CN108275992B - 宽温低功耗高磁导率锰锌铁氧体材料及其制备方法 - Google Patents

宽温低功耗高磁导率锰锌铁氧体材料及其制备方法 Download PDF

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CN108275992B
CN108275992B CN201810049071.9A CN201810049071A CN108275992B CN 108275992 B CN108275992 B CN 108275992B CN 201810049071 A CN201810049071 A CN 201810049071A CN 108275992 B CN108275992 B CN 108275992B
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ferrite material
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manganese
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黄有东
李申华
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Nantong Sanjia Magnetic Industry Co ltd
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Abstract

本发明公开了一种宽温低功耗高磁导率锰锌铁氧体材料及其制备方法，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成分：Fe2O3 55.8～58.7%、ZnO 9.8～11.2%，余量为MnO，总量为100%；本发明通过相对降低主体组成中的Fe2O3的含量，并结合特殊的掺杂工艺，使得晶粒得到充分细化，减少不规则的大晶粒的概率，有效改善了锰锌软磁铁氧体材料的功率损耗，同时拓宽了材料的工作温度范围，具有宽温、低功耗和较高的磁导率等优异性能，有利于变压器器件的小型化，降低工业规模化生产的成本，提高工作效率。

Description

宽温低功耗高磁导率锰锌铁氧体材料及其制备方法
技术领域
本发明涉及锰锌铁氧体材料领域，特别是涉及一种宽温低功耗高磁导率锰锌铁氧体材料及其制备方法。
背景技术
由于电子信息产业的高速发展，电子产品更新换代速度加快，产品向环保型、节能型和小型化发展。这使得电子产品的基础材料——磁性材料得到空前发展。在通讯行业、IT行业、汽车行业等等的大量应用，促使高性能铁氧体产品的快速发展。
目前，家用电子产品逐步体积减少，并且要求节能降耗，带来的电源变压器的结构向小型化、扁平化发展，产品重量大幅度减少，成本降低。现有磁性材料由于受使用温度、磁导率、功耗等的限制，不能满足行业发展的需求。
发明内容
本发明主要解决的技术问题是提供一种宽温低功耗高磁导率锰锌铁氧体材料及其制备方法。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种宽温低功耗高磁导率锰锌铁氧体材料，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3～5%；所述主体组分包括如下质量百分含量的成分：Fe2O3 55.8～58.7%、ZnO 9.8～11.2%，余量为MnO，总量为100%；所述掺杂组分包括CaCO3、SiO2、NiO、Nb2O5、SnO2、Co2O3、La2O3和Li2CO3。
在本发明一个较佳实施例中，所述掺杂组分中各成分的质量比为：CaCO3：SiO2：NiO：Nb2O5：SnO2：Co2O3：La2O3：Li2CO3为3～4：2～3：1～2：1～1.5：0.8～1.2：0.5～0.8：0. 3～0.5：0.5～1。
在本发明一个较佳实施例中，所述ZnO的纯度大于99.9%，比表面积为4.5～4.8m2/g；所述Mn3O4的纯度大于99.8%，比表面积为6.0～10.0m2/g；所述Fe2O3的纯度大于99.8%，比表面积为4.2～4.5m2/g。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种宽温低功耗高磁导率锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配方量称取主体组分和掺杂组分；
（2）一次研磨：将称量的Fe2O3、MnO、ZnO、CaCO3和NiO加入到球磨机中，加入去离子水进行球磨处理，取出后沥干，得到平均粒径为3～5μm的混合料；
（3）预烧：将步骤（2）中经一次研磨和烘干后的混合物料加入预烧炉中，预烧处理，得到预烧粉料；
（4）二次研磨：向步骤（3）中得到的预烧粉中加入掺杂组分中的剩余组分，然后加入去离子水进行球磨处理，取出，烘干，得到平均粒径为0.5～1.0μm的混合料；
（5）制坯：向步骤（4）中经二次研磨所得的混合料中加入粘合浆料，混合均匀后，用模具压制成所需的坯样；
（6）烧结成型：将步骤（5）中所得的坯样放入钟罩炉内，在一定氧分压下进行加热烧结，再降温冷却处理，得到所述宽温低功耗高直流叠加特性锰锌铁氧体材料。
在本发明一个较佳实施例中，所述步骤（2）中，所述料、球和去离子水的质量比为1∶3～3.5∶1.5～1.8；所述球磨处理的时间为6h以上；所述步骤（4）中，所述料、球和去离子水的质量比为1∶3.5～4∶1.5～2.0；所述球磨处理的时间为12h以上。
在本发明一个较佳实施例中，所述步骤（3）中，所述预烧处理的工艺条件为：空气气氛下，在950～980℃下恒温烧结2～3h，然后通入氮气，使氧分压在为5～8%，随炉降温至500℃，再控制氧分压为2～3%，继续降温至室温。
在本发明一个较佳实施例中，所述步骤（5）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（6）中，所述烧结工艺条件为：先在大气气氛中，以1～1.5℃/min的升温速率从室温升至650℃，然后在氧分压为0.05%的条件下，以2～3℃/min的升温速率从650℃升至1000℃，再调整氧分压至1%，以5～8℃/min的升温速率从1000℃升至1150℃，再以10℃/min的升温速率从1150℃升温至1380℃，保温3.5～6.5h；降温阶段，在1～3%的氧分压下，以2～2.5℃/min的降温速率从1380℃降温至1100℃，再在氧分压为0.5～1.5%，以5～8℃/min的降温速率从1100℃降至500℃，最后以0.01～0.05%的氧分压，2.5～3℃/min的速率将至室温。
本发明的有益效果是：本发明一种宽温低功耗高磁导率锰锌铁氧体材料的制备方法，通过相对降低主体组成中的Fe2O3的含量，并结合特殊的掺杂工艺和烧结成型工艺，使得晶粒得到充分细化，减少不规则的大晶粒的概率，有效改善了锰锌软磁铁氧体材料的功率损耗，同时拓宽了材料的工作温度范围，具有宽温、低功耗和较高的磁导率等优异性能，有利于变压器器件的小型化，降低工业规模化生产的成本，提高工作效率。
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
本发明揭示了一种宽温低功耗高磁导率锰锌铁氧体材料，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3%；所述主体组分包括如下质量百分含量的成分：Fe2O3 55.8%、ZnO 9.8%，MnO 34.4；所述掺杂组分包括CaCO3、SiO2、NiO、Nb2O5、SnO2、Co2O3、La2O3和Li2CO3，且掺杂组分中各成分的质量比为：CaCO3：SiO2：NiO：Nb2O5：SnO2：Co2O3：La2O3：Li2CO3为3：2：1：1：0.8：0.5：0. 3：0.5。
其中，所述ZnO的纯度大于99.9%，比表面积为4.5～4.8m2/g；所述Mn3O4的纯度大于99.8%，比表面积为6.0～10.0m2/g；所述Fe2O3的纯度大于99.8%，比表面积为4.2～4.5m2/g。通过选择高纯度和高比表面积的原材料，有助于提高锰锌铁氧体产品的密度和细化晶粒，保证产品具有高的饱和磁通密度和低的功率损耗。
上述的宽温低功耗高磁导率锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配方量称取主体组分和掺杂组分；
（2）一次研磨：将称量的Fe2O3、MnO、ZnO、CaCO3和NiO加入到球磨机中，加入去离子水使料、球和去离子水的质量比为1∶3∶1.5；然后进行球磨处理6h以上，取出后沥干，得到平均粒径为3～5μm的混合料；
（3）预烧：将步骤（2）中经一次研磨和烘干后的混合物料加入预烧炉中，在空气气氛下，先在950℃下恒温烧结3h，然后通入氮气，使氧分压在为5%，随炉降温至500℃，再控制氧分压为2%，继续降温至室温，完成预烧处理，得到预烧粉料；
（4）二次研磨：向步骤（3）中得到的预烧粉中加入掺杂组分中的剩余组分，然后加入去离子水，使料、球和去离子水的质量比为1∶3.5∶1.5，然后进行球磨处理12h以上，取出，烘干，得到平均粒径为0.5～1.0μm的混合料；
（5）制坯：向步骤（4）中经二次研磨所得的混合料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，用模具压制成所需的坯样；
（6）烧结成型：将步骤（5）中所得的坯样放入钟罩炉内，在一定氧分压下进行加热烧结，再降温冷却处理，得到所述宽温低功耗高直流叠加特性锰锌铁氧体材料。所述烧结工艺条件为：先在大气气氛中，以1℃/min的升温速率从室温升至650℃，然后在氧分压为0.05%的条件下，以2℃/min的升温速率从650℃升至1000℃，再调整氧分压至1%，以5℃/min的升温速率从1000℃升至1150℃，再以10℃/min的升温速率从1150℃升温至1380℃，保温3.5h；降温阶段，在1%的氧分压下，以2℃/min的降温速率从1380℃降温至1100℃，再在氧分压为0.5%，以5℃/min的降温速率从1100℃降至500℃，最后以0.01%的氧分压，2.5℃/min的速率将至室温。
实施例2
本发明揭示了一种宽温低功耗高磁导率锰锌铁氧体材料，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%；所述主体组分包括如下质量百分含量的成分：Fe2O3 58.7%、ZnO 11.2%，MnO 30.1；所述掺杂组分包括CaCO3、SiO2、NiO、Nb2O5、SnO2、Co2O3、La2O3和Li2CO3，且掺杂组分中各成分的质量比为：CaCO3：SiO2：NiO：Nb2O5：SnO2：Co2O3：La2O3：Li2CO3为4：3：2：1.5：1.2：0.8：0.5：1。
其中，所述ZnO的纯度大于99.9%，比表面积为4.5～4.8m2/g；所述Mn3O4的纯度大于99.8%，比表面积为6.0～10.0m2/g；所述Fe2O3的纯度大于99.8%，比表面积为4.2～4.5m2/g。通过选择高纯度和高比表面积的原材料，有助于提高锰锌铁氧体产品的密度和细化晶粒，保证产品具有高的饱和磁通密度和低的功率损耗。
上述的宽温低功耗高磁导率锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配方量称取主体组分和掺杂组分；
（2）一次研磨：将称量的Fe2O3、MnO、ZnO、CaCO3和NiO加入到球磨机中，加入去离子水使料、球和去离子水的质量比为1∶3.5∶1.8；然后进行球磨处理6h以上，取出后沥干，得到平均粒径为3～5μm的混合料；
（3）预烧：将步骤（2）中经一次研磨和烘干后的混合物料加入预烧炉中，在空气气氛下，先在980℃下恒温烧结2h，然后通入氮气，使氧分压在为8%，随炉降温至500℃，再控制氧分压为3%，继续降温至室温，完成预烧处理，得到预烧粉料；
（4）二次研磨：向步骤（3）中得到的预烧粉中加入掺杂组分中的剩余组分，然后加入去离子水，使料、球和去离子水的质量比为1∶4∶2.0，然后进行球磨处理12h以上，取出，烘干，得到平均粒径为0.5～1.0μm的混合料；
（5）制坯：向步骤（4）中经二次研磨所得的混合料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，用模具压制成所需的坯样；
（6）烧结成型：将步骤（5）中所得的坯样放入钟罩炉内，在一定氧分压下进行加热烧结，再降温冷却处理，得到所述宽温低功耗高直流叠加特性锰锌铁氧体材料。所述烧结工艺条件为：先在大气气氛中，以1.5℃/min的升温速率从室温升至650℃，然后在氧分压为0.05%的条件下，以3℃/min的升温速率从650℃升至1000℃，再调整氧分压至1%，以8℃/min的升温速率从1000℃升至1150℃，再以10℃/min的升温速率从1150℃升温至1380℃，保温6.5h；降温阶段，在3%的氧分压下，以2.5℃/min的降温速率从1380℃降温至1100℃，再在氧分压为1.5%，以8℃/min的降温速率从1100℃降至500℃，最后以0.05%的氧分压，3℃/min的速率将至室温。
所述锰锌铁氧体材料，经测试，其工作温度在-10～120℃的温度范围内，
1.0KHz，0.3V， 23±3℃，初始磁导率μi＝3000±25%。
100KHz、200mT，25℃，Pv≤650mW/cm3，
100KHz、200mT，100℃，Pv≤350 mW/cm3;
1194A/m,100℃的BS≥420mT。
本发明通过相对降低主体组成中的Fe2O3的含量，并结合特殊的掺杂工艺和烧结成型工艺，使得晶粒得到充分细化，减少不规则的大晶粒的概率，有效改善了锰锌软磁铁氧体材料的功率损耗，同时拓宽了材料的工作温度范围，具有宽温、低功耗和较高的磁导率等优异性能，有利于变压器器件的小型化，降低工业规模化生产的成本，提高工作效率。
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 (5)

1.一种宽温低功耗高磁导率锰锌铁氧体材料，其特征在于，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3～5%；所述主体组分包括如下质量百分含量的成分：Fe2O3 55 .8～58 .7%、ZnO 9 .8～11 .2%，余量为MnO，总量为100%；所述掺杂组分包括CaCO3、SiO2、NiO、Nb2O5、SnO2、Co2O3、La2O3和Li2CO3；所述掺杂组分中各成分的质量比为：CaCO3：SiO2：NiO：Nb2O5：SnO2：Co2O3：La2O3：Li2CO3为3～4：2～3：1～2：1～1 .5：0 .8～1 .2：0.5～0 .8：0 . 3～0 .5：0 .5～1；
所述的宽温低功耗高磁导率锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配方量称取主体组分和掺杂组分；
（2）一次研磨：将称量的Fe2O3、MnO、ZnO、CaCO3和NiO加入到球磨机中，加入去离子水进行球磨处理，取出后沥干，得到平均粒径为3～5μm的混合料；
（3）预烧：将步骤（2）中经一次研磨和烘干后的混合物料加入预烧炉中，预烧处理，得到预烧粉料；
（4）二次研磨：向步骤（3）中得到的预烧粉中加入掺杂组分中的剩余组分，然后加入去离子水进行球磨处理，取出，烘干，得到平均粒径为0 .5～1 .0μm的混合料；
（5）制坯：向步骤（4）中经二次研磨所得的混合料中加入粘合浆料，混合均匀后，用模具压制成所需的坯样；
（6）烧结成型：将步骤（5）中所得的坯样放入钟罩炉内，在一定氧分压下进行加热烧结，再降温冷却处理，得到所述宽温低功耗高磁导率锰锌铁氧体材料；
所述烧结工艺条件为：先在大气气氛中，以1～1 .5℃/min的升温速率从室温升至650℃，然后在氧分压为0 .05%的条件下，以2～3℃/min的升温速率从650℃升至1000℃，再调整氧分压至1%，以5～8℃/min的升温速率从1000℃升至1150℃，再以10℃/min的升温速率从1150℃升温至1380℃，保温3 .5～6 .5h；降温阶段，在1～3%的氧分压下，以2～2 .5℃/min的降温速率从1380℃降温至1100℃，再在氧分压为0 .5～1 .5%，以5～8℃/min的降温速率从1100℃降至500℃，最后以0 .01～0 .05%的氧分压，2 .5～3℃/min的速率降至室温。
2.根据权利要求1所述的宽温低功耗高磁导率锰锌铁氧体材料，其特征在于，所述ZnO的纯度大于99 .9%，比表面积为4 .5～4 .8m2/g；所述Mn3O4的纯度大于99 .8%，比表面积为6 .0～10 .0m2/g；所述Fe2O3的纯度大于99 .8%，比表面积为4 .2～4 .5m2/g。
3.根据权利要求1所述的宽温低功耗高磁导率锰锌铁氧体材料，其特征在于，所述步骤（2）中，所述料、球和去离子水的质量比为1∶3～3 .5∶1 .5～1 .8；所述球磨处理的时间为6h以上；所述步骤（4）中，所述料、球和去离子水的质量比为1∶3 .5～4∶1 .5～2 .0；所述球磨处理的时间为12h以上。
4.根据权利要求1所述的宽温低功耗高磁导率锰锌铁氧体材料，其特征在于，所述步骤（3）中，所述预烧处理的工艺条件为：空气气氛下，在950～980℃下恒温烧结2～3h，然后通入氮气，使氧分压为5～8%，随炉降温至500℃，再控制氧分压为2～3%，继续降温至室温。
5.根据权利要求1所述的宽温低功耗高磁导率锰锌铁氧体材料，其特征在于，所述步骤（5）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%。
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