CN105931781B - 一种烧结钕铁硼回收废料的再生利用方法 - Google Patents

一种烧结钕铁硼回收废料的再生利用方法 Download PDF

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CN105931781B
CN105931781B CN201610455267.9A CN201610455267A CN105931781B CN 105931781 B CN105931781 B CN 105931781B CN 201610455267 A CN201610455267 A CN 201610455267A CN 105931781 B CN105931781 B CN 105931781B
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喻玺
杜君峰
戚植奇
喻春晖
孙爱芝
许琛
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GANZHOU FORTUNE ELECTRONIC Ltd
University of Science and Technology Beijing USTB
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
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    • 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
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
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    • B22F9/00—Making metallic powder or suspensions thereof
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    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • 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
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • 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
    • H01F1/0575—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 pressed, sintered or bonded together
    • H01F1/0576—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 pressed, sintered or bonded together pressed, e.g. hot working
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

Abstract

本发明涉及一种烧结钕铁硼回收废料的再生利用方法，属于稀土永磁材料技术领域。将清洗干净的机加工切割的边角料、电镀不合格产品等NdFeB回收废料，进行机械破碎，过筛，得到大颗粒磁粉（筛网的尺寸介于60‑300目），在大气环境下，取向成型，制成毛坯，毛坯的密度可达到6.0g/cm3，随后对毛坯进行真空热处理，得到高性能的NdFeB永磁体。本发明中原料磁粉为破碎NdFeB回收废料得到的约百微米级的磁粉，磁粉的储存、磁体的取向成型过程及成型后毛坯的储存可以在大气环境中进行，简化了生产工艺，提升了生产效率。

Description

一种烧结钕铁硼回收废料的再生利用方法
技术领域
本发明涉及一种烧结钕铁硼回收废料的再生利用方法，属于稀土永磁材料技术领域。
背景技术
在烧结钕铁硼生产的各个环节中，特别是机加工过程会产生大量的废料，其比例超过原料重量的20%。目前，关于废料的回收方法主要有两大类：一是利用萃取法、复盐沉淀法得到稀土氯化物、氧化物，再经湿法冶金提纯得到稀土金属；二是进行适当的处理(如清洗、去皮等)后，返回到熔炼炉重熔或者送到制粉工序再利用，得到烧结NdFeB磁体。但上述方法还存在不足：方法一的不足在于：处理方法工艺较复杂，投入大、成本高；使用化学方法提纯会产生含有大量酸根和氯根的废水、废液等，产生了新的“三废”排放问题，造成环境的污染。方法二的不足在于：该过程均涉及到微米磁粉（一般为3-5μm）的制备和取向成型过程，两者均需要在N2保护下进行，生产过程较复杂。
因此，本发明利用机加工边角料和电镀产生的烧结NdFeB磁体回收废料，直接进行机械破碎，得到大颗粒磁粉（如过80目筛，磁粉粒径≤200μm），在大气环境下，无需保护气氛，取向成型，最后经热处理，制备高性能的钕铁硼磁体。
本发明开发了一种无污染的、成型工艺简便，能够制备高性能永磁体的烧结NdFeB废料的再生利用技术。
发明内容
本发明的目的在于针对现有烧结钕铁硼机加工边角料和电镀废料的再利用，提供一种工艺简单，操作简便的制备高性能钕铁硼磁体的方法。
本发明的核心在于：在烧结NdFeB磁体生产过程中，制备微米磁粉（3-5μm）的目的是利用其为单晶粉末颗粒，经磁场取向成型后，具有良好的晶体织构，有利于制备高性能的各向异性的烧结NdFeB磁体。而烧结NdFeB废料破碎后的磁粉继承了烧结磁体优异的织构特性，以此为原料经取向成型制备的毛坯，也能具有良好的织构。但是，烧结NdFeB破碎后，材料的矫顽力、退磁曲线方形度和磁能积会急剧恶化。本发明将上述烧结NdFeB废料破碎后的磁粉在室温取向成型，通过控制毛坯密度和热处理的工艺，使得磁体的矫顽力和磁能积大大提高。与3-5μm左右的磁粉相比，本发明将NdFeB废料破碎成-60目至-300目的大颗粒的粉末，其抗氧化性大大提高，因此，磁粉和毛坯的储存、取向成型过程可以在大气的环境下进行，无需N2保护，因此制粉和成型工艺更加简便。
本发明的技术方案为：将清洗干净、去皮后的烧结钕铁硼回收废料在N2气或惰性气体保护下进行机械破碎，得到的磁粉在大气环境下，于磁场中取向成型，制成毛坯，随后热处理，制成高性能的钕铁硼磁体，具体步骤包括：
（1）制粉：
将清洗干净的烧结钕铁硼回收废料在N2气或惰性气体保护下进行机械破碎，破碎后的粉末过筛，筛下粉末为原料磁粉。
筛网的尺寸介于60~300目之间，若筛网的孔径太粗，磁粉粒径太大，会造成热处理后制成的磁体组织孔洞多，外观差、密度低，磁性能差；若筛网的孔径太细，磁粉容易氧化，不利于在大气环境下压制成型，磁体性能低。
（2）制备毛坯
在无需气体保护的环境下，在室温条件下，将上述制得的钕铁硼粉末取向压制成型，制成毛坯，取向磁场的强度≥0.5T，毛坯的密度为4.0~6.0g/cm3之间。
取向磁场的强度太小，不利于磁粉的取向，降低磁体的各向异性和磁能积。毛坯的密度小于4.0g/cm3时，毛坯强度太差，难以移动；密度高于6.0g/cm3时，压制压力过大，降低取向效果，模具损伤严重。
（3）热处理
将上述毛坯置于真空烧结炉中抽真空至5x10-3Pa，然后进行热处理，热处理的温度范围为500-1080℃，时间为0.5~10h，冷却后得到NdFeB磁体。
与现有技术相比，本发明的有益效果如下：
1）本发明的原料粉末——机械破碎烧结NdFeB废料得到的的磁粉的粒径尺寸大（如过80目筛，磁粉粒径≤200微米），远大于技术背景中所述的回收方法二中的粉末颗粒尺寸（3-5μm），因此，制粉的工艺更加简单，制粉效率更高。
2）由于本发明所制备的NdFeB粉末颗粒的尺寸粒径在百微米级，因此，磁粉的储存、磁体的取向成型过程及成型后毛坯的储存环境无需气体保护，进一步提升了生产效率。
3）现有技术中，采用重熔或者重新制粉的方法实现对NdFeB回收废料的再利用，但原料中只能添加少量的回收废料（一般添加量不超过20%），而本发明全部以NdFeB回收废料为原料来制备高性能的永磁体。
附图说明
图1 是表示实施例1中的毛坯及各实施例的磁体的退磁曲线。
具体实施方式
下面通过实施例对本发明作进一步的详细说明，以下实施例是对本发明的解释而本发明并不局限于以下实施例。
原料为N系烧结钕铁硼磁体的机加工边角料，烧结钕铁硼磁体的原始矫顽力为Hci=12.1kOe；取向成型的磁场强度为1.5T。
实施例1
将清洗干净的原料在氮气保护下机械破碎，过60目筛，将筛下粉末在大气环境下取向成型，毛坯的密度为5.5g/cm3，毛坯经1000℃，保温1h热处理后，得到磁体。
实施例2
将清洗干净的原料在氮气保护下机械破碎，过120目筛，将筛下粉末在大气环境下取向成型，毛坯的密度为5.3g/cm3，毛坯经950℃，保温1h热处理后，得到磁体。
实施例3
将清洗干净的原料在氮气保护下机械破碎，过60目筛，将筛下粉末在大气环境下取向成型，毛坯的密度为5.2g/cm3，毛坯经800℃，保温1h热处理后，得到磁体。
将所得磁体进行磁性能检测，同时给出了实施例1中毛坯的磁性能，退磁曲线见图1，具体性能见表1。
表1. 实施例毛坯及磁体的磁性能对比。
虽然本发明已以实施例公开如上，但其并非用以限定本发明的保护范围，任何熟悉该项技术的技术人员，在不脱离本发明的构思和范围内所作的更动与润饰，均应属于本发明的保护范围。

Claims (5)

1.一种烧结钕铁硼回收废料的再生利用方法，其特征在于，将烧结钕铁硼回收废料经清洗、去皮后，破碎成粉末；然后将粉末颗粒进行磁场取向成型，制成毛坯；随后对毛坯进行真空热处理，得到高性能的烧结NdFeB永磁体，具体包括如下步骤：
（1）制粉：
将清洗干净的烧结钕铁硼回收废料在N2气或惰性气体保护下进行机械破碎，破碎后的粉末过筛，筛下粉末为原料磁粉，筛网的尺寸介于60~300目之间；
（2）制备毛坯：
在无需气体保护的环境下，在室温条件下，将上述制得的钕铁硼粉末取向压制成型，制成毛坯；
（3）热处理：
将上述毛坯置于真空烧结炉中抽真空至5x10-3Pa，然后进行热处理，热处理的温度范围为500-1080℃，时间为0.5~10h，冷却后得到NdFeB磁体。
2.根据权利要求1所述一种烧结钕铁硼回收废料的再生利用方法，其特征在于，所述的烧结钕铁硼回收废料是指机加工切割的边角料和/或电镀不合格产品。
3.根据权利要求1所述一种烧结钕铁硼回收废料的再生利用方法，其特征在于，所述的机械破碎方法是指利用鄂式破碎机和/或震动破碎机和/或锤式破碎机方法对钕铁硼回收废料进行破碎处理。
4.根据权利要求1所述一种烧结钕铁硼回收废料的再生利用方法，其特征在于，所述的毛坯的密度介于4.0~6.0g/cm3之间。
5.根据权利要求1所述一种烧结钕铁硼回收废料的再生利用方法，其特征在于，所述的取向场的强度≥0.5T。
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