CN108249908A - 低功耗高磁导率和磁滞伸缩锰锌铁氧体及其制备方法 - Google Patents

低功耗高磁导率和磁滞伸缩锰锌铁氧体及其制备方法 Download PDF

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CN108249908A
CN108249908A CN201810050313.6A CN201810050313A CN108249908A CN 108249908 A CN108249908 A CN 108249908A CN 201810050313 A CN201810050313 A CN 201810050313A CN 108249908 A CN108249908 A CN 108249908A
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李申华
黄有东
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CHANGSHU SANJIA MAGNETIC Co Ltd
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Abstract

本发明公开了一种低功耗高磁导率和磁滞伸缩锰锌铁氧体及其制备方法，包括主体组分和掺杂组分；所述主体组分包括如下质量百分含量的组分：Fe2O3 71.1～71.3%、ZnO 6.5～6.7%，余量为MnO，总量为100%；所述掺杂组分包括如下组分：CaO、Nb2O5、ZrO2、V2O5、Co2O3和NiO；所述掺杂组分占所述主体组分总质量的1～5%。本发明通过使用高纯和高比表面积的原材料，并结合合适的预烧温度和保温时间，提高了产品的密度和细化晶粒，保证高的饱和磁通密度Bs和低的功耗；通过烧结条件的控制，达到细化晶粒，提高产品的电阻率，使产品在使用时不发热，提高效率。

Description

低功耗高磁导率和磁滞伸缩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，特别是涉及一种低功耗高磁导率和磁滞伸缩锰锌铁氧体及其制备方法。
背景技术
当前，电子产品向小型化和高效化方向发展已成趋势，环保要求更加突出，电源变压器小型、高效、节能在家用和工厂电器电子产品中一直占主导地位，今后发展高效化、小型化仍是主流。环保要求对磁性材料产品的使用和要求更加严格：主要要求噪声小，能耗低，效率高。
磁芯是决定变压器性能的重要因素之一。为满足这种电源变压器的需求，具有低功率损耗、高饱和磁通密度、高的磁导率及具有优良的磁滞伸缩系数，使用过程噪声低等性能的磁芯产品应运而生，目前的各种磁芯产品在性能上仍不能满足上述要求。
发明内容
本发明主要解决的技术问题是提供一种低功耗高磁导率和磁滞伸缩锰锌铁氧体及其制备方法，能够满足现有变压器的性能要求。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种低功耗高磁导率和磁滞伸缩锰锌铁氧体，包括：主体组分和掺杂组分；所述主体组分包括如下质量百分含量的组分：Fe2O3 71.1～71.3%、ZnO 6.5～6.7%，余量为MnO，总量为100%；所述掺杂组分包括如下组分：CaO、Nb2O5、ZrO2、V2O5、Co2O3和NiO；所述掺杂组分占所述主体组分总质量的1～5%。
在本发明一个较佳实施例中，所述掺杂组分中各元素的质量比为：CaO：Nb2O5：ZrO2：V2O5：Co2O3：NiO为3～5：1～2：1～3：2～3：3～4：1～2。
在本发明一个较佳实施例中，所述锰锌铁氧体在25℃下的初始磁导率大于等于3000；100KHZ，200mT，25℃下的功率损耗低于550KW/m3；100KHZ，200mT，100℃下的功率损耗低于350KW/m3；居里温度大于等于230℃；1194A/m，25℃下的饱和磁通密度高于510mT，1194A/m，100℃下的饱和磁通密度高于420mT。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，包括如下步骤：
（1）称量：按配方量称取主体组分和掺杂组分备用；
（2）主体组分预处理：将称好的主体组分放入强混机和振磨机中强混研磨，然后放入回转窑预烧处理，得到预烧粉末；
（3）物料混合：将步骤（2）中得到的预烧粉末与步骤（1）中称量好的掺杂组分混合，然后经过砂磨机共混研磨得到粒径为0.8～1.0μm的混合物料，烘干，备用；
（4）造粒：向步骤（3）中共混研磨后的主体组分和掺杂组分中加入一定量的粘合浆料，混合均匀后，烘干造粒，粒料用模具压制成所需的坯样；
（5）烧结成型：将步骤（4）中所得的坯样放入钟罩炉内，根据平衡氧分压的气氛曲线烧结成型，得到所述低功耗高磁导率和磁滞伸缩锰锌铁氧体。
在本发明一个较佳实施例中，所述步骤（2）中，所述预烧处理的工艺条件为：950～1050℃，2～3h。
在本发明一个较佳实施例中，所述步骤（4）中，所述粘合浆料为质量浓度为6～8%的PVA浆料，其加入质量占所述主体组分和掺杂组分总质量的8～10%。
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：先在大气气氛中，以1～1.5℃/min的升温速率从室温升至650℃，然后在平衡氧分压的条件下，先以1～1.5℃/min的升温速率从650℃升至1100℃，再以5～8℃/min的升温速率从1100℃升至1340℃，保温3.5～6.5h；最后先以1～1.5℃/min的降温速率从1340℃降温至1100℃，再以5～8℃/min的降温速率从1100℃降至室温。
本发明的有益效果是：本发明一种低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，通过使用高纯和高比表面积的原材料，并结合合适的预烧温度和保温时间，提高了产品的密度和细化晶粒，保证高的饱和磁通密度Bs和低的功耗；通过烧结条件的控制，达到细化晶粒，提高产品的电阻率，使产品在使用时不发热。
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
本发明揭示了一种低功耗高磁导率和磁滞伸缩锰锌铁氧体，包括：主体组分和掺杂组分；所述掺杂组分占所述主体组分总质量的1%；其中，所述主体组分包括如下质量百分含量的组分：Fe2O3 71.1%、ZnO 6.5%，MnO 22.4，总量为100%；所述掺杂组分包括如下各元素组分：CaO、Nb2O5、ZrO2、V2O5、Co2O3和NiO；且质量比计算，CaO：Nb2O5：ZrO2：V2O5：Co2O3：NiO为3：1：1：2：3：1。
上述低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，包括如下步骤：
（1）称量：按配方量称取主体组分和掺杂组分备用；其中，称取主体组分，包括Fe2O3、ZnO 和MnO共2kg；称取掺杂组分中各组分共0.02kg；
（2）主体组分预处理：将称好的主体组分放入强混机和振磨机中强混研磨1h以上，然后放入950℃的预烧炉中进行预烧处理2～3h，得到平均粒径为6～10μm的预烧粉末；
（3）物料混合：将步骤（2）中得到的预烧粉末与步骤（1）中称量好的掺杂组分混合，然后经过砂磨机共混研磨得到粒径为0.8～1.0μm的混合物料，烘干，备用；
（4）造粒并成坯：向步骤（3）中共混研磨后的主体组分和掺杂组分中加入占所述主体组分和掺杂组分总质量的8%的质量浓度为6%的PVA浆料作为粘合浆料，混合均匀后造粒，用模具压制成所需的坯样；
（5）烧结成型：将步骤（4）中所得的坯样放入钟罩炉内，根据平衡氧分压的气氛曲线烧结成型，得到所述低功耗高磁导率和磁滞伸缩锰锌铁氧体；具体地，所述烧结的工艺条件为：先在大气气氛中，以1℃/min的升温速率从室温升至650℃，然后在平衡氧分压的条件下，先以1℃/min的升温速率从650℃升至1100℃，再以5℃/min的升温速率从1100℃升至1340℃，保温6.5h；最后先以1℃/min的降温速率从1340℃降温至1100℃，再以5℃/min的降温速率从1100℃降至室温。
实施例2
本发明揭示了一种低功耗高磁导率和磁滞伸缩锰锌铁氧体，包括：主体组分和掺杂组分；所述掺杂组分占所述主体组分总质量的5%；其中，所述主体组分包括如下质量百分含量的组分：Fe2O3 71.3%、ZnO 6.7%，MnO 22%；所述掺杂组分包括如下各元素组分：CaO、Nb2O5、ZrO2、V2O5、Co2O3和NiO；且 质量比计算，CaO：Nb2O5：ZrO2：V2O5：Co2O3：NiO为5：2：3：3：4：2。
上述低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，包括如下步骤：
（1）称量：按配方量称取主体组分和掺杂组分备用；其中，称取主体组分，包括Fe2O3、ZnO 和MnO共2kg；称取掺杂组分中各组分共0.1kg；
（2）主体组分预处理：将称好的主体组分放入强混机和振磨机中强混研磨1h以上，然后放入1050℃的预烧炉中进行预烧处理2～3h，得到平均粒径为6～10μm的预烧粉末；
（3）物料混合：将步骤（2）中得到的预烧粉末与步骤（1）中称量好的掺杂组分混合，然后共混研磨得到粒径为0.8～01.0μm的混合物料，烘干，备用；
（4）造粒并成坯：向步骤（3）中共混研磨后的主体组分和掺杂组分中加入占所述主体组分和掺杂组分总质量的10%的质量浓度为8%的PVA浆料作为粘合浆料，混合均匀后造粒，用模具压制成所需的坯样；
（5）烧结成型：将步骤（4）中所得的坯样放入钟罩炉内，根据平衡氧分压的气氛曲线烧结成型，得到所述低功耗高磁导率和磁滞伸缩锰锌铁氧体；具体地，所述烧结的工艺条件为：先在大气气氛中，以1.5℃/min的升温速率从室温升至650℃，然后在平衡氧分压的条件下，先以1.5℃/min的升温速率从650℃升至1100℃，再以8℃/min的升温速率从1100℃升至1340℃，保温3.5h；最后先以11.5℃/min的降温速率从1340℃降温至1100℃，再以8℃/min的降温速率从1100℃降至室温。
上述方法得到的所述锰锌铁氧体在25℃下的初始磁导率大于等于3000；100KHZ，200mT，25℃下的功率损耗低于550KW/m3；100KHZ，200mT，100℃下的功率损耗低于350KW/m3；居里温度大于等于230℃；1194A/m，25℃下的饱和磁通密度高于510mT，1194A/m，100℃下的饱和磁通密度高于420mT。另外，所得锰锌铁氧体在规定频率下允许有一个较大的磁通偏移，偏移量为100～500。
本发明通过使用高纯和高比表面积的原材料，并结合合适的预烧温度和保温时间，提高了产品的密度和细化晶粒，保证高的饱和磁通密度Bs和低的功耗。
通过烧结条件的控制，达到细化晶粒，提高产品的电阻率，使产品在使用时不发热。
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 (7)

1.一种低功耗高磁导率和磁滞伸缩锰锌铁氧体，其特征在于，包括：主体组分和掺杂组分；所述主体组分包括如下质量百分含量的组分：Fe2O3 71.1～71.3%、ZnO 6.5～6.7%，余量为MnO，总量为100%；所述掺杂组分包括如下组分：CaO、Nb2O5、ZrO2、V2O5、Co2O3和NiO；所述掺杂组分占所述主体组分总质量的1～5%。
2.根据权利要求1所述的低功耗高磁导率和磁滞伸缩锰锌铁氧体，其特征在于，所述掺杂组分中各组分的质量比为：CaO：Nb2O5：ZrO2：V2O5：Co2O3：NiO为3～5：1～2：1～3：2～3：3～4：1～2。
3.根据权利要求1所述的低功耗高磁导率和磁滞伸缩锰锌铁氧体，其特征在于，所述锰锌铁氧体在25℃下的初始磁导率大于等于3000；100KHZ，200mT，25℃下的功率损耗低于550KW/m3；100KHZ，200mT，100℃下的功率损耗低于350KW/m3；居里温度大于等于230℃；1194A/m，25℃下的饱和磁通密度高于490mT，1194A/m，100℃下的饱和磁通密度高于420mT。
4.一种如权利要求1-3任一项所述的低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，其特征在于，包括如下步骤：
（1）称量：按配方量称取主体组分和掺杂组分备用；
（2）主体组分预处理：将称好的主体组分放入强混机和振磨机中强混研磨，然后放入回转窑预烧处理，得到预烧粉末；
（3）物料混合：将步骤（2）中得到的预烧粉末与步骤（1）中称量好的掺杂组分混合，然后经过砂磨机共混研磨得到粒径为0.8～1.0μm的混合物料，烘干，备用；
（4）造粒：向步骤（3）中共混研磨后的主体组分和掺杂组分中加入一定量的粘合浆料，混合均匀后，烘干造粒，粒料用模具压制成所需的坯样；
（5）烧结成型：将步骤（4）中所得的坯样放入钟罩炉内，根据平衡氧分压的气氛曲线烧结成型，得到所述低功耗高磁导率和磁滞伸缩锰锌铁氧体。
5.根据权利要求4所述的低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，其特征在于，所述步骤（2）中，所述预烧处理的工艺条件为：950～1050℃，2～3h。
6.根据权利要求4所述的低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，其特征在于，所述步骤（4）中，所述粘合浆料为质量浓度为6～8%的PVA浆料，其加入质量占所述主体组分和掺杂组分总质量的8～10%。
7.根据权利要求4所述的低功耗高磁导率和磁滞伸缩锰锌铁氧体的制备方法，其特征在于，所述步骤（5）中，所述烧结的工艺条件为：先在大气气氛中，以1～1.5℃/min的升温速率从室温升至650℃，然后在平衡氧分压的条件下，先以1～1.5℃/min的升温速率从650℃升至1100℃，再以5～8℃/min的升温速率从1100℃升至1340℃，保温3.5～6.5h；最后先以1～1.5℃/min的降温速率从1340℃降温至1100℃，再以5～8℃/min的降温速率从1100℃降至室温。
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