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CN107275027B - 应用钇的富铈稀土永磁体及其制备方法 - Google Patents

应用钇的富铈稀土永磁体及其制备方法 Download PDF

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CN107275027B
CN107275027B CN201710330274.0A CN201710330274A CN107275027B CN 107275027 B CN107275027 B CN 107275027B CN 201710330274 A CN201710330274 A CN 201710330274A CN 107275027 B CN107275027 B CN 107275027B
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严密
彭白星
金佳莹
马天宇
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Zhejiang University ZJU
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    • 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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    • 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
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Abstract

本发明公开应用钇的富铈稀土永磁体及其制备方法。本发明制备的稀土永磁体含有一种RE‑Fe‑B主相和一种或者多种添加钇的富铈主相。不同的主相分开设计成分、配料和制粉后，将相应主相合金粉末按照比例均匀混合，然后经磁场压型、烧结和热处理，制备具有多主相结构的稀土永磁体。通过优化烧结和热处理工艺，进一步缓解磁稀释效应，提高磁体的综合磁性能。本发明实现了钇元素在稀土永磁体中的大量应用，且永磁体的性能能够达到商用的标准，降低了原材料的成本的同时也满足了市场的需求。

Description

应用钇的富铈稀土永磁体及其制备方法
技术领域
本发明涉及应用钇的富铈稀土永磁体及其制备方法
背景技术
近年来，由于受到了国内外研究人员的广泛关注，用Ce(铈)元素取代部分Nd(钕)元素后制备的富Ce稀土永磁体已经取得了较大的进展。虽然Ce2Fe14B的内禀磁性能(饱和磁极化强度JS＝1.17T，磁晶各向异场HA＝26kOe)比Nd2Fe14B的内禀磁性能(饱和磁极化强度JS＝1.60T，磁晶各向异场HA＝73kOe)要弱很多，但是研究人员通过优化制备工艺，改变传统的制备方法，大大弱化了Ce加入到钕铁硼磁体后的所产生的严重磁稀释效应。而作为另外一种储量很高，价格较低的稀土元素Y(钇)，却一直未能应用到稀土永磁体的生产中。所以将Y元素应用到永磁体的制造中，不论是从降低成本还是平衡稀土资源利用的角度来说都有着十分重要的意义。
Y2Fe14B化合物的磁晶各向异场HA在室温下不仅和Ce2Fe14B相近，而且还有着更大的饱和磁极化强度JS(1.41T)和更高的居里温度TC(565K)，其2:14:1化合物由于不存在3d电子与4f电子的耦合作用，在基础研究中被广泛涉及。而Ce2Fe14B的居里温度(424K)在所有的RE2Fe14B化合物中是最低的，所以单独用Ce替换部分Nd元素的烧结钕铁硼磁体的磁性能比未替换前的磁体要恶化很多，而且不利于磁体在复杂环境中的使用。本发明不仅可以将Y元素大量应用到稀土永磁体的制造中，而且还能够保持甚至提高富Ce磁体的磁性能。在稀土价格一路上涨，全球稀土产业面临成本控制难题的现状下，将两种高丰度稀土共同使用，能够进一步减少价格高、丰度低的镨、钕、铽、镝等稀土元素的使用量，有效实现原料成本的控制。同时这样也能平衡稀土资源的利用，保护我国珍贵的稀土资源。
发明内容
本发明的目的是克服钇元素长期以来不能应用到稀土永磁体中的不足，提供应用钇的富铈稀土永磁体及其制备方法。
应用钇的富铈稀土永磁体具有多主相结构，包括一种RE-Fe-B主相和一种或者多种添加钇的富铈主相。
RE-Fe-B主相成分的质量百分数通式为REaFe100-a-b-cMbBc，一种或者多种添加钇的富铈主相成分的质量百分数通式均为[(YxCe1-x)yRE1-y]aFe100-a-b-cMbBc，式中RE为Nd、Pr、Dy、Tb、Gd、Er、Ho中的一种或几种，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、Zr元素中一种或几种；x、y、a、b、c满足以下关系：0<x≤0.6，0.01≤y<1，28≤a≤33，0.5≤b≤2，0.8≤c≤1.5。
所述的RE-Fe-B主相占主相总质量的10％～90％，所有添加钇的富铈主相占主相总质量的10％～90％；当稀土永磁体中包含两种或者两种以上添加钇的富铈主相时，则各添加钇的富铈主相成分是不同的。
应用钇的富铈稀土永磁体的制备方法具体如下：
1)按照设计的主相成分分别进行配料，在真空度高于10-2Pa的真空中频感应炉中熔炼不同主相合金，采用速凝铸带技术得到厚度为0.2～0.5mm的不同主相合金甩片，然后经过氢爆和气流磨工艺制备平均粒度为3～4μm的相应主相合金粉末；
2)将相应主相合金粉末按照比例均匀混合，得到不同Y-Ce取代量的混合主相粉末；
3)将混合主相粉末在1.5～2T的磁场下进行取向压型，得到生坯；
4)将得到的生坯进行真空封装，15～20MPa间冷等静压1～3min，放入高真空正压烧结炉，在1000～1080℃间烧结2.5～5h，850～950℃间进行一级回火，480～680℃间进行二级回火，得到稀土永磁体。
本发明与现有技术相比具有的有益效果：1)本发明解决了长期以来钇元素不能应用到稀土永磁体中的难题，实现了钇元素在稀土永磁体中的大量应用；2)通过在富铈主相合金中添加丰度较高的钇元素，保持甚至提高了富铈主相的磁性能，从而使得永磁体的磁性能达到商用的标准，可进行广泛地生产应用；3)本发明所提供的应用钇的富铈稀土永磁体的制备方法，根据各稀土元素的不同特性选择合适的烧结工艺和热处理的工艺，使磁体充分致密的同时又防止了主相晶粒的进一步长大，满足了实际的应用需求；4)通过对添加钇的富铈主相成分进行合金元素的优化设计，进一步抑制磁稀释效应，在较高钇和铈含量时磁体也能保持很好的磁性能；5)通过应用价格较低的稀土元素钇和铈，有效地实现了原料成本的控制，同时也减少了镨、钕、铽、镝等稀土元素的使用量，保护了我国珍贵的稀土资源。
具体实施方式
应用钇的富铈稀土永磁体具有多主相结构，包括一种RE-Fe-B主相和一种或者多种添加钇的富铈主相；
RE-Fe-B主相成分的质量百分数通式为REaFe100-a-b-cMbBc，一种或者多种添加钇的富铈主相成分的质量百分数通式均为[(YxCe1-x)yRE1-y]aFe100-a-b-cMbBc，式中RE为Nd、Pr、Dy、Tb、Gd、Er、Ho中的一种或几种，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、Zr元素中一种或几种；x、y、a、b、c满足以下关系：0<x≤0.6，0.01≤y<1，28≤a≤33，0.5≤b≤2，0.8≤c≤1.5。
所述的RE-Fe-B主相占主相总质量的10％～90％，所有添加钇的富铈主相占主相总质量的10％～90％；当稀土永磁体中包含两种或者两种以上添加钇的富铈主相时，则各添加钇的富铈主相成分是不同的。
应用钇的富铈稀土永磁体的制备方法具体如下：
1)按照设计的主相成分分别进行配料，在真空度高于10-2Pa的真空中频感应炉中熔炼不同主相合金，采用速凝铸带技术得到厚度为0.2～0.5mm的不同主相合金甩片，然后经过氢爆和气流磨工艺制备平均粒度为3～4μm的相应主相合金粉末；
2)将相应主相合金粉末按照比例均匀混合，得到不同Y-Ce取代量的混合主相粉末；
3)将混合主相粉末在1.5～2T的磁场下进行取向压型，得到生坯；
4)将得到的生坯进行真空封装，15～20MPa间冷等静压1～3min，放入高真空正压烧结炉，在1000～1080℃间烧结2.5～5h，850～950℃间进行一级回火，480～680℃间进行二级回火，得到稀土永磁体。
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)以质量百分数计，成分为[(Y0.2Ce0.8)0.5Nd0.5]30.5Fe67.11Co0.8Zr0.59B1的主相A和Nd30.5Fe67.11Co0.8Zr0.59B1的主相B分别配料，在真空度高于10-2Pa的真空中频感应炉熔炼后，采用速凝铸带技术得到厚度为0.31mm的相应主相甩片；
2)将相应主相甩片经过氢爆和气流磨工艺制备平均粒度为3.3μm的相应合金粉末；
3)按照3:7的质量比将A、B主相合金粉末均匀混合后，在氮气保护下将混合主相粉末在2T的磁场下取向成型，并经17MPa冷等静压制成生坯；
4)将生坯放在真空烧结炉中进行烧结，烧结温度为1075℃，烧结时间3h，在890℃间进行一级回火，560℃间进行二级回火，得到稀土永磁体。
5)磁体磁性能为Br＝13.2kGs，Hcj＝11.8kOe，(BH)max＝43.6MGOe。
对比例1：
1)以质量百分数计，成分为(Ce0.5Nd0.5)30.5Fe68.5B1的主相A和Nd30.5Fe68.5B1的主相B分别配料，在真空度高于10-2Pa的真空中频感应炉熔炼后，采用速凝铸带技术得到厚度为0.31mm的相应主相甩片；
2)将相应主相甩片经过氢爆和气流磨工艺制备平均粒度为3.3μm的相应合金粉末；
3)按照3:7的质量比将A、B主相合金粉末均匀混合后，在氮气保护下将混合主相粉末在2T的磁场下取向成型，并经17MPa冷等静压制成生坯；
4)将生坯放在真空烧结炉中进行烧结，烧结温度为1080℃，烧结时间3h，在890℃间进行一级回火，580℃间进行二级回火，得到稀土永磁体。
5)磁体磁性能为Br＝12.8kGs，Hcj＝11.4kOe，(BH)max＝41.8MGOe；
说明：通过对比例1和实施例1的比较可以发现，实施例1中添加钇的富铈磁体的各项磁性能指标都好于对比例中的磁体，进一步说明了本发明不仅实现了钇元素在稀土永磁体中的应用，而且也能提高富铈磁体的磁性能。而且磁体的综合磁性能也达到了商用牌号的标准，降低了原材料的成本，满足了应用需求。同时，通过对比发现，本发明(实施例1)中成分合金元素的优化设计以及热处理工艺的改良优化都是保障磁体性能较高的原因。
实施例2：
1)以质量百分数计，成分为[(Y0.25Ce0.75)0.6Nd0.4]30.2Fe67.45Co0.8Ga0.55B1的主相A、成分为[(Y0.25Ce0.75)0.4Nd0.6]30.2Fe67.45Co0.8Ga0.55B1的主相B和成分为Nd30.2Fe67.45Co0.8Ga0.55B1的主相C分别配料，在真空度高于10-2Pa的真空中频感应炉熔炼后，采用速凝铸带技术得到厚度为0.33mm的相应主相甩片；
2)将相应主相甩片经过氢爆和气流磨工艺制备平均粒度为3.1μm的相应合金粉末；
3)按照2:2:1的质量比将A、B和C主相合金粉末均匀混合后，在氮气保护下将混合主相粉末在2T的磁场下取向成型，并经17MPa冷等静压制成生坯；
4)将生坯放在真空烧结炉中进行烧结，烧结温度为1080℃，烧结时间3h，在890℃间进行一级回火，560℃间进行二级回火，得到稀土永磁体；
5)磁体磁性能为Br＝12.7kGs，Hcj＝8.8kOe，(BH)max＝36.1MGOe。
实施例3：
1)以质量百分数计，成分为[(Y0.3Ce0.7)0.5Nd0.5]30.5Fe67.11Co1.39B1的主相A和Nd30.5Fe67.11Co1.39B1的主相B分别配料，在真空度高于10-2Pa的真空中频感应炉熔炼后，采用速凝铸带技术得到厚度为0.31mm的相应主相甩片；
2)将相应主相甩片经过氢爆和气流磨工艺制备平均粒度为3.3μm的相应合金粉末；
3)按照1:4的质量比将A、B主相合金粉末均匀混合后，在氮气保护下将混合主相粉末在2T的磁场下取向成型，并经17MPa冷等静压制成生坯；
4)将生坯放在真空烧结炉中进行烧结，烧结温度为1075℃，烧结时间3h，在890℃间进行一级回火，580℃间进行二级回火，得到稀土永磁体。
5)磁体磁性能为Br＝13.5kGs，Hcj＝12.1kOe，(BH)max＝45.1MGOe。

Claims (1)

1.应用钇的富铈稀土永磁体，其特征在于：该永磁体具有多主相结构，包括一种RE-Fe-B主相和多种添加钇的富铈主相，其中RE-Fe-B主相占主相总质量的10%~90%，所有添加钇的富铈主相占主相总质量的10%~90%；
RE-Fe-B主相成分的质量百分数通式为REaFe100-a-b-cMbBc，多种添加钇的富铈主相成分的质量百分数通式均为[(YxCe1-x)yRE1-y]aFe100-a-b-cMbBc，式中RE为Nd、Pr、Dy、Tb、Gd、Er、Ho中的一种或几种，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、Zr元素中一种或几种；x、y、a、b、c满足以下关系：0<x≤0.6，0.01≤y<1，28≤a≤33，0.5≤b≤2，0.8≤c≤1.5；当稀土永磁体中包含两种或者两种以上添加钇的富铈主相时，则各添加钇的富铈主相成分中y是不同的，其中一种添加钇的富铈主相成分中0.6≤y<1。
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