CN108275991A - 电源变压器用低功耗锰锌铁氧体材料及其制备方法 - Google Patents

电源变压器用低功耗锰锌铁氧体材料及其制备方法 Download PDF

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CN108275991A
CN108275991A CN201810049764.8A CN201810049764A CN108275991A CN 108275991 A CN108275991 A CN 108275991A CN 201810049764 A CN201810049764 A CN 201810049764A CN 108275991 A CN108275991 A CN 108275991A
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consumption
ferrite material
component
power transformer
doping
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黄有东
李申华
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CHANGSHU SANJIA MAGNETIC Co Ltd
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CHANGSHU SANJIA MAGNETIC Co Ltd
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Abstract

本发明公开了一种电源变压器用低功耗锰锌铁氧体材料及其制备方法，包括主体成分和掺杂组分；所述掺杂组分占主体组分总质量的3～6%；主体组分包括质量百分含量为Fe2O3 69.38～70.51%、Mn3O4 22.02～23.30%，余下为ZnO，总和为100%；掺杂组分包括CaCO3、CaO、SiO2、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3和Li2CO3。本发明有效提高了锰锌铁氧体材料的饱和磁通密度，并降低高、低温功率损耗，所得产品在较宽的工作温度范围内具有低的功率损耗，高的饱和磁通密度和磁导率，技术含量高，性能优异，在开关电源变压器、汽车充电器等领域，具有广阔的应用市场。

Description

电源变压器用低功耗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，特别是涉及一种电源变压器用低功耗锰锌铁氧体材料及其制备方法。
背景技术
在现代科技社会中，磁性材料已成为必不可少的功能性基础材料。其应用领域有航空、航天、汽车、电子信息、通讯、照明、家用电器、矿山机械、工业技术等。其在国民经济中的地位越来越重要，特别是家庭用电器如电视机、电脑、音响、DVD机、空调机、洗 衣机、手机、汽车、玩具、灯具、家具等都离不开磁性材料，其磁性材料的用途越来越重要。
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。另外，随着信息产业技术的迅猛发展，在整机应用时要进一步降低功率转换信号传输所产生的各种能量损耗，要求最强烈的就是开关电源用功率铁氧体材料及磁芯元件，而现有开关电源变压器高频工作时会产生铁损、铜损、温升及电感等问题，不能满足使用需求。
发明内容
本发明主要解决的技术问题是提供一种电源变压器用低功耗锰锌铁氧体材料及其制备方法，能够满足现有电源变压器行业的发展需求。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种电源变压器用低功耗锰锌铁氧体材料，所述锰锌铁氧体材料在23±3℃下的初始磁导率大于等于2800；在100KHZ，200mT，25℃下的功率损耗小于等于700mW/cm3；100KHZ，200mT，100℃下的功率损耗小于等于350mW/cm3； 1194A/m，100℃下的饱和磁通密度高于420mT；所述锰锌铁氧体材料包括：主体成分和掺杂组分；所述掺杂组分占所述主体组分总质量的3～6%；所述主体组分包括如下质量百分含量的成分：Fe2O3 69.38～70.51%、Mn3O4 22.02～23.30%，余下为ZnO，总和为100%；所述掺杂组分包括：CaCO3、CaO、SiO2、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3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：CaO：SiO2：MoO3：Nb2O5：Ta2O5：ZrO2：Co2O3：K2CO3：Li2CO3为2～3：1～2：3～4：0.5～1：1～1.2：0.5～0.8：0.6～1.2：1～1.5：1～1.5。
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10～15m2/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，本发明采用的一个技术方案是：提供一种电源变压器用低功耗锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配方量的主体组分和掺杂组分换算成质量份，然后称量备用；
（2）一次研磨：将称量的Fe2O3、Mn3O4和ZnO加入到球磨机中，加入去离子水进行球磨处理，得到平均粒径为3～5μm的混合料，然后烘干；
（3）预烧：将步骤（2）中经一次研磨和烘干后的主体组分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，然后加入去离子水进行球磨处理，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，在平衡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，所述去离子水的加入量占所述主体组分总质量的1～1.5倍，所述球磨处理的时间为1.5h以上；所述步骤（4）中，所述去离子水的加入量占所述主体组分和掺杂组分总质量的2～2.5倍；所述球磨处理的时间为2h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℃，然后在平衡氧分压的条件下，先2～3℃/min的升温速率从650℃升至1000℃，再以5～8℃/min的升温速率从1000℃升至1150℃，最后以10℃/min的升温速率从1150℃升温至1350℃，保温4～6h；所述降温工艺条件为：在1～3%的氧分压下，以2～2.5℃/min的降温速率从1350℃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：本发明一种电源变压器用低功耗锰锌铁氧体材的制备方法，通过使用高纯度、高比表面积的原材料，并提高主体组分中氧化锌的含量，有效提高了锰锌铁氧体材料的饱和磁通密度，并降低高、低温功率损耗，所得的锰锌铁氧体材料在较宽的工作温度范围内具有低的功率损耗，高的饱和磁通密度和磁导率，技术含量高，性能优异，在开关电源变压器、汽车充电器等领域，具有广阔的应用市场。
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
本发明揭示了一种电源变压器用低功耗锰锌铁氧体材料，包括：主体成分和掺杂组分；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 69.38%、Mn3O4 22.02%，ZnO为8.6%；所述掺杂组分包括：CaCO3、CaO、SiO2、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3和Li2CO3，其中，各成分的质量比为：CaCO3：CaO：SiO2：MoO3：Nb2O5：Ta2O5：ZrO2：Co2O3：K2CO3：Li2CO3为23：1：3：0.5：1：0.5：0.6：1：1。
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10～15m2/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。
上述电源变压器用低功耗锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配量量的主体组分和掺杂组分换算成质量份，然后称量备用；
（2）一次研磨：将称量的Fe2O3、Mn3O4和ZnO加入到球磨机中，加入占所述主体组分总质量的1倍的去离子水进行球磨处理1.5h以上，得到平均粒径为3～5μm的混合料，然后烘干；
（3）预烧：将步骤（2）中经一次研磨和烘干后的主体组分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，预烧处理后，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，然后加入占所述主体组分和掺杂组分总质量的2倍的去离子水进行球磨处理2h以上，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80%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，在平衡氧分压下进行加热烧结，然后降温冷却处理，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℃，然后在平衡氧分压的条件下，先2℃/min的升温速率从650℃升至1000℃，再以5℃/min的升温速率从1000℃升至1150℃，最后以10℃/min的升温速率从1150℃升温至1350℃，保温4h；所述降温工艺为：在1%的氧分压下，以2℃/min的降温速率从1350℃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
本发明揭示了一种电源变压器用低功耗锰锌铁氧体材料，包括：主体成分和掺杂组分；所述掺杂组分占所述主体组分总质量的6%；所述主体组分包括如下质量百分含量的成分：Fe2O3 70.51%、Mn3O4 22.02～23.30%，ZnO为6.19%；所述掺杂组分包括：CaCO3、CaO、SiO2、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3和Li2CO3，其中，各成分的质量比为：CaCO3：CaO：SiO2：MoO3：Nb2O5：Ta2O5：ZrO2：Co2O3：K2CO3：Li2CO3为3：2：4：1：1.2：0.8：1.2：1.5：1.5。
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10～15m2/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。
上述电源变压器用低功耗锰锌铁氧体材料的制备方法，包括如下步骤：
（1）称料：将配量量的主体组分和掺杂组分换算成质量份，然后称量备用；
（2）一次研磨：将称量的Fe2O3、Mn3O4和ZnO加入到球磨机中，加入占所述主体组分总质量的1.5倍的去离子水进行球磨处理1.5h以上，得到平均粒径为3～5μm的混合料，然后烘干；
（3）预烧：将步骤（2）中经一次研磨和烘干后的主体组分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，预烧处理后，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，然后加入占所述主体组分和掺杂组分总质量的2～2.5倍的去离子水进行球磨处理2h以上，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，在平衡氧分压下进行加热烧结，然后降温冷却处理，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℃，然后在平衡氧分压的条件下，先3℃/min的升温速率从650℃升至1000℃，再以8℃/min的升温速率从1000℃升至1150℃，最后以10℃/min的升温速率从1150℃升温至1350℃，保温6h；所述降温工艺为：在3%的氧分压下，以2.5℃/min的降温速率从1350℃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。
上述方法得到的所述锰锌铁氧体，经测试，密度高于4.8g/cm3，在23±3℃下的初始磁导率大于等于2800；100KHZ，200mT，25℃下的功率损耗小于等于700mW/cm3；100KHZ，200mT，100℃下的功率损耗小于等于350mW/cm3；居里温度大于等于235℃；1194A/m，100℃下的饱和磁通密度高于420mT。
本发明所得的锰锌铁氧体材料，通过使用高纯度、高比表面积的原材料，并提高主体组分中氧化锌的含量，有效提高了锰锌铁氧体材料的饱和磁通密度，并降低高、低温功率损耗，所得的锰锌铁氧体材料在较宽的工作温度范围内具有低的功率损耗，高的饱和磁通密度和磁导率，技术含量高，性能优异，在开关电源变压器、汽车充电器等领域，具有广阔的应用市场。
主体成分中铁和锌的调整和掺杂组分成分的配比，赋予铁氧体材料良好的宽温高直流叠加特性，并有效控制其高温损耗，通过预烧、两次球磨和烧结成型工艺的调控，使得材料的晶粒细化、均匀，所得材料的密度大，居里温度高，磁滞性能优异。
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 (8)

1.一种电源变压器用低功耗锰锌铁氧体材料，其特征在于，所述锰锌铁氧体材料在23±3℃下的初始磁导率大于等于2800；在100KHZ，200mT，25℃下的功率损耗小于等于700mW/cm3；100KHZ，200mT，100℃下的功率损耗小于等于350mW/cm3；1194A/m，100℃下的饱和磁通密度高于420mT；所述锰锌铁氧体材料包括：主体成分和掺杂组分；所述掺杂组分占所述主体组分总质量的3～6%；所述主体组分包括如下质量百分含量的成分：Fe2O3 69.38～70.51%、Mn3O4 22.02～23.30%，余下为ZnO，总和为100%；所述掺杂组分包括：CaCO3、CaO、SiO2、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3和Li2CO3。
2.根据权利要求1所述的电源变压器用低功耗锰锌铁氧体材料，其特征在于，所述掺杂组分中各成分的质量比为：CaCO3：CaO：SiO2：MoO3：Nb2O5：Ta2O5：ZrO2：Co2O3：K2CO3：Li2CO3为2～3：1～2：3～4：0.5～1：1～1.2：0.5～0.8：0.6～1.2：1～1.5：1～1.5。
3.根据权利要求1所述的电源变压器用低功耗锰锌铁氧体材料，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5.2～5.5m2/g；所述Fe2O3的纯度大于99.8%，比表面积为4.2～4.5m2/g。
4.根据权利要求1-3任一项所述的电源变压器用低功耗锰锌铁氧体材料的制备方法，其特征在于，包括如下步骤：
（1）称料：将配方量的主体组分和掺杂组分换算成质量份，然后称量备用；
（2）一次研磨：将称量的Fe2O3、Mn3O4和ZnO加入到球磨机中，加入去离子水进行球磨处理，得到平均粒径为3～5μm的混合料，然后烘干；
（3）预烧：将步骤（2）中经一次研磨和烘干后的主体组分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，然后加入去离子水进行球磨处理，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，在平衡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。
5.根据权利要求4所述的电源变压器用低功耗锰锌铁氧体材料的制备方法，其特征在于，所述步骤（2）中，所述去离子水的加入量占所述主体组分总质量的1～1.5倍，所述球磨处理的时间为1.5h以上；所述步骤（4）中，所述去离子水的加入量占所述主体组分和掺杂组分总质量的2～2.5倍；所述球磨处理的时间为2h以上。
6.根据权利要求4所述的电源变压器用低功耗锰锌铁氧体材料的制备方法，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。
7.根据权利要求4所述的电源变压器用低功耗锰锌铁氧体材料的制备方法，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%。
8.根据权利要求4所述的电源变压器用低功耗锰锌铁氧体材料的制备方法，其特征在于，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℃，然后在平衡氧分压的条件下，先2～3℃/min的升温速率从650℃升至1000℃，再以5～8℃/min的升温速率从1000℃升至1150℃，最后以10℃/min的升温速率从1150℃升温至1350℃，保温4～6h；所述降温工艺条件为：在1～3%的氧分压下，以2～2.5℃/min的降温速率从1350℃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。
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