-52.5)：(30.5-31.5)：(16.5-17.5)；
2)配辅料：取相当于主料0.005-0.010wt％的ZrO2、0.006-0.012wt％的Nb2O5、0.013-0.018wt％的CaCO3、0.005-0.001wt％的SiO2和0.035-0.05wt％的SnO2；
3)预烧：将步骤1)配好的主料加适量去离子水充分混合搅拌后用钆片机钆制成2-4mm厚度的料片，进行预烧；
4)辅料超细粉碎：将步骤2)配好的辅料除了SiO2外，加入适量的去离子水，进行辅料球磨，球磨一段时间后加入SiO2继续球磨；
5)主料、辅料混合与粉碎球磨：将步骤3)预烧好的主料加入步骤4)超细粉碎的辅料，加入去离子水和分散剂进行球磨，喷雾造粒制成颗粒料；
6)成型：将喷雾造粒颗粒料加入0.015wt％的硬脂酸锌，用混料机充分混合后压制毛坯；
7)烧结：将步骤6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以100-130℃/小时速率升温至800-850℃，保温1-1.5小时；在10.5％氧含量的氮气氛围中，以60-90℃/小时速率升温至1300-1350℃，烧结后降温得到四高特性的锰锌铁氧体磁心。
步骤3)进行预烧的温度为870-920℃，预烧时间为1-2小时。
步骤4)进行辅料球磨60分钟时加入SiO2继续球磨30分钟，检测粉末粒度为0.4-0.6μm。
步骤5)加入去离子水和分散剂进行球磨1.5-2小时，喷雾造粒制成40-180目的颗粒料。
步骤6)加入0.015wt％的硬脂酸锌，用混料机充分混合10分钟，然后压制毛坯。
步骤7)烧结时间为3-3.5小时；烧结后在0.001-0.003％氧含量的氮气氛围中降温。
与现有技术相比，本发明的有益效果是：
1、本发明通过对添加杂质进行超细粉碎后加入主料，保证了铁氧体化反应的均匀、充分，并有效增大了晶粒，使得磁心成分的均匀分布、气孔减少、烧结密度高，使用该材料生产的磁心具有较高的磁导率。
2、本发明的锰锌软磁铁氧体材料具有较高的居里温度，解决了原来的高导磁材最高工作温度较低的问题，使得用该材料生产的磁心具有较高的理论工作温度。
3、本发明的锰锌软磁铁氧体材料具有较高的饱和磁通密度，有效的提高了磁心的工作效率。
4、本发明的锰锌软磁铁氧体材料在保证以上三个主要磁性参数的基础上，还具有良好的频谱稳定性，使得磁心在0.5kHz到1MHz的相当宽频的工作范围内中仍能保持良好的工作特性。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
一种四高特性锰锌软磁铁氧体材料的制备方法，包括以下步骤：
(1)配主料：取Fe2O3、MnO和ZnO配主料，其摩尔比为(51.5-52.5)：(30.5-31.5)：(16.5-17.5)；
(2)配辅料：相当于主料0.005-0.010wt％的ZrO2、0.006-0.012wt％的Nb2O5、0.013-0.018wt％的CaCO3、0.005-0.001wt％的SiO2、0.035-0.05wt％的SnO2；
(3)预烧：将步骤(1)配好的主料加适量去离子水水充分混合搅拌后用钆片机钆制成2-4mm厚度的料片，进行预烧，预烧温度为870-920℃，预烧时间为1-2小时；
(4)辅料超细粉碎：将步骤(2)配好的辅料除了SiO2外，加入适量的去离子水，进行辅料球磨，球磨时间60分钟时加入SiO2继续球磨30分钟，检测粉末粒度为0.4-0.6μm；
(5)主料、辅料混合与粉碎球磨：将步骤(3)预烧好的主料加入步骤(4)超细粉碎的辅料，加入去离子水和分散剂进行球磨1.5-2小时，喷雾造粒制成40-180目的颗粒料；
(6)成型：将喷雾造粒颗粒料加入0.015wt％的硬脂酸锌，用混料机充分混合10分钟，然后压制毛坯；
(7)烧结：将步骤(6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以100-130℃/小时速率升温至800-850℃，保温1-1.5小时；在10.5％氧含量的氮气氛围中，以60-90℃/小时速率升温至1300-1350℃，烧结时间为3-3.5小时；烧结后在0.001-0.003％氧含量的氮气氛围中降温即可得到四高特性的锰锌铁氧体磁心。
通过以上实验例制得的软磁铁氧体磁心的性能数据：
表1软磁铁氧体磁心的性能数据
Figure GDA0003112809760000031
以上所述，仅是本发明的较佳实施例，并非对本发明作任何形式上的限制，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，依据本发明的技术实质，对以上实施例所作的任何简单的修改、等同替换与改进等，均仍属于本发明技术方案的保护范围之内。

Claims (6)

1.一种具有四高特性的锰锌软磁铁氧体材料的制备方法，其特征在于：包括以下步骤：
1)配主料：取Fe2O3、MnO和ZnO配主料，其摩尔比为(51.5-52.5)：(30.5-31.5)：(16.5-17.5)；
2)配辅料：取相当于主料0.005-0.010wt％的ZrO2、0.006-0.012wt％的Nb2O5、0.013-0.018wt％的CaCO3、0.005-0.001wt％的SiO2和0.035-0.05wt％的SnO2；
3)预烧：将步骤1)配好的主料加适量去离子水充分混合搅拌后用钆片机钆制成2-4mm厚度的料片，进行预烧；
4)辅料超细粉碎：将步骤2)配好的辅料除了SiO2外，加入适量的去离子水，进行辅料球磨，球磨一段时间后加入SiO2继续球磨；
5)主料、辅料混合与粉碎球磨：将步骤3)预烧好的主料加入步骤4)超细粉碎的辅料，加入去离子水和分散剂进行球磨，喷雾造粒制成颗粒料；
6)成型：将喷雾造粒颗粒料加入0.015wt％的硬脂酸锌，用混料机充分混合后压制毛坯；
7)烧结：将步骤6)成型后的毛坯整齐排在氧化锆板上，放入钟罩炉，在0.05-0.10％氧含量的氮气氛围中，先以100-130℃/小时速率升温至800-850℃，保温1-1.5小时；在10.5％氧含量的氮气氛围中，以60-90℃/小时速率升温至1300-1350℃，烧结后降温得到四高特性的锰锌铁氧体磁心。
2.根据权利要求1所述的具有四高特性的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤3)进行预烧的温度为870-920℃，预烧时间为1-2小时。
3.根据权利要求1所述的具有四高特性的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤4)进行辅料球磨60分钟时加入SiO2继续球磨30分钟，检测粉末粒度为0.4-0.6μm。
4.根据权利要求1所述的具有四高特性的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤5)加入去离子水和分散剂进行球磨1.5-2小时，喷雾造粒制成40-180目的颗粒料。
5.根据权利要求1所述的具有四高特性的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤6)加入0.015wt％的硬脂酸锌，用混料机充分混合10分钟，然后压制毛坯。
6.根据权利要求1所述的具有四高特性的锰锌软磁铁氧体材料的制备方法，其特征在于：步骤7)烧结时间为3-3.5小时；烧结后在0.001-0.003％氧含量的氮气氛围中降温。
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