CN107098693B - 一种高频抗干扰锰锌铁氧体及其制备方法 - Google Patents

一种高频抗干扰锰锌铁氧体及其制备方法 Download PDF

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CN107098693B
CN107098693B CN201710293210.8A CN201710293210A CN107098693B CN 107098693 B CN107098693 B CN 107098693B CN 201710293210 A CN201710293210 A CN 201710293210A CN 107098693 B CN107098693 B CN 107098693B
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柯宇翔
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Suzhou Guanda Magnetic Co ltd
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Abstract

本发明公开了一种高频抗干扰锰锌铁氧体及其制备方法，包括主成分和辅助成分；主成分包括：Fe2O3、MnO、ZnO；辅助成分包括：Bi2O3、MoO3、Co2O3、K2CO3、TiO2、P2O5、Nb2O5。所述制备方法包括称料、掺杂、压制坯料、排坯和烧结处理步骤。本发明经科学的材料配方设计、烧结工艺及窑炉气氛优化等措施，使得制备的锰锌铁氧体具有具备较高的磁导率特性，磁芯居里温度高，且具有良好的温升特性，温度曲线平坦、高温功耗低，工作环境适应性强等优点，达到EMC的安规要求。

Description

一种高频抗干扰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材料领域，特别是涉及一种10MHz至40MHz的高频抗干扰锰锌铁氧体及其制备方法。
背景技术
随着跨领域工业电子设备产业的高速发展，元件设备越来越趋于智能化、小型化、低能耗和抗干扰。而元件设备性能优化的核心在于嵌套的软磁铁氧体磁芯的优化。软磁铁氧体由于其成本方面的优势，越来越多的被用来替换传统磁芯，其良好的配合特性也能帮助实现元器件更好的特性，特别是在EMC抗干扰应用中。
软磁铁氧体能够应用于与抗干扰滤波器配合使用的设备设施，如无线通讯，智能电表终端、工业集成设备、海底电缆、光缆水下设备等特殊环境。磁性材料在滤波器、开关电源、及滤波器应用电子产品中均占有部分体积并消耗部分能源，因此提高磁芯初始磁导率及频率特性，使大功率产品向小型号、高效化发展，对我国电子产业结构调整，节能减排提供有效帮助。但现有的铁氧体在滤波器应用领域中，还存在诸多不足之处，如常温条件下的磁导率特性、温度特性差，饱和磁通密度低，磁芯居里温度达不到要求等。
发明内容
本发明主要解决的技术问题是提供一种10MHz至40MHz高频抗干扰锰锌铁氧体及其制备方法，能够解决现有铁氧体材料在滤波器应用领域中存在的上述不足之处。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种高频抗干扰锰锌铁氧体，包括：主成分和辅助成分；所述主成分包括如下摩尔百分含量的组分：Fe2O3 50.5～55.5mol%、MnO 22.5～33.5mol%、ZnO 16～27mol%；相对于所述主成分的总重量，所述辅助成分的组分及其含量为：Bi2O3 300～2000ppm、MoO3 100～3000ppm、Co2O3 50～2000ppm、K2CO3 100～800ppm、TiO2 50～500ppm、P2O5 30～300ppm、Nb2O5：30～300ppm。
在本发明一个较佳实施例中，所述Fe2O3和ZnO的纯度为95%以上。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种10MHz至40MHz高频抗干扰锰锌铁氧体的制备方法，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将步骤（1）中称取的辅助成分先后分3次以上加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先进行混合预烧，再进行研磨处理，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向步骤（2）中得到的混合料中先后加入去离子水和分散剂，搅拌成均一的浆料，再将所述浆料压制成磁芯坯料；
（4）排坯：将步骤（3）中得到的坯料在烧结架上按一定的间距逐层排列，并在最底层的坯料下方加装带槽口的垫片；
（5）烧结处理：将步骤（4）中经排坯后的坯料整体置入烧结窑炉内，在平衡气氛下烧结成型，得到所述高频抗干扰锰锌铁氧体。
在本发明一个较佳实施例中，所述步骤（2）中，所述混合预烧的条件为：温度400～500℃，时间5～15min；所述混合研磨在行星球磨机中进行，每次研磨时间为5～15min。
在本发明一个较佳实施例中，所述步骤（4）中，所述坯料的排列层数为5～8层，层间间距为1～1.5cm，前后左右间距0.5～1cm。
在本发明一个较佳实施例中，所述步骤（5）中，所述烧结的工艺条件为：在5～8%氮气含量的平衡气压下，先以30～50℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1350～1400℃，恒温保持4～5h，然后再以30～50℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温。
本发明的有益效果是：本发明经科学的材料配方设计、烧结工艺及窑炉气氛优化等措施，使得制备的锰锌铁氧体具有具备较高的磁导率特性，磁芯居里温度高，且具有良好的温升特性，温度曲线平坦、高温功耗低，工作环境适应性强等优点，达到EMC的安规要求，可广泛应用于宽带滤波器、脉冲滤波器、电感器、滤波器、共模扼流圈及传输系统中的接口滤波器、隔离滤波器等领域，市场前景广阔。
具体实施方式
下面对本发明的较佳实施例进行详细阐述，以使本发明的优点和特征能更易于被本领域技术人员理解，从而对本发明的保护范围做出更为清楚明确的界定。
本发明实施例包括：
实施例1
一种10MHz至40MHz的高频抗干扰锰锌铁氧体，包括：主成分和辅助成分；所述主成分包括如下摩尔百分含量的组分：Fe2O3 50.5mol%、MnO 22.5～33.5mol%、ZnO 16mol%；其中，Fe2O3和ZnO均为高纯度，其纯度为95%以上，MnO来自大比表面积的Mn3O4。
相对于所述主成分的总重量，所述辅助成分的组分及其含量为：Bi2O3 300ppm、MoO3 3000ppm、Co2O3 50ppm、K2CO3 100ppm、TiO2 500ppm、P2O5 30ppm、Nb2O5：300ppm，其中，Nb2O5的添加有助于提高铁氧体的Q值及抗干扰性能。
上述10MHz至40MHz高频抗干扰锰锌铁氧体的制备方法，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将上述称取的辅助成分先后均分3次加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先在400℃下混合预烧15min，再在行星球磨机中研磨处理5～15min，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向上述中得到的混合料中先后加入去离子水制备成质量浓度为60%的混悬液，然后加入占混合料（未加去离子水）3%质量百分数的分散剂搅拌混合成均一的浆料，再将所述浆料压制成磁芯坯料；
（4）排坯：烧结之间，将步骤（3）中得到的坯料在烧结架上按层间间距为1cm，前后左右间距0.5cm的条件逐层排列5～8层，并在最底层的坯料下方加装带槽口的垫片；其中，层间间距及底部带槽口的垫片均利于热气流通，保证了坯料性能的均一稳定；
（5）烧结处理：将步骤（4）中经排坯后的坯料整体置入烧结窑炉内，在氮氧平衡气氛下烧结成型，具体烧结工艺条件为：在5%氮气含量的平衡气压下，先以30℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1350℃，恒温保持5h，然后再以30℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温，得到所述高频抗干扰锰锌铁氧体。
实施例2
一种10MHz至40MHz高频抗干扰锰锌铁氧体，包括：主成分和辅助成分；所述主成分包括如下摩尔百分含量的组分：Fe2O3 50.5mol%、MnO 22.5mol%、ZnO 27mol%；其中，Fe2O3和ZnO均为高纯度，其纯度为95%以上，MnO来自大比表面积的Mn3O4。
相对于所述主成分的总重量，所述辅助成分的组分及其含量为：Bi2O3 300～2000ppm、MoO3 3000ppm、Co2O3 2000ppm、K2CO3 100ppm、TiO2 50ppm、P2O5 300ppm、Nb2O5：200ppm。
上述10MHz至40MHz高频抗干扰锰锌铁氧体的制备方法，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将上述称取的辅助成分先后均分3次加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先在500℃下混合预烧5min，再在行星球磨机中研磨处理5～15min，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向上述中得到的混合料中先后加入去离子水制备成质量浓度为60%的混悬液，然后加入占混合料（未加去离子水）3%质量百分数的分散剂搅拌混合成均一的浆料，再将所述浆料压制成磁芯坯料；
（4）排坯：烧结之间，将步骤（3）中得到的坯料在烧结架上按层间间距为1.5cm，前后左右间距1cm的条件逐层排列5～8层，并在最底层的坯料下方加装带槽口的垫片；其中，层间间距及底部带槽口的垫片均利于热气流通，保证了坯料性能的均一稳定；
（5）烧结处理：将步骤（4）中经排坯后的坯料整体置入烧结窑炉内，在氮氧平衡气氛下烧结成型，具体烧结工艺条件为：在8%氮气含量的平衡气压下，先以50℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1400℃，恒温保持4h，然后再以50℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温，得到所述高频抗干扰锰锌铁氧体。
上述方法得到的锰锌铁氧体，为与抗干扰滤波器配合使用的高性能的锰锌软磁铁氧体产品，其主要特点是温度曲线平坦，温度变化小、抗折程度高，功耗低，工作环境适应性强。经测试，具体性能特点如下：
1）性能层面，1.0KHz，0.3V，25±3℃条件下，初始磁导率μi=12000±25%；
2）具有良好的温度特性，比温度系数低，温度曲线平坦，适合工作温度为0～120℃；
3）高饱和磁通密度，1194A/m，25±3℃条件下，Bs＞390mT；
4）磁芯居里温度高，Tc≥120℃，最高达125℃；
5）良好的阻抗特性，在10MHz至40MHz保持阻抗值随测试频率提高而上升，可以达到EMC的安装要求。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (2)

1.一种高频抗干扰锰锌铁氧体的制备方法，所述高频抗干扰锰锌铁氧体包括：主成分和辅助成分；所述主成分包括如下摩尔百分含量的组分：Fe2O3 50.5～55.5mol%、MnO 22.5～33.5mol%、ZnO 16～27mol%；相对于所述主成分的总重量，所述辅助成分的组分及其含量为：Bi2O3 300～2000ppm、MoO3 100～3000ppm、Co2O3 50～2000ppm、K2CO3 100～800ppm、TiO250～500ppm、P2O5 30～300ppm、Nb2O5 30～300ppm；其特征在于，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将步骤（1）中称取的辅助成分先后分3次以上加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先进行混合预烧，再进行研磨处理，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；所述混合预烧的条件为：温度400～500℃，时间5～15min；所述混合研磨在行星球磨机中进行，每次研磨时间为5～15min；
（3）压制坯料：向步骤（2）中得到的混合料中先后加入去离子水和分散剂，搅拌成均一的浆料，再将所述浆料压制成磁芯坯料；
（4）排坯：将步骤（3）中得到的坯料在烧结架上按一定的间距逐层排列，并在最底层的坯料下方加装带槽口的垫片；所述坯料的排列层数为5～8层，层间间距为1～1.5cm，前后左右间距0.5～1cm；
（5）烧结处理：将步骤（4）中经排坯后的坯料整体置入烧结窑炉内，在平衡气氛下烧结成型，得到所述高频抗干扰锰锌铁氧体；所述烧结的工艺条件为：在5～8%氮气含量的平衡气压下，先以30～50℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1350～1400℃，恒温保持4～5h，然后再以30～50℃/min的降温速率降至1100℃，恒温保持1～2h，最后随炉自然冷却至室温。
2.根据权利要求1所述的高频抗干扰锰锌铁氧体的制备方法，其特征在于，所述Fe2O3和ZnO的纯度为95%以上。
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