CN111470858B - 一种耐高压的永磁铁氧体磁体及其制造方法 - Google Patents

一种耐高压的永磁铁氧体磁体及其制造方法 Download PDF

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CN111470858B
CN111470858B CN202010306253.7A CN202010306253A CN111470858B CN 111470858 B CN111470858 B CN 111470858B CN 202010306253 A CN202010306253 A CN 202010306253A CN 111470858 B CN111470858 B CN 111470858B
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sintering aid
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刘辉
张鹏杰
李炳山
魏汉中
李亚峰
孙威
全小康
谢光环
王倩
贾丽颖
王峰
刘冬
胡国辉
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Beikuang Magnets Fuyang Co ltd
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Abstract

本发明提供一种耐高压的永磁铁氧体磁体及其制造方法，分子式为SrFe2nO19，其中n＝(5.8‑6.2)，按配比称取铁红、碳酸锶和添加剂，混合均匀后进行预烧，获得预烧料磁粉；按照预烧料磁粉重量称取定量的烧结助剂，烧结助剂中不含Si的氧化物，且没有含Si的化合物。在微粉碎阶段不添加SiO2，在晶界相中不存在Si的单质形态，因而烧结磁体的电导率显著下降，磁体的耐压性能显著提高，能够满足电机对产品的耐压参数要求。同时通过优化烧结助剂的组成和添加量，磁体性显著提升。为了提高矫顽力，烧结助剂添加了碳酸钙、硼酸、氧化镧和氧化钴。

Description

一种耐高压的永磁铁氧体磁体及其制造方法
技术领域
本发明涉及永磁材料技术领域，具体为一种耐高压的永磁铁氧体磁体及其制造方法。
背景技术
铁氧体烧结磁体在各种电动机、发电机、扬声器等各种用途中被使用。作为代表性的铁氧体烧结磁体，已知有具有六方晶的M型磁铁铅矿结构的Sr铁氧体(SrFe12O19)和Ba铁氧体(BaFe12O19)。这些铁氧体烧结磁体，以氧化铁和锶(Sr)或钡(Ba)的碳酸盐等为原料，通过粉末冶金法比较廉价地制造。
近年来，出于对环境的保护等，在汽车用电装部件、电器设备用零件等之中，以零件的小型化、轻量化以及高效率化为目的，要求铁氧体烧结磁体的高性能化。特别是用于汽车用电装部件的电动机，其所要求的铁氧体烧结磁体，一面要保持高残留磁通密度Br(一般要求Br≥410mT，即4100Gs)，一面要具有即使在薄型化时的强大的反磁场作用下也不会去磁的高矫顽力HcJ(一般要求HcJ≥286kA/m，即3600Oe)。
与此同时，出于以人为本的制造理念的普及，对电气设备安全性的要求越来越高。特别是为了防止电机在使用过程中发生漏电等不安全因素，对电动机中的烧结磁体的耐电压参数提出了明确要求(一般要求耐压值≥10kV)。这对于铁氧体烧结磁体而言，是一个新的课题，即要求铁氧体烧结磁体保持较高的磁体性能，同时具备一定的耐电压性能。
目工业上铁氧体烧结磁体由以下的制造工序制造。首先，将氧化铁和Sr或Ba的碳酸盐等进行混合，通过预烧进行铁氧体化反应，得到预烧料。将预烧料进行粗粉碎，将粗粉碎得到的粉末按规定量投入球磨机，同时添加添加SiO2、CaCO3等助剂，以水为介质进行湿式微粉碎，粉碎至平均粒径0.7μm左右。得到的料浆在磁场中成形，干燥后进行烧结。经过磨加工和清洗工序得到铁氧体烧结磁体。
众所周知，一般的铁氧体烧结磁体的烧结工艺被归类为液相烧结。为了促进液相烧结，获得最佳的晶相组织，现有技术人员一般都着眼于烧结助剂的研究。作为烧结助剂已知有CaCO3和SiO2等，会在烧结前的粉碎工序添加。烧结助剂在烧结(焙烧)时成为液相成分的一部分，在烧结后的烧结体中作为晶界相的一种成分存在。
在现有技术条件下，烧结助剂中添加的SiO2后，其中不可避免出现部分Si以单质形态存在。由于Si是半导体材料，室温时电导率约在1mΩ·cm～1GΩ·cm之间。SiO2的添加量越多，单质形态的Si也就越多，导致磁体的导电率越高。也就是磁体越不耐压。
因此现有技术制造的磁体无法同时满足市场对耐压性能和优异磁性能的需求。
发明内容
本发明所解决的技术问题在于提供一种耐高压的永磁铁氧体磁体及其制造方法，以解决上述背景技术中提出的问题。
本发明所解决的技术问题采用以下技术方案来实现：一种耐高压的永磁铁氧体磁体及其制造方法，分子式为SrFe2nO19，其中n＝(5.8-6.2)，包括如下步骤：
步骤一：按配比称取铁红、碳酸锶和添加剂，混合均匀后进行预烧，获得预烧料磁粉；
步骤二：按照预烧料磁粉重量称取定量的烧结助剂，烧结助剂中不含Si的氧化物，且没有含Si的化合物，同时添加0.2～0.6wt％的碳酸钙，添加0.1～0.4wt％的硼酸，添加1.0～3.0wt％的氧化镧，添加0.5～1.5wt％的氧化钴；
步骤三：将预烧料磁粉连同烧结助剂一起投入球磨机中，以水为介质进行微粉碎，粒度控制在0.7μm；
步骤四：将微粉碎后的料浆置于磁场中成型，施加磁场，压制成型，磁粉全部沿着易磁化方向排列，得到压坯；
步骤五：将成型后的压坯置于窑炉中进行烧结，升温速率为6℃/min，烧结温度为1180℃-1280℃，保温2小时，随炉自然冷却至室温，随后对烧结磁体的上下表面进行磨加工，得到烧结磁体。
作为本发明的优选方案为：所述步骤四中的磁场强度为8000-10000Oe，成型压力为7-9MPa。
作为本发明的优选方案为：所述步骤五中烧结温度控制在1180-1250℃之间。
与现有技术相比，本发明的有益效果是：在微粉碎阶段不添加SiO2，减少了晶界相中单质形态的Si，因而烧结磁体的电导率显著下降，磁体的耐压性能显著提高，能够满足电机对产品的耐压参数要求。同时通过优化烧结助剂的组成和添加量，磁体性显著提升。为了提高矫顽力，添加了碳酸钙、硼酸、氧化镧和氧化钴。
附图说明
图1为本发明的耐压性能测量图一；
图2为本发明的耐压性能测量图二。
具体实施方式
为了使本发明的实现技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体图示，进一步阐述本发明。
如图1～2所示，
实施例1
步骤一：按照分子式SrFe2nO19，称取铁红、碳酸锶和添加剂，混合均匀后进行预烧，获得预烧料磁粉。
步骤二：按照预烧料磁粉重量称取定量的烧结助剂，烧结助剂中不含Si的氧化物、碳酸盐等含Si的化合物，同时添加0.2～0.6wt％的碳酸钙，添加0.1～0.4wt％的硼酸，添加1.0～3.0wt％的氧化镧，添加0.5～1.5wt％的氧化钴。
步骤三：将预烧料磁粉连同烧结助剂一起投入球磨机中，以水为介质进行微粉碎，粒度控制在0.7μm；
步骤四：将微粉碎后的料浆置于磁场中成型，施加磁场，压制成型，磁粉全部沿着易磁化方向排列,磁场强度为8000-10000Oe，成型压力为7-9MPa，得到成型体；
步骤五：将成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1180℃-1280℃，保温2小时，随炉自然冷却至室温，随后对烧结磁体的上下表面进行磨加工，获得干压异性烧结铁氧体。烧结温度过低，导致磁体密度过低，无法获得优异的剩磁，烧结温度过高，易产生晶粒的异常生长，导致矫顽力降低。因此烧结温度最好控制在1180-1250℃。
实施例2
按照分子式SrFe2nO19，分别按n＝5.8、5.9、6.0、6.1、6.2，称取铁红和碳酸锶，混合均匀后在1300度预烧，获得预烧料磁粉。将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。将二氧化硅作为烧结助剂进行试验，其中二氧化硅的添加量分别为0、0.05、0.10、0.2、0.3wt％，微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的耐压性能进行测量(实施例采用的耐压测试仪的最大测量值为13kV)。具体性能见图1。
实施例3
按照分子式SrFe2nO19，分别按n＝5.8、5.9、6.0、6.1、6.2，称取铁红和碳酸锶，同时添加总质量0.2wt％的SiO2，混合均匀后在1300度预烧，获得预烧料磁粉。同时将二氧化硅作为烧结助剂进行试验，将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。其中二氧化硅的添加量分别为0、0.05、0.10、0.2、0.3wt％，微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的耐压性能进行测量。具体性能见图2。
实施例4
按照分子式SrFe2nO19，分别按n＝6.1，称取铁红和碳酸锶，混合均匀后分别在1280、1300、1320、1340度预烧，获得预烧料磁粉。将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。同时将二氧化硅作为烧结助剂进行试验，其中二氧化硅的添加量分别为0、0.05、0.10、0.2、0.3wt％，微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的耐压性能进行测量。具体性能见表1。
表1
Figure GDA0003406871380000051
实施例5
按照分子式SrFe2nO19，分别按n＝6.1，称取铁红和碳酸锶，同时添加总质量0.2wt％的SiO2(在预烧前添加SiO2，称为“前添加”)，混合均匀后分别在1280、1300、1320、1340度预烧，获得预烧料磁粉。同时将二氧化硅作为烧结助剂进行试验，将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。其中二氧化硅的添加量分别为0、0.05、0.10、0.2、0.3wt％(在预烧后的微粉碎阶段添加SiO2，称为“后添加”)，微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的耐压性能进行测量。具体性能见表2。
表2
Figure GDA0003406871380000052
Figure GDA0003406871380000061
综上所述，从实施例2至实施例5可以看出，不论是否在预烧前添加SiO2，只要在微粉碎阶段添加SiO2，产品的耐压性能就显著下降。由此可见在微粉碎阶段是否添加SiO2是决定产品耐压性能的决定性因素。即在微粉碎阶段不添加SiO2，产品的耐压性能有质的提高。
实施例6
按照分子式SrFe2nO19，分别按n＝6.1，称取铁红和碳酸锶，同时添加总质量0.2wt％的SiO2，混合均匀后分别在1300度预烧，获得预烧料磁粉。将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。其中二氧化硅的添加量为0wt％，碳酸钙的添加量为0.2、0.4、0.6、0.8、1.0wt％，硼酸的添加量为0.4wt％的，氧化镧的添加量为2.0wt％、氧化钴的添加量为1.0wt％。微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的磁性能和耐压性能进行测量。具体性能见表3。
表3
Figure GDA0003406871380000062
Figure GDA0003406871380000071
实施例7
按照分子式SrFe2nO19，分别按n＝6.1，称取铁红和碳酸锶，同时添加总质量0.2wt％的SiO2，混合均匀后分别在1300度预烧，获得预烧料磁粉。将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。其中二氧化硅的添加量为0wt％，碳酸钙的添加量为0.2wt％，硼酸的添加量为0、0.1、0.2、0.3、0.4wt％，氧化镧的添加量为2.0wt％、氧化钴的添加量为1.0wt％。微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的磁性能和耐压性能进行测量。具体性能见表4。
表4
Figure GDA0003406871380000072
实施例8
按照分子式SrFe2nO19，分别按n＝6.1，称取铁红和碳酸锶，同时添加总质量0.2wt％的SiO2，混合均匀后分别在1300度预烧，获得预烧料磁粉。将预烧料磁粉和烧结助剂投入球磨机进行微粉碎。其中二氧化硅的添加量为0wt％，碳酸钙的添加量为0.2wt％，硼酸的添加量为0.4wt％，氧化镧的添加量分别为1.0、1.5、2.0、2.5wt％，氧化钴的添加量分别为0.5、0.75、1.0、1.25wt％。微粉碎至平均粒径0.7μm，得到的料浆在磁场中成形，成型磁场强度为10000Oe，成型压力为7MPa，获得的成型体是直径为33mm，高度为12mm的圆柱体。将干燥后的成型体置于烧结炉中烧结，升温速率为6℃/min，烧结温度为1220℃，保温2小时，随炉自然冷却至室温，获得烧结磁体。经过磨加工和清洗工序得到铁氧体烧结磁体。对烧结磁体的上下表面进行磨加工，对该磁体的磁性能和耐压性能进行测量。具体性能见表5。
表5
Figure GDA0003406871380000081
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明的要求保护范围由所附的权利要求书及其等效物界定。

Claims (3)

1.一种耐高压的永磁铁氧体磁体的制造方法，其特征在于：分子式为SrFe2nO19，其中n=6.1、6.2，包括如下步骤：
步骤一：按配比称取铁红、碳酸锶和添加剂，混合均匀后进行预烧，获得预烧料磁粉；
步骤二：按照预烧料磁粉重量称取定量的烧结助剂，烧结助剂中不含Si的氧化物，且没有含Si的化合物；烧结助剂为碳酸钙、硼酸、氧化镧和氧化钴，烧结助剂中占总质量的质量份数范围为：碳酸钙0.2～0.6wt％、硼酸0.1～0.4wt％、氧化镧1.0～3.0wt％和氧化钴0.5～1.5wt％；
步骤三：将预烧料磁粉连同烧结助剂一起投入球磨机中，以水为介质进行微粉碎，粒度控制在0.7μm；
步骤四：将微粉碎后的料浆置于磁场中成型，施加磁场，压制成型，磁粉全部沿着易磁化方向排列，得到压坯；
步骤五：将成型后的压坯置于窑炉中进行烧结，升温速率为6℃/min，烧结温度为1180℃-1280℃，保温2小时，随炉自然冷却至室温，随后对烧结磁体的上下表面进行磨加工，得到烧结磁体。
2.根据权利要求1所述的一种耐高压的永磁铁氧体磁体的制造方法，其特征在于：所述步骤四中的磁场强度为8000-10000Oe，成型压力为7-9MPa。
3.根据权利要求1所述的一种耐高压的永磁铁氧体磁体的制造方法，其特征在于：所述步骤五中烧结温度控制在1180-1250℃之间。
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