CN112125657B - 一种宽温大功率MnZn铁氧体材料及其制备方法 - Google Patents

一种宽温大功率MnZn铁氧体材料及其制备方法 Download PDF

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CN112125657B
CN112125657B CN202010897738.8A CN202010897738A CN112125657B CN 112125657 B CN112125657 B CN 112125657B CN 202010897738 A CN202010897738 A CN 202010897738A CN 112125657 B CN112125657 B CN 112125657B
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程晗
李平
龙彬
胡迪
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Changshu Haobo Electronic Technology Co ltd
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Abstract

本发明公开了一种宽温大功率MnZn铁氧体材料及其制备方法，包括：主体组分和辅助添加组分，主体组分包括摩尔百分含量为61～65mol%的Fe2O3，12.5～14.5mol%的ZnO，其余为MnO，总量为100%；所述辅助添加组分以占所述主体组分的重量百分含量计，包括：Co2O3、CaCO3、Nb2O5、TiO2、NiO。本发明采取独特的富铁配方设计，制备得到的宽温大功率MnZn铁氧体材料的常温和高温Bs值高，‑40℃~120℃下的初始磁导率变化幅度小，符合极地低温、赤道热带、高山、高原等极端温度环境下的使用要求。

Description

一种宽温大功率MnZn铁氧体材料及其制备方法
技术领域
本发明涉及磁性材料领域，特别是涉及一种宽温大功率MnZn铁氧体材料及其制备方法。
背景技术
科技技术的进步，电动汽车、自动仓库搬运设备、太阳能发电、CATV机器电源、无停电电源装置UPS、通信设备电源等大功率电流使用条件下的变压器，以及高铁、空调、风扇、压缩机、医疗设备等各种电器设备中使用的电抗器扼流圈对磁性材料的抗磁饱和能力要求越来越高。同时，这些电器设备在地球不同温度带广泛使用，要求设备在-40℃~+120℃的环境温度条件下能正常启动工作。现有的磁性材料的磁感应强度低，易于磁饱和，初始磁导率在上述温度范围内变化明显，不能满足宽温变、大工作电流的使用要求。
发明内容
本发明主要解决的技术问题是提供一种宽温大功率MnZn铁氧体材料及其制备方法，能够解决现有铁氧体材料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：提供一种宽温大功率MnZn铁氧体材料，所述宽温大功率MnZn铁氧体材料的起始磁导率为1600±25%；材料饱和磁通密度25℃下为600mT，100℃下为500mT；其包括：主体组分和辅助添加组分，其中，所述主体组分包括以各自标准物计的摩尔百分含量为61～65mol%的Fe2O3，12.5～14.5mol%的ZnO，其余为MnO，总量为100%；所述辅助添加组分以占所述主体组分的重量百分含量计，包括：Co2O30.2～0.3wt%、CaCO3 0.03～0.1wt%、Nb2O5 0.01～0.0.05wt%、TiO2 0.01～0.08wt%、NiO0.01～0.025wt%。
在本发明一个较佳实施例中，所述宽温大功率MnZn铁氧体材料的比温度系数系数αμr：-40～20℃下为-3.0×10-6/℃～5.0×10-6/℃，20～140℃下为-0.3×10-6/℃～1.2×10-6/℃。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种宽温大功率MnZn铁氧体材料的制备方法，包括如下步骤：
（1）主体组分处理：按配方量称取Fe2O3、ZnO和Mn3O4并对块状料进行振磨、预烧和粉碎处理，得到主体组分粉末；
（2）砂磨处理：将称料准备后的Co2O3、CaCO3、Nb2O5 、TiO2 和NiO与步骤（1）得到的主体组分粉末混合，然后进行砂磨处理，使达到设定的粒度；
（3）颗粒干燥成型：向步骤（2）中砂磨处理后的混合粉末中加入胶水制备成胶浆，再通过喷雾干燥制备成颗粒料，将所得颗粒料装入模具中，压制成生坯；
（4）烧结：将步骤（3）中制得的生坯放入烧结窑炉内，调节烧结窑炉内的气体环境和温度环境，烧制成所述宽温大功率MnZn铁氧体材料。
在发明一个较佳实施例中，所述步骤（1）中，所述预烧的温度为860±30℃。
在发明一个较佳实施例中，所述步骤（4）中，所述烧制的工艺条件为：
先以1.5～2.0℃/min的升温速度从室温升至600℃；然后调节氧分压为1.5%，先以1.2～1.8℃/min的升温速度从600℃升至1200℃，再以5.0～6.0℃/min的升温速度从1200℃升温至1300～1340℃，在此温度下调节调节氧分压为4.0～6.0%，并保温4.2～5.5h；
调节氧分压为平衡状态，先以0.5～2.0℃/min的降温速率，从1300～1340℃降温至1000℃；再随炉自然冷却至室温。
本发明的有益效果是：本发明一种宽温大功率MnZn铁氧体材料的制备方法，采取独特的富铁配方设计，通过严格的平衡气氛烧结工艺，制备得到的宽温大功率MnZn铁氧体材料的常温和高温Bs值高，-40℃~120℃下的初始磁导率变化幅度小，解决锰锌铁氧体材料在极地低温、赤道热带、高山、高原等极端温度环境下的交通、通讯、新能源汽车、太阳能等电源保障，使全球蜂窝通讯基站建设、动车、新能源应用等延申到世界的每一个角落，市场前景广阔，具有较好的经济效益和社会效益。
附图说明
图1是本发明一种宽温大功率MnZn铁氧体材料一较佳实施例1的初始磁导率与温度之间的关系图。
具体实施方式
下面结合附图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。
请参阅图1，本发明实施例包括：
实施例1
本发明揭示了一种宽温大功率MnZn铁氧体材料，包括：主体组分和辅助添加组分，其中，所述主体组分包括62.4mol%的Fe2O3，13.6mol%的ZnO和24.0mol%的MnO；其中，Fe2O3纯度≥99.5%，其比表面积大于等于4.05m2/g；MnO以Mn3O4为原料，其中Mn的摩尔百分含量≥71.1%，比表面积为11～15m2/g；ZnO的纯度≥99.7%。
所述辅助添加组分以占所述主体组分的重量百分含量计，包括：Co2O3 0.2wt%、CaCO3 0.08wt%、Nb2O5 0.025wt%、TiO2 0.01wt%和NiO 0.015wt%。
上述一种宽温大功率MnZn铁氧体材料的制备方法，包括如下步骤：
（1）主体组分处理：按配方量称取Fe2O3、ZnO和Mn3O4，并放入振磨机内进行碾磨、粉碎，然后放入强混料装置中充分搅拌，通过860±30℃回转炉完成预烧，使三种氧化物发生初步固相反应；预烧后的物料以300～350kg/h进行振磨粉碎；
（2）砂磨处理：按配方比例称量Co2O3、CaCO3、Nb2O5、TiO2 和NiO与步骤（1）得到的主体组分粉末和去离子水，按固体含量为65%的浓度混合，然后进行砂磨处理，使砂磨后的混合浆料的固体颗粒平均粒径达到0.9±0.2μm；
（3）颗粒干燥成型：向步骤（2）中砂磨处理后的浆料中加入PVA溶液，即胶水，再经充分搅拌混合制备成胶浆，所得胶浆再通过喷雾制备成颗粒料；将颗粒料装入到规格为φ25*15*10的环形模具中，压制成磁环生坯；
（4）烧结：将步骤（3）中制得的生坯放入烧结窑炉内，调节烧结窑炉内的气体环境和温度环境，在1350℃下保温5.2h，烧制成所述宽温大功率MnZn铁氧体材料，即环型磁环；
具体地，先以1.5℃/min的升温速度从室温升至600℃；然后调节氧分压为1.5%，先以1.2℃/min的升温速度从600℃升至1200℃，再以5.0℃/min的升温速度从1200℃升温至1300～1340℃，在此温度下调节调节氧分压为4.0%，并保温4.2h；
调节氧分压为平衡状态，先以0.5℃/min的降温速率，从1300～1340℃降温至1000℃；再随炉自然冷却至室温。
该实施例所得的铁氧体材料特性见表1。
实施例2
与实施例1的区别在于，所述主体组分包括62.5mol%的Fe2O3，13.3mol%的ZnO和24.2mol%的MnO；所述辅助添加组分以占所述主体组分的重量百分含量计，包括：Co2O30.22wt%、CaCO3 0.08wt%、Nb2O5 0.025wt%、TiO2 0.015wt%、NiO 0.015wt%。烧制成所述宽温大功率MnZn铁氧体材料，即环型磁环，其铁氧体材料特性见表1。
表1 本发明环形磁芯的材料性能
Figure 859463DEST_PATH_IMAGE001
表1的材料Bs比常规大功率材料PC40有大幅度的提升，使本发明的材料在实际工作温度区间25~100℃更能承载更大的工作电流而不易饱和。
采用上述实施例1的配方及其制备方法制得的规格为φ25*15*10的环型磁环，温度曲线测试其结果如图1所示。
上述实施例的数据表明：本发明制备的宽温大功率MnZn铁氧体材料，在-40℃～120℃的条件下，其磁导率曲线平坦，以本发明的铁氧体材料制备的设备能够在-40℃～120℃的宽温度环境下正常工作，解决极地低温-赤道热带、高山、高原等极端温度环境下的交通、通讯、新能源汽车、太阳能等电源保障，使蜂窝通讯基站建设、动车、新能源应用等延伸到世界的每一个角落。
本发明一种宽温大功率MnZn铁氧体材料的制备方法，采用新的技术和工艺，通过大量的实验，采取独特的富铁配方设计和严格的平衡气氛烧结工艺，制备得到的宽温大功率MnZn铁氧体材料，均匀性好、一致性高，无异相晶粒，很好的控制了材料的微观结构和化学键，得到宽温大功率MnZn铁氧体材料，能适应为-40℃～120℃环境温度的使用要求，得到国际国内市场的认可，具有较好的经济效益和社会效益。
在本发明的描述中，需要说明的是，术语“上”、“下”、“左”、“右”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，或者是该发明产品使用时惯常摆放的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (2)

1.一种宽温大功率MnZn铁氧体材料，其特征在于，所述宽温大功率MnZn铁氧体材料的起始磁导率为1600±25%；材料饱和磁通密度25℃下为600mT，100℃下为500mT；其包括：主体组分和辅助添加组分，其中，所述主体组分包括以各自标准物计的摩尔百分含量为61～65mol%的Fe2O3，12.5～14.5mol%的ZnO，其余为MnO，总量为100%；所述辅助添加组分以占所述主体组分的重量百分含量计，包括：Co2O3 0.2～0.3wt%、CaCO3 0.03～0.1wt%、Nb2O5 0.01～0.05wt%、TiO2 0.01～0.08wt%、NiO 0.01～0.025wt%；所述宽温大功率MnZn铁氧体材料的比温度系数αμr：-40～20℃下为-3.0×10-6/℃～5.0×10-6/℃，20～140℃下为-0.3×10-6/℃～1.2×10-6/℃；
所述宽温大功率MnZn铁氧体材料的制备方法，包括如下步骤：
（1）主体组分处理：按配方量称取Fe2O3、ZnO和Mn3O4 并对块状料进行振磨、预烧和粉碎处理，得到主体组分粉末；
（2）砂磨处理：将称料准备后的Co2O3、CaCO3、Nb2O5 、TiO2 和NiO与步骤（1）得到的主体组分粉末混合，然后进行砂磨处理，使达到设定的粒度；
（3）颗粒干燥成型：向步骤（2）中砂磨处理后的混合粉末中加入胶水制备成胶浆，再通过喷雾干燥制备成颗粒料，将所得颗粒料装入模具中，压制成生坯；
（4）烧结：将步骤（3）中制得的生坯放入烧结窑炉内，调节烧结窑炉内的气体环境和温度环境，烧制成所述宽温大功率MnZn铁氧体材料；所述烧制的工艺条件为：
先以1.5～2.0℃/min的升温速度从室温升至600℃；然后调节氧分压为1.5%，先以1.2～1.8℃/min的升温速度从600℃升至1200℃，再以5.0～6.0℃/min的升温速度从1200℃升温至1300～1340℃，在此温度下调节氧分压为4.0～6.0%，并保温4.2～5.5h；
调节氧分压为平衡状态，先以0.5～2.0℃/min的降温速率，从1300～1340℃降温至1000℃；再随炉自然冷却至室温。
2.根据权利要求1所述的一种宽温大功率MnZn铁氧体材料，其特征在于，所述步骤（1）中，所述预烧的温度为860±30℃。
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