CN107056268A - 汽车充电桩用大功率锰锌铁氧体磁芯及其制备方法 - Google Patents

汽车充电桩用大功率锰锌铁氧体磁芯及其制备方法 Download PDF

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CN107056268A
CN107056268A CN201710293735.1A CN201710293735A CN107056268A CN 107056268 A CN107056268 A CN 107056268A CN 201710293735 A CN201710293735 A CN 201710293735A CN 107056268 A CN107056268 A CN 107056268A
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柯宇翔
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GUANDA MAGNETIC IND CO Ltd SUZHOU
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Abstract

本发明公开了一种汽车充电桩用大功率锰锌铁氧体磁芯，包括主成分和副成分；主成分Fe2O3、MnO和ZnO；副成分包括钙氧化物、镍氧化物、铋氧化物和钼氧化物，副成分的总量相对于主成分总量的重量百分比含量为0.20~0.90wt%。其制备方法步骤如下：称料；掺杂；压制坯料；排坯；烧结处理。本发明通过特殊的掺杂工艺及烧结工艺曲线，使其材料的磁导率在负温度与高温条件下都具备较高的磁导率，居里温度高，且具有良好的温升特性，温度曲线平坦、高温功耗低，工作环境适应性强，为用户提供了使用领域更广泛，体积更小，更高效，损耗低的电源设备，市场前景广阔。

Description

汽车充电桩用大功率锰锌铁氧体磁芯及其制备方法
技术领域
本发明涉及锰锌铁氧体领域，特别是涉及一种汽车充电桩用大功率锰锌铁氧体磁芯及其制备方法。
背景技术
随着跨领域电子设备产业的高速发展，电动汽车行业充电桩产业发展迅速，而其中最关键的技术在于嵌套的软磁铁氧体材料及产品。软磁铁氧体由于其成本方面的优势，越来越多的被用来替换传统永磁，同时其良好的配合特性也能帮助实现元器件更好的特性。功率型锰锌铁氧体材料功耗低，频率特性好，适用温度范围广，有利于设计大型充电电源，抗干扰程度高，不同温度工作环境下的稳定性好，符合电子元器件的发展趋势。
磁性材料在滤波器、开关电源、及变压器应用电子产品中均占有部分体积并消耗部分能源。因此提高磁芯初始磁导率及频率特性，使大功率产品向小型号、高效化发展，对我国电子产业结构调整，节能减排提供有效帮助。
发明内容
本发明主要解决的技术问题是提供一种汽车充电桩用大功率锰锌铁氧体磁芯及其制备方法。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种汽车充电桩用大功率锰锌铁氧体磁芯，包括：主成分和副成分；所述主成分包括以各自标准物计的摩尔百分比含量为50～54mol%的Fe2O3、39～42mol%的MnO和5～9mol%的ZnO；所述副成分包括钙氧化物、镍氧化物、铋氧化物和钼氧化物，相对所述主成分总量，钛氧化物、镍氧化物、铋氧化物和钼氧化物以其标准物CaCO3、NiO、Bi2O3和MoO3计的总重量百分比含量为0.20~0.90wt%。
在本发明一个较佳实施例中，所述副成分以各自标准物计的重量百分比含量分别为：CaCO3 250～ 1200ppm、NiO 200～5000ppm、Bi2O3 100～1000ppm，MoO3 80～600ppm。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将步骤（1）中称取的辅助成分先后分3次以上加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先进行混合预烧，再进行研磨处理，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向步骤（2）中得到的混合料中先后加入去离子水和分散剂，搅拌成均一的浆料，再将所述浆料用专用模具压制成磁芯坯料；
（4）排坯：将步骤（3）中得到的坯料在烧结架上按一定的空间间距进行单层排坯处理，并在磁芯坯料的底层撒一层刚玉砂；
（5）烧结处理：将步骤（4）中经排坯后的磁芯坯料置入烧结窑炉内，在平衡气氛下烧结成型。
在本发明一个较佳实施例中，所述步骤（2）中，所述混合预烧的条件为：温度600～800℃，时间5～15min；所述混合研磨在行星球磨机中进行，每次研磨时间为5～15min。
在本发明一个较佳实施例中，所述步骤（4）中，所述磁芯坯料的空间间距为1～1.5cm。
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：在5～8%氮气含量的平衡气压下，先以30～50℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1400℃，恒温保持6h，然后再以30～50℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温。
本发明的有益效果是：本发明通过特殊的掺杂工艺及烧结工艺曲线，使其材料的磁导率在负温度与高温条件下都具备较高的磁导率，居里温度高，且具有良好的温升特性，温度曲线平坦、高温功耗低，工作环境适应性强，为用户提供了使用领域更广泛，体积更小，更高效，损耗低的电源设备，市场前景广阔。
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
一种汽车充电桩用大功率锰锌铁氧体磁芯，包括：主成分和副成分；所述主成分包括氧化铁、氧化锰和氧化锌，氧化铁、氧化锰和氧化锌以各自标准物计的摩尔百分比含量为Fe2O3 50mol%、MnO 42mol%、ZnO 8mol%；所述副成分包括钙氧化物、镍氧化物、铋氧化物和钼氧化物，相对所述主成分总量，钛氧化物、镍氧化物、铋氧化物和钼氧化物以其标准物CaCO3、NiO、Bi2O3和MoO3计的总重量百分比含量为0.20wt%，具体地，副成分以各自标准物计的重量百分比含量分别为：CaCO3 250ppm、NiO 200 ppm、Bi2O3 100 ppm，MoO3 80 ppm。
上述汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将上述称取的辅助成分先后分3次以上加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先在600℃下混合预烧15min，再在行星球磨机中研磨处理5～15min，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向步骤（2）中得到的混合料中先后加入去离子水和分散剂，搅拌成均一的浆料，再将所述浆料用专用模具压制成磁芯坯料；
（4）排坯：将步骤（3）中得到的坯料在烧结架上按1cm的空间间距（即前后左右间距）进行单层排坯处理，并在底层撒一层刚玉砂，垫片下方设计多方向的槽口；磁芯之间的空间间距设计便于热气流流通，从而使整个磁芯在烧结窑炉中的受热程度均匀，可有效保证磁芯的整体性能均一稳定；
（5）烧结处理：将步骤（4）中经排坯后的磁芯坯料置入烧结窑炉内，在充分考虑节能及排胶、烧结均匀性及兼顾主成分及辅助成分特性的基础上，按布莱克方程式设定气氛曲线，并采用如下烧结工艺进行烧结：在5%氮气含量的平衡气压下，先以50℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1400℃，恒温保持6h，然后再以50℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温；通过延长高温条件下的烧结保温时间，达到降低磁芯的高温功耗水平、提高TC，降低产品温度系数, 使温度曲线趋于平坦之目的。另外，通过适当降低烧结温度，在保证高温功耗水平、提高TC及降低产品温度系数的前提下降低了颗粒间的活性，一方面用于减少磁芯微观间隙，增加饱和磁通密度，另一方面也间接提高了烧结后的产品强度。
实施例2
一种汽车充电桩用大功率锰锌铁氧体磁芯，包括：主成分和副成分；所述主成分包括氧化铁、氧化锰和氧化锌，氧化铁、氧化锰和氧化锌以各自标准物计的摩尔百分比含量为Fe2O3 54mol%、MnO 39mol%、ZnO 7mol%；所述副成分包括钙氧化物、镍氧化物、铋氧化物和钼氧化物，相对所述主成分总量，钛氧化物、镍氧化物、铋氧化物和钼氧化物以其标准物CaCO3、NiO、Bi2O3和MoO3计的总重量百分比含量为0.90wt%，具体地，副成分以各自标准物计的重量百分比含量分别为：CaCO3 1200ppm、NiO 5000ppm、Bi2O3 1000ppm，MoO3 600ppm。
上述汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将上述称取的辅助成分先后分3次以上加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先在800℃下混合预烧5min，再在行星球磨机中研磨处理5～15min，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向步骤（2）中得到的混合料中先后加入去离子水和分散剂，搅拌成均一的浆料，再将所述浆料用专用模具压制成磁芯坯料；
（4）排坯：将步骤（3）中得到的坯料在烧结架上按1.5cm的空间间距（即前后左右间距）进行单层排坯处理，并在底层撒一层刚玉砂，垫片下方设计多方向的槽口；磁芯之间的空间间距设计便于热气流流通，从而使整个磁芯在烧结窑炉中的受热程度均匀，可有效保证磁芯的整体性能均一稳定；
（5）烧结处理：将步骤（4）中经排坯后的磁芯坯料置入烧结窑炉内，在充分考虑节能及排胶、烧结均匀性及兼顾主成分及辅助成分特性的基础上，按布莱克方程式设定气氛曲线，并采用如下烧结工艺进行烧结：在8%氮气含量的平衡气压下，先以30℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1400℃，恒温保持6h，然后再以30℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温；其中，较长的保温时间有助于达到降低磁芯的高温功耗水平、提高TC，降低产品温度系数, 使温度曲线趋于平坦之目的。另外，通过适当降低烧结温度，在保证高温功耗水平、提高TC及降低产品温度系数的前提下降低了颗粒间的活性，一方面用于减少磁芯微观间隙，增加饱和磁通密度，另一方面也间接提高了烧结后的产品强度。
上述方法得到的汽车充电桩用大功率锰锌铁氧体磁芯，是一种适应汽车充电桩用大功率的低损耗铁氧体材料产品，磁芯不易开裂和变形，居里温度高，且具有良好的温升特性，温度曲线平坦、高温功耗低，工作环境适应性强。经测试，具体性能特点如下：
1）性能层面，1.0KHz，0.3V，25±3℃条件下，初始磁导率μi=3300±25%；
2）具有良好的温度特性，温度曲线平坦，适合工作温度为-30～200℃；
3）居里温度高，Tc≥230℃；
4）高温功耗低，100KHz 200mT 70～100℃的功耗小于350kw/m3。
本发明的锰锌铁氧体磁芯为用户提供使用领域更广泛，体积更小，更高效，损耗低的电源设备，并且能够应用于与其他充电设备设施，如无线通讯，智能电表终端、工业集成设备、海底电缆、光缆水下设备等特殊环境。
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 (6)

1.一种汽车充电桩用大功率锰锌铁氧体磁芯，其特征在于，包括：主成分和副成分；所述主成分包括以各自标准物计的摩尔百分比含量为50～54mol%的Fe2O3、39～42mol%的MnO和5～9mol%的ZnO；所述副成分包括钙氧化物、镍氧化物、铋氧化物和钼氧化物，相对所述主成分总量，钛氧化物、镍氧化物、铋氧化物和钼氧化物以其标准物CaCO3、NiO、Bi2O3和MoO3计的总重量百分比含量为0.20~0.90wt%。
2.根据权利要求1所述的汽车充电桩用大功率锰锌铁氧体磁芯，其特征在于，所述副成分以各自标准物计的重量百分比含量分别为：CaCO3 250～ 1200ppm、NiO 200～5000ppm、Bi2O3 100～1000ppm，MoO3 80～600ppm。
3.一种如权利要求1或2所述的汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，其特征在于，包括如下步骤：
（1）称料：按配方称取所述主成分和辅助成分；
（2）掺杂：将步骤（1）中称取的辅助成分先后分3次以上加入到称取的主成分中，每次加入辅助成分后，将加入的辅助成分与主成分先进行混合预烧，再进行研磨处理，最后将全部的辅助成分与主成分混合研磨得到平均粒径为0.1～0.3μm的混合组分；
（3）压制坯料：向步骤（2）中得到的混合料中先后加入去离子水和分散剂，搅拌成均一的浆料，再将所述浆料用专用模具压制成磁芯坯料；
（4）排坯：将步骤（3）中得到的坯料在烧结架上按一定的空间间距进行单层排坯处理，并在磁芯坯料的底层撒一层刚玉砂；
（5）烧结处理：将步骤（4）中经排坯后的磁芯坯料置入烧结窑炉内，在平衡气氛下烧结成型。
4.根据权利要求3所述的汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，其特征在于，所述步骤（2）中，所述混合预烧的条件为：温度600～800℃，时间5～15min；所述混合研磨在行星球磨机中进行，每次研磨时间为5～15min。
5.根据权利要求3所述的汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，其特征在于，所述步骤（4）中，所述磁芯坯料的空间间距为1～1.5cm。
6.根据权利要求3所述的汽车充电桩用大功率锰锌铁氧体磁芯的制备方法，其特征在于，所述步骤（5）中，所述烧结的工艺条件为：在5～8%氮气含量的平衡气压下，先以30～50℃/min的升温速率从室温升至1000℃，然后再以100℃/min的升温速率升温至1400℃，恒温保持6h，然后再以30～50℃/min的降温速率将至1100℃，恒温保持1～2h，最后随炉自然冷却至室温。
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