CN107200572A - 一种低磁导率温度系数MnZn铁氧体烧结方法 - Google Patents

一种低磁导率温度系数MnZn铁氧体烧结方法 Download PDF

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CN107200572A
CN107200572A CN201710316946.2A CN201710316946A CN107200572A CN 107200572 A CN107200572 A CN 107200572A CN 201710316946 A CN201710316946 A CN 201710316946A CN 107200572 A CN107200572 A CN 107200572A
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temperature
magnetic permeability
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颜冲
雷国莉
葛洪良
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China Jiliang University
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Abstract

本发明提供一种低磁导率温度系数MnZn铁氧体材料的烧结方法，该方法降温段分成三个温度变化阶段，主要包括有：a、第一个降温阶段；b、保温阶段；c、第二个降温阶段。本发明由于在整个降温过程中通过对温度和氧分压的控制，能够降低MnZn铁氧体材料的磁导率温度系数。应用本发明制备的MnZn铁氧体，室温磁导率高，在‑40～200℃的温度范围磁导率变化小。

Description

一种低磁导率温度系数MnZn铁氧体烧结方法
技术领域
本发明涉及一种MnZn铁氧体材料的烧结方法，尤其涉及一种低磁导率温度系数MnZn铁氧体材料的烧结方法。
背景技术
MnZn铁氧体广泛用于电子、通讯领域作为电源变压器和电感器材料。作为这些电子元器件使用的铁氧体磁心，有时其工作环境十分恶劣，如大功率无极灯中使用的磁心，其最高工作温度可能超过200℃。同时在严寒地区，其最低启动温度可能低于-40℃，即希望其在-40～200℃的宽温范围仍然能够正常启动和工作。这就要求MnZn铁氧体材料在-40～200℃宽温范围磁导率变化小，即具有较低的磁导率温度系数。常规的MnZn铁氧体材料难以满足要求，因此需要开发一种宽温低磁导率温度系数MnZn铁氧体材料。低磁导率温度系数MnZn铁氧体的制备，除选用合适的主配方设计和合适的微量添加物外，烧结工艺的控制也是十分重要的。
发明内容
本发明的目的是提供一种在-40～200℃的宽温范围磁导率温度系数都较低的MnZn铁氧体材料烧结方法。在此温度范围，实现了25℃时初始磁导率在3000以上，以此为基数的初始磁导率温度系数在±20%以内。
通过提供以下内容的本发明达到了以上目的。
一种低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，降温部分包括以下步骤：
a、第一个降温阶段：从最高保温温度至1000℃以0.5~2.5℃/分钟降温速率降温，在平衡氧气氛中进行；
b、保温阶段：当降温到1200~1050℃范围，选定一个温度作为保温段，保温时间为0.5~2小时，氧分压维持在0.5~2%；
c、第二个降温阶段：从1000℃降温至室温，降温速率为2.5~5.0℃/分钟，降温过程维持平衡氧分压。
进一步的，步骤a中,所述第一个降温阶段中以1.0~2.0℃/分钟的降温速率降温。
进一步的，步骤b中,所述保温阶段为1150~1100℃范围，选定一个温度作为保温段，保温时间为0.5~1小时，氧分压维持在0.5~1%。
进一步的，步骤c中，所述保温阶段降温至室温，降温速率为3.0~4.0℃/分钟，900℃以下氧分压维持在200ppm以下。
进一步的，所述低磁导率温度系数MnZn铁氧体材料的主要材料为Fe2O3、MnO和ZnO。
进一步的，所述低磁导率温度系数MnZn铁氧体材料还包含有Co2O3作为辅助成分。
进一步的，所述低磁导率温度系数MnZn铁氧体材料还包含有SiO2、CaCO3、SnO2、TiO2、Sb2O3、ZrO2、Nb2O5、Ta2O5、V2O5中的任意四种组合作为微量添加剂成分。
具体实施方式
实施例1
以Fe2O3、MnO、ZnO含量分别为53.2mol％的Fe2O3、38.3mol％的MnO和8.5mol％的ZnO作为主配方。然后把原材料进行湿式混合，然后900℃下预烧2小时。根据主配方的重量，向预烧后的混合物中加入150ppm的SiO2、900ppm的CaCO3、500ppm的TiO2、300ppm的Ta2O5和3500ppm的Co2O3，湿式砂磨，得到一种铁氧体料浆。向料浆中加入按铁氧体粉末重量计算的1wt％的PVA粘结剂，进行喷雾造粒。在一定的压力下把造粒后的粉料成型为测试用的标准环形铁氧体磁心。把成型体在控制氧分压的条件下于1300℃烧结5小时。降温阶段温度控制如表1进行。其中第一降温段维持平衡氧分压，保温阶段的时间为1小时，氧分压为1.0%，第二降温段900℃以下氧分压为100ppm。最终得到外径为25mm、内经为15mm、高为7mm的环形烧结体。通过X荧光分析仪，检测铁氧体磁心的最终组成与设计组成是否一致。
用LCR电感测试仪测量磁心在-40～200℃范围的初始磁导率，磁导率温度系数通过（μT-μ0）/μ0×100%计算得到。其中μT为-40～200℃范围某一温度下材料的初始磁导率，μ0为25℃下材料的初始磁导率。测试条件为f=10kHz、B<0.25mT。
从表1看出，在本发明的降温温度控制方法范围内，25℃时铁氧体材料初始磁导率都在3000以上，在-40～200℃的宽温范围，初始磁导率温度系数在±20%以内。当降温温度控制不在本发明范围内，则或会使25℃初始磁导率下降，或者磁导率温度系数增大。
实施例2
磁心的制备工艺与实施例102相同。只是保温阶段时间、保温阶段氧分压和第二降温阶段900℃以后的氧分压如表2所示。
从表2可以看出，添加剂在本发明范围内，25℃时铁氧体材料初始磁导率都在3000以上，在-40～200℃的宽温范围，初始磁导率温度系数在±20%以内。当主配方不在本发明范围内，则或会使25℃初始磁导率下降，或者磁导率温度系数增大。
表1
表2。

Claims (7)

1.一种低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，降温部分包括以下步骤：
a、第一个降温阶段：从最高保温温度至1000℃以0.5~2.5℃/分钟降温速率降温，在平衡氧气氛中进行；
b、保温阶段：当降温到1200~1050℃范围，选定一个温度作为保温段，保温时间为0.5~2小时，氧分压维持在0.5~2%；
c、第二个降温阶段：从1000℃降温至室温，降温速率为2.5~5.0℃/分钟，降温过程维持平衡氧分压。
2.根据权利要求1所述的低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，步骤a中,所述第一个降温阶段中以1.0~2.0℃/分钟的降温速率降温。
3.根据权利要求1所述的低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，步骤b中,所述保温阶段为1150~1100℃范围，选定一个温度作为保温段，保温时间为0.5~1小时，氧分压维持在0.5~1%。
4.根据权利要求1所述的低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，步骤c中，所述保温阶段降温至室温，降温速率为3.0~4.0℃/分钟，900℃以下氧分压维持在200ppm以下。
5.根据权利要求1所述的低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，所述低磁导率温度系数MnZn铁氧体材料的主要材料为Fe2O3、MnO和ZnO。
6.根据权利要求5所述的低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，所述低磁导率温度系数MnZn铁氧体材料还包含有Co2O3作为辅助成分。
7.根据权利要求5或6所述的低磁导率温度系数MnZn铁氧体材料的烧结方法，其特征在于，所述低磁导率温度系数MnZn铁氧体材料还包含有SiO2、CaCO3、SnO2、TiO2、Sb2O3、ZrO2、Nb2O5、Ta2O5、V2O5中的任意四种组合作为微量添加剂成分。
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