CN106384639B - 一种高性能粘结钕铁硼永磁材料的制备方法 - Google Patents

一种高性能粘结钕铁硼永磁材料的制备方法 Download PDF

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CN106384639B
CN106384639B CN201610964233.2A CN201610964233A CN106384639B CN 106384639 B CN106384639 B CN 106384639B CN 201610964233 A CN201610964233 A CN 201610964233A CN 106384639 B CN106384639 B CN 106384639B
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包小倩
高学绪
卢克超
马斌
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University of Science and Technology Beijing USTB
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    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
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Abstract

一种高性能粘结钕铁硼永磁材料的制备方法，属于稀土永磁材料领域。其特征在于通过气相沉积的方法在快淬钕铁硼粉的表面包覆低熔点金属或合金薄膜(熔点范围300－600℃)，而后在该金属或合金熔点0.85－0.95倍的温度下真空热压成型，最终得到高性能粘结钕铁硼磁体。该低熔点金属或合金成份由R‑M,R‑N,R‑(M,N)或N‑N组成，熔点范围300－600℃，R为La,Ce,Pr,Nd,Gd,Tb,Dy,Ho中的一种及以上，M为Fe,Co,Ni中的一种及以上，N为Cu,Al,Ga,Zn,Sn,Ag中的一种及以上。该发明的优点是磁体强度高、磁性能高，且由于磁体导电性好，相较于传统的粘结钕铁硼磁体，更有利于磁体防腐蚀层的电泳处理。

Description

一种高性能粘结钕铁硼永磁材料的制备方法
技术领域
本发明属于稀土永磁材料领域，特别涉及一种高性能粘结钕铁硼永磁材料的制备方法。
背景技术
粘结钕铁硼磁体具有形状复杂、尺寸精度高、无需二次加工、材料利用率高、生产效率高、成本低、磁性能优良等的特点，在硬盘驱动器、光盘驱动器、办公自动化、消费电子、家用电器、汽车工业等得到广泛应用。
粘结磁体的生产方式主要有注射成型、挤出成型、模压成型等方式。粘结磁体生产的特点是需要将磁粉、粘合剂、偶联剂、润滑剂等按照一定比例混合，然后通过注射成型、挤压成型或者模压成型工艺制备磁体。其中，粘合剂一般有热塑性树脂、热固性树脂、合成橡胶以及低熔点金属或者合金等，偶联剂一般有硅烷偶联剂和钛酸酯偶联剂，润滑剂一般有石蜡、硬脂酸锌、硬脂酸锂和氮化硼等。由于大量添加这些有机物，减少磁粉的比重。比如，在专利US6143193中使用挤压成型工艺磁粉所占的体积分数为77.6-82.5％，注射成型工艺只到67.6-75.5％。因此，受到磁体致密度和非磁性相体积分数的影响，虽然粘结磁体磁性能中矫顽力基本保持了磁粉的矫顽力，但是磁体的磁能积远低于磁粉的理论值。
粘结磁体中通常使用有机聚合物作为粘结剂，最常用有PPS和Nylon。但是由于有机聚合物的低熔点特性，比如常用有机物的PPS和Nylon的熔点只有280℃左右和170℃左右，因此，使用这些有机聚合物作为粘结剂的磁体，在较高温度环境中应用时其磁性能和机械性能都将大幅度下降。
发明内容
本发明目的在于解决传统粘结磁体中通常使用有机聚合物作为粘结剂在较高温度环境中应用时其磁性能和机械性能都将大幅度下降的问题。
一种高性能粘结钕铁硼永磁材料的制备方法，其特征在于：通过气相沉积的方法在快淬钕铁硼粉的表面包覆低熔点金属或合金薄膜，而后在该金属或合金熔点0.85－0.95倍的温度下真空热压成型，该金属或合金软化并具有良好的延展性，起粘结剂的作用，最终得到高强度高磁性能的粘结钕铁硼磁体；低熔点金属或合金成份由R-M,R-N,R-(M,N)或N-N组成，熔点300－600℃，R为La,Ce,Pr,Nd,Gd,Tb,Dy,Ho中的一种及以上，M为Fe,Co,Ni中的一种及以上，N为Cu,Al,Ga,Zn,Sn,Ag中的一种及以上；
具体工艺步骤为：
1)用气相沉积的方法在快淬钕铁硼粉末颗粒表面包覆低熔点R-M,R-N,R-(M,N)和N-N薄层；
2)对经过表面包覆的快淬钕铁硼粉真空热压成型，得到高强度高磁性能粘结钕铁硼磁体。
工艺步骤1)中气相沉积采用磁控溅射或真空蒸镀的方法；
工艺步骤1)中快淬钕铁硼粉的颗粒尺寸为50－200μm；
工艺步骤1)中，在气相沉积过程中，使钕铁硼粉末颗粒处于悬浮运动状态，从而保证R-M,R-N,R-(M,N)或N-N合金均匀包覆在快淬钕铁硼粉末颗粒的表面，包覆层的厚度为50－500nm；
工艺步骤2)中压力为50-500MPa，保压时间5－30min，真空度10-2－10-4Pa。
粘结钕铁硼永磁材料中粘结剂主要起粘结成型的作用，传统的粘结剂通常是有机粘结剂，如环氧树脂等，但这种磁体在温度升高时磁性能特别是机械性能明显下降。本发明选择熔点为300－600℃的低熔点、非磁性的金属或合金作为粘结剂，并且通过气相沉积的方法将低熔点金属或合金均匀包覆在快淬钕铁硼粉的表面(为了实现均匀包覆，通过振动或旋转等方式使钕铁硼粉悬浮运动，通过控制气相沉积工艺参数控制包覆层的厚度)，随后将经过低熔点金属或合金包覆处理的快淬钕铁硼粉末装入模具内，经过真空热压成型，得到高强度高磁性能的粘结磁体。热压温度维持在包覆金属或合金熔点的0.85－0.95倍，此温度下金属或合金发生软化但不熔化，软化的金属或合金具有良好的延展性，同时在压力的作用下，金属或合金包覆体将钕铁硼粉紧密地联接在一起，即起粘结剂的作用。快淬钕铁硼粉在600－700℃以上的温度容易发生晶粒长大，从而影响钕铁硼粉本身的性能，因此金属或合金的熔点选择300－600℃，且真空热压时的温度只有它们的0.85－0.95倍，此温度下热压保温的时间也只有短短的5－30min，因此钕铁硼粉本身的组织结构和磁性能均不会发生明显的变化。传统粘结钕铁硼磁体中粘结剂(非磁性相)的含量较高，约占30％左右的体积分数，而本发明中起粘结作用的低熔点金属或合金的占比大幅下降。
本发明的优点是：
1)磁体致密度和强度高；
2)非磁性相少，磁性能高；
3)粘结剂是导电性好的合金，有利于粘结磁体表面防腐蚀层的电泳处理。
具体实施方式
实施例1：
1)选用颗粒尺寸为75－125μm的商用快淬钕铁硼磁粉；
2)熔炼Ce80Co20(质量分数)合金靶材；
3)用磁控溅射的方法在钕铁硼粉表面沉积Ce80Co20合金薄层，先抽真空至(3-5)×10-3Pa后通入0.1Pa氩气作为保护气体，维持单位靶面积的溅射功率为10w/cm2，溅射时间为2h,沉积层厚度为180nm；
4)经过表面包覆的钕铁硼粉放入模具中，经过真空热压成型，真空度达到2×10- 3Pa以上后氩气保护，热压温度为490℃，压力大小为100MPa，保压时间8min,最终获得具有高磁性能和高机械强度的粘结磁体。
实施例2：
1)选用颗粒尺寸为75－125μm的商用快淬钕铁硼磁粉；
2)熔炼Nd65Dy25Al10(质量分数)合金靶材；
3)用磁控溅射的方法在钕铁硼粉表面沉积Nd65Dy25Al10合金薄层，先抽真空至(3-5)×10-3Pa后通入0.1Pa氩气作为保护气体，维持单位靶面积的溅射功率为8w/cm2，时间为2h,沉积层厚度为150nm；
4)经过表面包覆的钕铁硼粉放入模具中，经过真空热压成型，真空度达到2×10- 2Pa以上后氩气保护，热压温度为580℃，压力大小为100MPa，保压时间10min,最终获得具有高磁性能和高机械强度的粘结磁体。
实施例3：
1)选用颗粒尺寸为75－125μm的商用快淬钕铁硼磁粉；
2)熔炼Pr83Co2Cu15(质量分数)合金靶材；
3)用磁控溅射的方法在钕铁硼粉表面沉积Pr83Co2Cu15合金薄层，先抽真空至(3-5)×10-3Pa后通入氩气作为保护气体，维持单位靶面积的溅射功率为6w/cm2，时间为2h,沉积层厚度为100nm；
4)经过表面包覆的钕铁硼粉放入模具中，经过真空热压成型，真空度达到2×10- 2Pa以上后氩气保护，热压温度为430℃，压力大小为100MPa，保压时间15min,最终获得具有高磁性能和高机械强度的粘结磁体。
实施例4：
1)选用颗粒尺寸为75－125μm的商用快淬钕铁硼磁粉；
2)熔炼Cu34Al66(质量分数)合金作为蒸发源；
3)用真空蒸镀的方法在钕铁硼粉表面沉积Cu34Al66合金薄层，先抽真空至4×10- 3Pa以上，电流/电压为75A/0.6V，蒸镀时间30min，得到厚度约75nm的包覆层，蒸镀时维持钕铁硼粉的悬浮运动，保证包覆均匀；
4)经过表面包覆的钕铁硼粉放入模具中，经过真空热压成型，真空度达到2×10- 2Pa以上后氩气保护，热压温度为520℃，压力大小为100MPa，保压时间15min,最终获得具有高磁性能和高机械强度的粘结磁体。

Claims (1)

1.一种高性能粘结钕铁硼永磁材料的制备方法，其特征在于通过气相沉积的方法在快淬钕铁硼粉的表面包覆低熔点金属或合金薄膜，而后在该金属或合金熔点0.85－0.95倍的温度下真空热压成型，该金属或合金软化并具有良好的延展性，起粘结剂的作用，最终得到高强度高磁性能的粘结钕铁硼磁体；低熔点金属或合金成份由R‐M,R‐N,R‐(M,N)或N‐N组成，熔点300－600℃，R为La,Ce,Pr,Nd,Gd,Tb,Dy,Ho中的一种及以上，M为Fe,Co,Ni中的一种及以上，N为Cu,Al,Ga,Zn,Sn,Ag中的一种及以上；
具体工艺步骤为：
1)用气相沉积的方法在快淬钕铁硼粉末颗粒表面包覆低熔点R‐M,R‐N,R‐(M,N)或N‐N薄层；
2)对经过表面包覆的快淬钕铁硼粉真空热压成型，得到高强度高磁性能粘结钕铁硼磁体；
工艺步骤1)中，在气相沉积过程中，使钕铁硼粉末颗粒处于悬浮运动状态，从而保证R‐M,R‐N,R‐(M,N)或N‐N合金均匀包覆在快淬钕铁硼粉末颗粒的表面，钕铁硼粉的颗粒尺寸为50－200μm，低熔点金属或合金沉积层厚度为50－500nm；
工艺步骤2)中，压力为50－500MPa，保压时间5－30min，真空度10‐2－10‐4Pa。
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