CN106252009A - 一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体及其制备方法 - Google Patents

一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体及其制备方法 Download PDF

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CN106252009A
CN106252009A CN201610600395.8A CN201610600395A CN106252009A CN 106252009 A CN106252009 A CN 106252009A CN 201610600395 A CN201610600395 A CN 201610600395A CN 106252009 A CN106252009 A CN 106252009A
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permanent magnet
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严密
金佳莹
张玉晶
彭白星
刘永胜
马天宇
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Zhejiang University ZJU
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Abstract

本发明公开一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体及其制备方法。本发明使用多合金工艺，其中主合金的成分设计富La/Ce/Y，能显著降低稀土永磁体的原材料成本；辅合金为稀土氢化物，在烧结和热处理的过程中形成包围主相边界的硬磁壳层，提高稀土永磁体的综合磁性能。本发明提供了一种高效利用高丰度稀土La/Ce/Y的途径，大幅降低磁体成本的同时保障其综合磁性能。

Description

一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体及 其制备方法
技术领域
本发明涉及稀土永磁材料领域，具体来说，涉及了一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体及其制备方法。
背景技术
第三代稀土永磁材料钕铁硼具有其他永磁体无法比拟的高的磁能积，因而被誉为“永磁之王”，是现代社会军民各领域不可或缺的战略性功能材料。1996～2008年间全球烧结钕铁硼的产量从6000吨增至63000吨，保持了近10％的年平均增长率(YangLuo.Proc.20th Int.Workshop on Rare Earth Permanent Magnets and TheirApplications.2008，27)。以2010年为例，钕铁硼在世界永磁体的市场占有率达到62％(该统计数据由US Magnetic Materials Association提供)。伴随着钕铁硼对Nd/Pr等稀土原材料的需求量持续增长，而其供应日趋紧张，稀土价格持续波动，全球稀土产业开始面临严峻的成本控制难题。因而，使用高丰度稀土元素La/Ce/Y部分取代当前供应紧张的Nd/Pr，制备商用RE-Fe-B永磁材料，成为了一项迫在眉睫的重要任务。
La/Ce/Y的2:14:1相的内禀磁性能远弱于Nd2Fe14B四方相，因而La/Ce/Y的取代往往伴随强烈的磁稀释效应，造成磁性能的大幅衰退。尤其是富La/Ce/Y永磁体的矫顽力，往往无法达到商用磁体的性能要求，因此，如何提高矫顽力成为了富La/Ce/Y永磁体产业化的主要瓶颈。目前，国内外普遍通过重稀土添加提高磁体内禀磁晶各向异性场HA的方式，来提高烧结钕铁硼磁体的矫顽力。重稀土的添加主要包括以下两种途径：一是熔炼添加，即在熔炼过程中直接添加Dy或Tb金属，但是会引起磁稀释效应，导致剩磁大幅降低；二是晶界扩散，即通过溅射、气相沉积、表面涂覆等方法在磁体表面包覆重稀土化合物，在烧结或热处理过程中使重稀土元素扩散到晶粒表面，形成磁硬壳层，重稀土元素不会过多进入主相晶粒内引起磁稀释，但是这种方法因扩散深度的限制仅适用于小块磁体，不适用于大批量生产。因此寻找一种能提高磁体矫顽力同时保持高剩磁和磁能积，并且控制生产成本，不大量消耗稀缺重稀土Dy、Tb，是当前高性能富La/Ce/Y稀土永磁体开发的重要目标。
发明内容
本发明的目的是克服现有技术的不足，提供一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体及其制备方法。
本发明使用多合金工艺，其中主合金的成分设计富La/Ce/Y，能显著降低稀土永磁体的原材料成本；辅合金为稀土氢化物，有效提升提高Pr、Nd、Ho、Gd、Tb、Dy(较La/Ce/Y的四方相化合物具有更高的HA)稀土元素的使用效率，在烧结和热处理的过程中形成包围主相边界的硬磁壳层，能大幅提高磁体的矫顽力同时保持其剩磁，因而提高富La/Ce/Y稀土永磁体的综合磁性能。本发明提供了一种高效利用高丰度稀土La/Ce/Y的途径，大幅降低磁体成本的同时保障其综合磁性能。
本发明提供了一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体的制备方法，其具体步骤如下：
1)采用SC(strip casting:速凝鳞片铸锭)、HD(hydrogen decrepitation:氢爆)、JM(jet milling:气流磨)工艺制备主合金粉末；
2)RE”100-y-zM'y合金真空中频感应熔炼后吸氢制备得到RE”100-y-zM'yHz稀土氢化物，破碎后制备得到辅合金粉末；
3)主合金粉末和辅合金粉末混合均匀后进行磁场取向压型得到生坯，其中，辅合金粉末占总粉末质量的0.1～10％；
4)将得到的生坯进行真空封装后冷等静压处理；
5)将步骤4)得到的生坯放入高真空正压烧结炉，烧结制成磁体；
6)800～980℃间进行一级回火，420～620℃间进行二级回火得到高性能富La/Ce/Y稀土永磁体。
优选的，所述步骤2)破碎后使用机械球磨或者气流磨来制备得到辅合金粉末。
优选的，所述步骤5)的烧结温度为1000～1100℃，烧结时间为2～5h。
优选的，所述步骤4)冷等静压使用的压力为150～200MPa，冷等静压处理时间为1～3min。
高性能富La/Ce/Y稀土永磁体包括主合金和辅合金，所述的主合金以原子百分数计，其成分为[(NdaRE1-a)1-xRE'x]hFe100-h-i-jMiBj，Nd为钕元素，RE为除去Nd、La、Ce、Y以外的其他镧系元素或者Sc中的一种或者几种，RE'为La、Ce、Y元素中的一种或者几种，Fe为铁元素，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、Zr元素中的一种或几种，B为硼元素；a、x、h、i和j分别满足以下关系：0.2≤a≤1、0<x≤0.8、12≤h≤20、0≤i≤2、5.5≤j≤6.5；所述的辅合金以原子百分数计，其成分为RE”100-y-zM'yHz，RE”为Pr、Nd、Ho、Gd、Tb、Dy中的一种或几种，M'为Al、B、Bi、Ca、Co、Cr、Cu、Fe、Ga、In、Mg、Mn、Mo、Nb、Ni、Pb、Si、Sn、Ta、Ti、V、W、Zn、Zr等元素中的一种或几种，H为氢元素；y和z分别满足以下关系：0≤y<100，0<z≤75，0<y+z<100。优选的，所述的辅合金占永磁体质量的0.1～10％。
本发明与现有技术相比具有的有益效果：1)主合金利用高丰度稀土La/Ce/Y部分取代Nd，降低成本的同时促进稀土元素的产销平衡；辅合金的成分设计选用Pr、Nd、Ho、Gd、Tb、Dy中的一种或几种来形成包围主相边界的硬磁壳层，仅包含少量或者不使用高价格重稀土元素Tb、Dy，进一步降低了生产成本，同时有助于保护珍贵的重稀土资源；因此，本发明提供的磁体能有效实现成本控制。2)辅合金为各类稀土氢化物，易于制备，在烧结和热处理的过程中分解成高活性的稀土合金，更容易形成均匀完整的硬磁壳层，同时配合优化的烧结和热处理工艺，能有效保障富La/Ce/Y稀土永磁体的综合磁性能。
具体实施方式
下面结合具体实施例对本发明做进一步说明，但本发明并不仅仅局限于以下实施例：
实施例1：
1)SC(strip casting:速凝鳞片铸锭)、HD(hydrogen decrepitation:氢爆)、JM(jet milling:气流磨)工艺的配合来制备主合金粉末，所述的主合金以原子百分数计，其成分为(Nd0.9Ce0.2)12Fe82B6；
2)Nd0.5Dy0.5真空中频感应熔炼后吸氢制备得到Nd0.5Dy0.5H3稀土氢化物，粗破碎后配合使用机械球磨来制备辅合金粉末；
3)主合金粉末和辅合金粉末混合均匀后进行磁场取向压型，其中，稀土氢化物辅合金粉末占总粉末质量的1％；
4)将得到的生坯进行真空封装后150MPa冷等静压1min；
5)将生坯放入高真空正压烧结炉，在1050℃烧结3h制成磁体；
6)890℃进行一级回火，500℃进行二级回火。
7)将制备好的磁体放入VSM中测量其磁性能，结果如下:Br＝1.38T,Hcj＝1376kA/m,(BH)max＝344kJ/m3。
实施例2：
1)SC(strip casting:速凝鳞片铸锭)、HD(hydrogen decrepitation:氢爆)、JM(jet milling:气流磨)工艺的配合来制备主合金粉末，所述的主合金以原子百分数计，其成分为(Nd0.6La0.1Ce0.3)15Fe77.7Ga0.2Al0.5Cu0.1B6.5；
2)Nd0.8Pr0.2真空中频感应熔炼后吸氢制备得到Nd0.8Pr0.2H2稀土氢化物，粗破碎后配合使用机械球磨来制备辅合金粉末；
3)主合金粉末和辅合金粉末混合均匀后进行磁场取向压型，其中，稀土氢化物辅合金粉末占总粉末质量的3％；
4)将得到的生坯进行真空封装后200MPa冷等静压2min；
5)将生坯放入高真空正压烧结炉，在1040℃烧结3h制成磁体；
6)890℃进行一级回火，480℃进行二级回火。
7)将制备好的磁体放入VSM中测量其磁性能，结果如下:Br＝1.26T,Hcj＝1138kA/m,(BH)max＝302kJ/m3。
实施例3：
1)SC(strip casting:速凝鳞片铸锭)、HD(hydrogen decrepitation:氢爆)、JM(jet milling:气流磨)工艺的配合来制备主合金粉末，所述的主合金以原子百分数计，其成分为(Nd0.9Y0.1)20Fe73.2Ga0.2Cu0.1B6.5；
2)Nd0.8Ho0.2真空中频感应熔炼后吸氢制备得到Nd0.8Ho0.2H2稀土氢化物，粗破碎后配合使用机械球磨来制备辅合金粉末；
3)主合金粉末和辅合金粉末混合均匀后进行磁场取向压型，其中，稀土氢化物辅合金粉末占总粉末质量的0.2％；
4)将得到的生坯进行真空封装后200MPa冷等静压3min；
5)将生坯放入高真空正压烧结炉，在1080℃烧结2.5h制成磁体；
6)900℃进行一级回火，500℃进行二级回火。
7)将制备好的磁体放入VSM中测量其磁性能，结果如下:Br＝1.28T,Hcj＝1206kA/m,(BH)max＝298kJ/m3。

Claims (6)

1.一种基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体，其特征在于包括主合金和辅合金，主合金以原子百分数计，其成分为[(NdaRE1-a)1-xRE'x]hFe100-h-i-jMiBj，Nd为钕元素，RE为除去Nd、La、Ce、Y以外的其他镧系元素或者Sc中的一种或者几种，RE'为La、Ce、Y元素中的一种或者几种，Fe为铁元素，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、Zr元素中的一种或几种，B为硼元素；a、x、h、i和j分别满足以下关系：0.2≤a≤1、0<x≤0.8、12≤h≤20、0≤i≤2、5.5≤j≤6.5；辅合金以原子百分数计，其成分为RE”100-y-zM'yHz，RE”为Pr、Nd、Ho、Gd、Tb、Dy中的一种或几种，M'为Al、B、Bi、Ca、Co、Cr、Cu、Fe、Ga、In、Mg、Mn、Mo、Nb、Ni、Pb、Si、Sn、Ta、Ti、V、W、Zn、Zr等元素中的一种或几种，H为氢元素；y和z分别满足以下关系：0≤y<100，0<z≤75，0<y+z<100。
2.根据权利要求1所述的基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体，其特征在于所述的辅合金占永磁体质量的0.1～10％。
3.一种权利要求1所述基于稀土氢化物添加的高性能富La/Ce/Y稀土永磁体的制备方法，其特征在于它的步骤如下：
1)采用SC、HD、JM工艺制备主合金粉末；
2)RE”100-y-zM'y合金真空中频感应熔炼后吸氢制备得到RE”100-y-zM'yHz稀土氢化物，破碎后制备得到辅合金粉末；
3)主合金粉末和辅合金粉末混合均匀后进行磁场取向压型得到生坯，其中，辅合金粉末占总粉末质量的0.1～10％；
4)将得到的生坯进行真空封装后冷等静压处理；
5)将步骤4)得到的生坯放入高真空正压烧结炉，烧结制成磁体；
6)800～980℃间进行一级回火，420～620℃间进行二级回火得到高性能富La/Ce/Y稀土永磁体。
4.根据权利要求3所述的方法，其特征在于所述步骤2)破碎后使用机械球磨或者气流磨来制备得到辅合金粉末。
5.根据权利要求3所述的方法，其特征在于所述步骤5)的烧结温度为1000～1100℃，烧结时间为2～5h。
6.根据权利要求3所述的方法，其特征在于所述步骤4)冷等静压使用的压力为150～200MPa，冷等静压处理时间为1～3min。
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