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 PDFInfo
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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
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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