CN106587974B - 一种提高干压粉料成型永磁铁氧体剩磁的方法 - Google Patents

一种提高干压粉料成型永磁铁氧体剩磁的方法 Download PDF

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CN106587974B
CN106587974B CN201611205990.8A CN201611205990A CN106587974B CN 106587974 B CN106587974 B CN 106587974B CN 201611205990 A CN201611205990 A CN 201611205990A CN 106587974 B CN106587974 B CN 106587974B
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陈思维
邓兴明
胡诗言
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Hunan Aerospace Magnet and Magneto Co Ltd
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Abstract

本发明涉及一种提高干压粉料成型永磁铁氧体剩磁的方法，包括以下步骤：(1)将永磁铁氧体预烧料与质量分数为预烧料1.2％‑3.0％的磁性能增强剂混合进行湿法球磨；(2)将步骤(1)所得永磁铁氧体料浆湿法成型，在烤箱中烘干；(3)将步骤(2)所得预磁化粗粉粉碎并加入润滑剂后过100目筛；(4)将步骤(3)所得永磁铁氧体干压粉料放入表面带有细孔的粉料盒，并在型腔表面来回滑动粉料盒，使粉料在磁场作用下自由落体取向，并压制成型；(5)将步骤(4)得到的成型生坯置于电窑中烧结得永磁铁氧体磁体毛坯。本方法所制作干压成型永磁铁氧体性能较好，其剩磁可以达到湿压成型永磁铁氧体的93％以上，工艺简单，生产效率高。

Description

一种提高干压粉料成型永磁铁氧体剩磁的方法
技术领域
本发明涉及一种提高本干压粉料成型永磁铁氧体性能的方法。
背景技术
通常各向异性永磁铁氧体的成型方法是采用传统湿压成型工艺，它具有多方面的优点如：产品性能好，生坯的取向较好。但其缺点也非常明显如：由于成型过程需排除料浆内大量水分其成型设备设计与制作复杂；工序较为复杂导致成型速度较慢生产效率较低。而干压成型的过程较为简单，无需考虑水分的排除，生产效率较高，特别适合于某些体积较小、产品性能不高、需要大的产品的生产。
现有的干压粉料的制备方法主要有两种，一种是将球磨后的料浆直接烘干然后掺入粘接剂与分散剂直接打碎过100目筛，另一种是在球磨料浆烘干之前对其进行预磁化，即将湿的球磨料浆置于磁场中进行预磁化，然后再将其进行烘干后混合粘接剂与分散剂打碎，此种粉料颗粒内部的磁性晶体在预磁化时，就已经取向排列，所有粉料颗粒都是取向好的几何体，这样的集合体在外磁场作用下会整个儿转动，其易磁化方向转到外磁场方向而被压紧，因此整个坯件就成为各向异性的了。对于配方相同的干压粉料，其成型时的取向越好剩磁越高，但由于干压粉料的颗粒间存在较大的摩擦力，因此，往往干压成型的生坯取向较湿压更差，性能更低。
发明内容
本发明的目的在于，针对现有技术的不足，提供一种提高干压粉料成型永磁铁氧体剩磁的方法。
本发明的技术方案为，一种提高干压粉料成型永磁铁氧体剩磁的方法，包括如下步骤：
(1)将永磁铁氧体预烧料与质量分数为预烧料1.2％-3.0％的磁性能增强剂混合进行湿法球磨，球磨至平均粒度小于0.95μm，得永磁铁氧体料浆；
(2)将步骤(1)所得永磁铁氧体料浆置于磁场强度9500Oe-10000Oe，压力12-15MPa的条件下湿法成型，得永磁铁氧体生坯，而后将生坯破碎后置于温度为150-200℃的烤箱中烘干，得预磁化粗粉；
(3)将步骤(2)所得预磁化粗粉粉碎并加入相当于其质量分数0.8％-1.5％的粘接剂与0.2％-0.6％的润滑剂后过100目筛，得永磁铁氧体干压粉料；
(4)将步骤(3)所得永磁铁氧体干压粉料放入表面带有细孔的粉料盒，并在型腔表面来回滑动粉料盒，使粉料在磁场为12000Oe作用下自由落体取向，并压制成型；
(5)将步骤(4)得到的成型生坯置于电窑中，在温度达到1150-1210℃后烧结10-15h，得永磁铁氧体磁体毛坯。
优选地，所述永磁铁氧体预烧料为锶铁氧体预烧料。
优选地，所述粘接剂为樟脑。
优选地，所述润滑剂为硬脂酸锌。
本发明的有益效果是：
(1)本发明方法所使用干压粉料经过磁场的预磁化，磁畴方向一致，具有更好的取向度。
(2)本发明方法成型填料方法采用了一种表面带有细孔的粉料盒在型腔表面来回滑动的方法，使粉料自由落体，取向效果更好，而普通的填料方式使粉料之间间隙较小，摩擦力较大取向效果不佳。
(3)本方法所制作干压成型永磁铁氧体性能较好，其剩磁可以达到湿压成型永磁铁氧体的93％以上，同时制作工艺简单，生产效率高。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1
(1)取1kg永磁铁氧体预烧料，加入磁性能增强剂，其中碳酸钙5.5g，二氧化硅3g，硼酸3.5g，葡萄糖酸钙6g并溶于水，并湿法球磨13h，得平均粒度为0.90μm的永磁铁氧体料浆；
(2)将步骤(1)所得永磁铁氧体料浆在磁场强度10000Oe条件下，压力14.5MPa的条件下，湿法压制成长方块形，得永磁铁氧体生坯；
(3)将步骤(2)所得永磁铁氧体生坯进行粗破碎，在180℃下，烘干5h至含水量小于0.3％，得具有取向性的磁性料块；
(4)将步骤(3)所得具有取向性的磁性料块中添加粘合剂樟脑粉10g和润滑剂硬脂酸钙4g，经粉碎机分散粉碎2min后，过100目筛，得各向异性干压粉料。
将所制得干压粉料置于表面带有细孔的粉料盒中，在磁场强度12000Oe，压力12MPa的条件下，将粉料盒在型腔表面来回滑动，使粉料自由落体的方法压制成直径30mm，厚度20mm的圆饼状样品，压制时间为10s；再置于烧结电窑中，以3℃/min的速率升温至1185℃，烧结2h，得干压永磁铁氧体产品。
检测所得干压永磁铁氧体产品的磁性能，结果参见表1。
实施例2
(1)取1kg永磁铁氧体预烧料，加入磁性能增强剂，其中碳酸钙6g，二氧化硅4g，硼酸3g，葡萄糖酸钙7g，并湿法球磨14h，得平均粒度为0.85μm的永磁铁氧体料浆；
(2)将步骤(1)所得永磁铁氧体料浆在磁场强度9500Oe条件下，压力14.5MPa的条件下，湿法压制成长方块形，得永磁铁氧体生坯；
(3)将步骤(2)所得永磁铁氧体生坯进行粗破碎，在200℃下，烘干5h至含水量小于0.3％，得具有取向性的磁性料块；
(4)将步骤(3)所得具有取向性的磁性料块中添加粘合剂樟脑粉8g和润滑剂硬脂酸钙2.5g，经粉碎机分散粉碎2min后，过100目筛，得各向异性干压粉料。
将所制得的干压粉料置于一个表面带有细孔的盒子中，将盒子在型腔表面来回滑动使粉料在磁场作用下自由落体取向，压制成直径30mm，厚度20mm的圆饼状样品，压制时间为10s；再置于烧结电窑中，以3℃/min的速率升温至1190℃，烧结2h，得干压永磁铁氧体产品。
将所得干压分成形永磁铁氧体圆饼的上下表面置于磨削机上磨削抛光，后采用TYU-2000型磁性材料自动测量装置对制得的产品的磁性能进行测试，测试结果参见表1。
对比例1
采用与实施例1相同的原材料施压成型，区别仅在于：将球磨料将直接湿压成型，压制成直径30mm，厚度20mm的圆饼状样品并烧结成永磁铁氧体产品。
将本对比例所得永磁铁氧体磁体毛坯的上下两表面磨削抛光，采用TYU-2000型磁性材料自动测量装置对制得的产品的磁性能进行测试，测试结果参见表1。
对比例2
采用与实施例1大致相同的主原料和工艺，区别仅在于：不添加任何磁性能增强剂，且干粉填料成型时采用传统一次性填料方式。
将本对比例所得永磁铁氧体磁体毛坯的上下两表面磨削抛光，采用TYU-2000型磁性材料自动测量装置对制得的产品的磁性能进行测试，测试结果参见表1。
表1实施例1-2和对比例1-2所得永磁铁氧体磁体毛坯磁性能对比表
实施例1与对比例1相比，剩磁仅相差166Gs，矫顽力仅相差190Oe，内禀矫顽力仅相差187Oe。
实施例1与对比例2相比，剩磁提高了366Gs，矫顽力提高了266Oe，内禀矫顽力提高了412Oe。
实施例2比对比例2剩磁提高了321Gs，矫顽力提高了185Oe，内禀矫顽力提高了467Oe。
从实验结果对比可知，在原材料相同时，传统湿压成型方法所得永磁铁氧体磁性能最好，干压成型方法较湿压成型方法所得永磁铁氧体性能低，如实施例1、实施例2、对比例2性能都低于对比例1湿压成型方法。而实施例1试验结果则明显好于实施例2与对比例2，说明磁性能增强剂与利用粉料盒使粉料自由落体取向的成型方法可以较好的提高干压成型永磁铁氧体的磁性能。

Claims (5)

1.一种提高干压粉料成型永磁铁氧体剩磁的方法，其特征是，包括如下步骤：
(1)将永磁铁氧体预烧料与质量分数为预烧料1.2％-3.0％的磁性能增强剂混合进行湿法球磨，球磨至平均粒度小于0.95μm，得永磁铁氧体料浆；
(2)将步骤(1)所得永磁铁氧体料浆置于磁场强度9500Oe-10000Oe，压力12-15MPa的条件下湿法成型，得永磁铁氧体生坯，而后将生坯破碎后置于温度为150-200℃的烤箱中烘干，得预磁化粗粉；
(3)将步骤(2)所得预磁化粗粉粉碎并加入相当于其质量分数0.8％-1.5％的粘接剂与0.2％-0.6％的润滑剂后过100目筛，得永磁铁氧体干压粉料；
(4)将步骤(3)所得永磁铁氧体干压粉料放入表面带有细孔的粉料盒，并在型腔表面来回滑动粉料盒，使粉料在磁场作用下自由落体取向，并压制成型；
(5)将步骤(4)得到的成型生坯置于电窑中，在温度达到1150-1210℃后烧结10-15h，得永磁铁氧体磁体毛坯；
所述磁性能增强剂为二氧化硅、碳酸钙、硼酸和葡萄糖酸钙溶液的混合物。
2.根据权利要求1所述提高干压粉料成型永磁铁氧体剩磁的方法，其特征是，所述永磁铁氧体预烧料为锶铁氧体预烧料。
3.根据权利要求1所述提高干压粉料成型永磁铁氧体剩磁的方法，其特征是，所述粘接剂为樟脑。
4.根据权利要求1所述提高干压粉料成型永磁铁氧体剩磁的方法，其特征是，所述润滑剂为硬脂酸锌。
5.根据权利要求1所述提高干压粉料成型永磁铁氧体剩磁的方法，其特征是，粉料盒表面细孔直径为0.250mm。
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