CN114085077A - 一种微调亚铁离子的高频低损耗锰锌铁氧体及其制备方法 - Google Patents

一种微调亚铁离子的高频低损耗锰锌铁氧体及其制备方法 Download PDF

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CN114085077A
CN114085077A CN202111607712.6A CN202111607712A CN114085077A CN 114085077 A CN114085077 A CN 114085077A CN 202111607712 A CN202111607712 A CN 202111607712A CN 114085077 A CN114085077 A CN 114085077A
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徐涛
聂建文
张强原
***
邢冰冰
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Abstract

本发明公开了一种微调亚铁离子的高频低损耗锰锌铁氧体及制备方法，该材料的主成分为四元系，采用富铁配方，分别为Fe2O3:Y‑X mol%(55≤Y≤60)，ZnO:＜5 mol%，MgO:X mol%(X≤0.4)，其余为MnO。制备该材料的工艺步骤是：配料；砂磨，并辅以超声分散；预烧，预烧后进行快速降温；砂磨，并辅以超声分散；造粒成型；烧结，烧结后进行快速降温。该铁氧体主配方中采用微量Mg离子取代Fe离子，并配合相应的制备工艺避免富镁杂相析出，通过电荷平衡利用二价Mg离子促使Fe离子偏向三价，达到微调亚铁离子的目的，使软磁铁氧体材料实现高频下低损耗特性，尤其对于高频高温下的损耗降低幅度较大。

Description

一种微调亚铁离子的高频低损耗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及其制备方法，具体涉及一种微调亚铁离子的高频低损耗锰锌铁氧体材料及制备方法。
背景技术
随着电子产品越来越往小型化发展，同时节能减排的需求越来越大，这类电子产品上的软磁铁氧体材料必然要往高频化方向发展。众所周知，铁氧体材料的损耗主要由磁滞损耗、涡流损耗和剩余损耗三者构成。在低频下，磁滞损耗占主要部分，越往高频发展，涡流损耗及剩余损耗的比重也不断提高。而烧结后过量的亚铁离子会明显降低材料的电阻率，增加高频下的涡流损耗及剩余损耗。目前科研界及企业界主要通过二次掺杂及烧结过程中的氧分压控制来调节材料中的亚铁离子，从而降低高频材料的损耗。
在开关电源等器件中，铁氧体需要在高温高频、高直流叠加的条件下工作，因此高温高饱和磁通密度是高频铁氧体材料的一个重要发展方向。采用富铁配方是提高铁氧体饱和磁通密度的重要方法之一。在富铁配方下，烧结后的亚铁离子不可避免会增加，因此高频下的总损耗增加，尤其是高温下的损耗。然而，在富铁配方下，通过二次掺杂及烧结过程控制来调节亚铁离子难度较大。首先，在预烧过程中，铁氧体已基本成相，目前二次掺杂的元素多为高价及变价元素，不易通过材料电荷平衡调节亚铁离子。另外，烧结过程控制受环境、设备等影响较大，容易造成波动。因此急需另外的方法来控制材料内部的亚铁离子在一个合适的水平，降低损耗。
公开号为CN113436823A的专利文献公开了一种包含Mg的铁氧体烧结磁铁，含量在0.01质量%至0.09质量%，目的是提高Br，没有提及调控亚铁离子，并且其体系不属于锰锌铁氧体。《少量缺铁对Mg-Mn-Zn铁氧体性能的影响》期刊文献(稀有金属材料与工程, 2008,37(A01):4.)公开了一种少量缺铁的Mg-Mn-Zn铁氧体，其制备方法属于溶胶凝胶法，并且Mg并非取代Fe，即Mg掺杂量不等于缺铁量。
发明内容
本发明正是为了克服现有方法的不足而提供一种微调亚铁离子的高频低损耗锰锌铁氧体及其制备方法。
为了实现以上目的，本发明所采用的技术方案是：
一种微调亚铁离子的高频低损耗锰锌铁氧体材料，材料主成分为四元系，同时采用富铁配方，分别为Fe2O3:Y-X mol%(55≤Y≤60)，ZnO:＜5 mol%，MgO:X mol%(X≤0.4)，其余为MnO；副成分为锰锌铁氧体领域的常规掺杂物。与常规MnZn铁氧体不同的是，该铁氧体主配方中采用微量Mg离子取代Fe离子，并配合相应的制备工艺避免富镁杂相析出，通过电荷平衡利用二价Mg离子促使Fe离子偏向三价，达到微调亚铁离子的目的。
微调亚铁离子的高频低损耗锰锌铁氧体材料的制备方法，包括以下步骤：
（1）配料：按照四元系配方，称取Fe2O3、ZnO、MgO和MnO，进行砂磨混合10~20min,同时为了让Mg混合均匀，使其预烧过程中均匀进入晶格，在砂磨的同时辅以超声分散3~15min；
（2）预烧：将上一步的粉料进行预烧处理，预烧温度在800℃~1000℃，由于Mg离子半径较大，为了防止冷却过程中Mg从晶格中析出，保温1h~3h,结束后马上将粉料转移至25℃环境中，冷却至室温；
（3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合至目标粒径,D50在0.8μm~1.8μm，在砂磨的同时辅以超声分散3~15min；
（4）造粒成型；
（5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1100℃~1300℃，保温3~5h,为了防止降温过程中Mg从晶格中析出，降温阶段采用较快降温速率，1100℃以下降温阶段，采用的降温速率为2℃/min-6℃/min之间。
优选的，一种微调亚铁离子的高频低损耗锰锌铁氧体材料的材料配方为Fe2O3:Y-X mol%(55≤Y≤57)，ZnO:＜5 mol%，MgO:X mol%(0.1≤X≤0.3)，其余为MnO。
优选的，步骤2中，预烧温度在850℃~950℃，保温1h~3h。
优选的，步骤5中，1100℃以下降温阶段的降温速率为3℃/min-5℃/min之间。
优选的，一种微调亚铁离子的高频低损耗锰锌铁氧体材料的材料副成分可以是Co2O3、TiO2、CaCO3、ZrO2、V2O5、Ta2O5、Nb2O5、CuO、SnO2中的一种或多种，含量范围是Co2O3：0-0.8wt%、TiO2：0-1wt%、CaCO3：0.01-0.2wt%、ZrO2：0-0.02wt%、V2O5：0.01-0.05wt%、Ta2O5：0.01-0.05wt%、Nb2O5：0.01-0.03wt%、CuO：0-0.02wt%、SnO2：0-0.02wt%，以上副成分是相对于主成分总量的重量百分比计算。
本发明的有益效果是: 通过四元系配方基础上，微量Mg取代Fe，同时配合上述预烧、砂磨及烧结工艺，超声让砂磨混合更均匀，促进热处理过程中形成均相，预烧和烧结的快速降温能够让高温下进入晶格中的镁固定在晶格中，减少富镁杂相的析出，有助于降低高频高Bm下的损耗，尤其是高温下的损耗，制备的高频铁氧体磁芯在3MHz、50mT下功耗（25℃）小于700 kW/m3，3MHz、50mT下功耗（100℃）小于700 kW/m3，使得软磁铁氧体材料在高频高Bm高温条件下也能保持较低功耗。
具体实施方式
实施例1：一种微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:56mol%，ZnO:4mol%，MgO:0.1mol%，MnO:39.9mol%；副成分为Co2O3、TiO2、CaCO3、ZrO2、V2O5、Ta2O5、Nb2O5、CuO、SnO2中的一种或多种，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称取的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,在砂磨开始阶段辅助超声分散5min；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，在砂磨开始阶段辅助超声分散10min；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为3.5℃/min。
实施例2：一种微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:58mol%，ZnO:4mol%，MgO:0.2mol%，MnO:37.8mol%，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称量对应比例的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,在砂磨开始阶段辅助超声分散5min；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，在砂磨开始阶段辅助超声分散10min；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为3.5℃/min。
实施例3：一种微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:60mol%，ZnO:1mol%，MgO:0.3mol%，MnO:38.7mol%，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称量对应比例的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,在砂磨开始阶段辅助超声分散5min；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，在砂磨开始阶段辅助超声分散10min；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为4℃/min。
对比例1：一种没有微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:56.1mol%，ZnO:4mol%， MnO:39.9mol%，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称量对应比例的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,在砂磨开始阶段辅助超声分散5min；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，在砂磨开始阶段辅助超声分散10min；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为3.5℃/min。
对比例2：一种没有微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:60.3mol%，ZnO:1mol%， MnO:38.7mol%；副成分为铁氧体领域的常规掺杂物，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称量对应比例的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,在砂磨开始阶段辅助超声分散5min；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，在砂磨开始阶段辅助超声分散10min；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为4℃/min。
对比例3：一种微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:56mol%，ZnO:4mol%，MgO:0.1mol%，MnO:39.9mol%；副成分为铁氧体领域的常规掺杂物，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称量对应比例的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,不辅助其他分散方式；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，不辅助其他分散方式；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为3.5℃/min。
对比例4：一种微调亚铁离子的高频低损耗锰锌铁氧体材料，由主成分和副成分组成，主成分分别为Fe2O3:56mol%，ZnO:4mol%，MgO:0.1mol%，MnO:39.9mol%；副成分为铁氧体领域的常规掺杂物，所有实施例及对比例均为相同副成分。
制备方法包括如下步骤：
1) 配料：按照四元系配方，称量对应比例的Fe2O3、ZnO、MgO和MnO，接着进行砂磨15min,在砂磨开始阶段辅助超声分散5min；
2）预烧：将上一步的粉料进行预烧处理，预烧处理温度在900℃，随炉冷却；
3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，控制粒径在1.0μm，在砂磨开始阶段辅助超声分散10min；
4）造粒成型；
5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1200℃, 1100℃以下降温阶段降温速率为1.5℃/min。
以上实施例和对比例制备的标准样环性能测试结果如下：
Figure 665447DEST_PATH_IMAGE002
对比例1相较实施例1没有微调亚铁离子，功耗偏高，尤其100℃。
对比例2相较实施例3没有微调亚铁离子，功耗偏高，尤其100℃。
对比例3相较实施例1微调了亚铁离子，但是混合过程没有辅助超声分散，功耗有所增加。
对比例4相较实施例1微调了亚铁离子，但是预烧和降温阶段没有快速降温，功耗有所增加。

Claims (8)

1.一种微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于：材料主成分为四元系，同时采用富铁配方，分别为Fe2O3:Y-X mol%(55≤Y≤60)，ZnO:＜5 mol%，MgO:X mol%(X≤0.4)，其余为MnO，同时配合避免镁元素析出制备方法，材料制备方法包括以下步骤：
（1）配料：按照四元系配方，称量Fe2O3、ZnO、MgO和MnO后，进行砂磨混合,同时辅以超声分散处理；
（2）预烧：将上一步的粉料进行预烧处理，预烧温度在800℃~1000℃，保温结束后马上转移至25℃环境中，迅速冷却至室温；
（3）砂磨：将副成分加入上一步处理后的预烧料中，接着进行砂磨混合，同时辅以超声分散处理；
（4）造粒成型；
（5）烧结：将成型毛坯置于平衡氧分压中烧结，烧结温度1100℃~1300℃，保温3~5h,1100℃以下降温阶段降温速率在2℃/min-6℃/min之间。
2.根据权利要求1所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于，可采用微量Mg离子取代Fe离子，达到微调亚铁离子的目的，55≤Y≤57，0.1≤X≤0.3。
3.根据权利要求1所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于,所述步骤（1）中，砂磨时间为10~20min。
4.根据权利要求1所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于,所述步骤（1）和步骤（3）中，进行超声分散的时间均为3min-15min。
5.根据权利要求1所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于,所述步骤（2）中，预烧温度在850℃~950℃，保温1h~3h。
6.根据权利要求1所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于,所述步骤（3）中，砂磨后的材料粒径为0.8μm~1.8μm。
7.根据权利要求1所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于,所述步骤（5）中，1100℃以下降温阶段降温速率在3℃/min-5℃/min之间。
8.根据权利要求1-7任一所述的微调亚铁离子的高频低损耗锰锌铁氧体材料，其特征在于,所述副成分可以是Co2O3、TiO2、CaCO3、ZrO2、V2O5、Ta2O5、Nb2O5、CuO、SnO2中的一种或多种,含量范围是：Co2O3：0-0.8wt%、TiO2：0-1wt%、CaCO3：0.01-0.2wt%、ZrO2：0-0.02wt%、V2O5：0.01-0.05wt%、Ta2O5：0.01-0.05wt%、Nb2O5：0.01-0.03wt%、CuO：0-0.02wt%、SnO2：0-0.02wt%。
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