CN106384638B - 一种高性能各向异性Sm‑Fe‑N永磁体的制备方法 - Google Patents

一种高性能各向异性Sm‑Fe‑N永磁体的制备方法 Download PDF

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CN106384638B
CN106384638B CN201610964191.2A CN201610964191A CN106384638B CN 106384638 B CN106384638 B CN 106384638B CN 201610964191 A CN201610964191 A CN 201610964191A CN 106384638 B CN106384638 B CN 106384638B
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包小倩
高学绪
高硕�
马斌
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    • 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
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    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
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Abstract

一种高性能各向异性Sm‑Fe‑N永磁体的制备方法，属于稀土永磁材料领域。其特征在于将各向异性Sm2Fe17Nx合金粉和少量低熔点金属/合金粉混合或者是在各向异性Sm2Fe17Nx合金粉的表面包覆一薄层低熔点金属/合金膜，之后在磁场下取向压型，而后在480－520℃温度下热压烧结致密化，得到高性能各向异性Sm‑Fe‑N永磁体。该低熔点金属/合金成份由R‑M,R‑N,R‑(M,N)或N‑N组成，熔点范围300－450℃，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。该发明的优点是可以制备高致密的各向异性Sm2Fe17Nx永磁体，因此可以获得高的永磁性能。

Description

一种高性能各向异性Sm-Fe-N永磁体的制备方法
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各向异性Sm-Fe-N永磁体的制备方法。
背景技术
Sm2Fe17Nx稀土永磁材料由于具有优异的内禀赋磁性能，它的饱和磁化强度达1.54T，(BH)max可达472.0kJ/m3，完全可与Nd-Fe-B相媲美；居里温度为470℃，比Nd-Fe-B永磁体高160℃；各向异性场为14T，远高于Nd-Fe-B的7T左右；并且其耐腐蚀性、热稳定性、抗氧化性也更优于Nd-Fe-B永磁材料，因此Sm2Fe17Nx稀土永磁材料具有广阔的前景。
二元Sm2Fe17化合物是易基面，各向异性场低，不能制作成为有实用意义的永磁体。1990年，Coey等利用气固相反应法研制出系列R2Fe17Nx化合物，其中Sm2Fe17Nx化合物显示出室温单轴各向异性，为钐铁氮稀土永磁材料的发展奠定了良好的基础。
目前Sm2Fe17Nx合金粉的制备方法，通常都是先通过快淬法、机械合金化法、还原扩散法、HDDR法、气雾化法等制得Sm2Fe17合金粉，而后将Sm2Fe17合金粉在500℃左右氮化处理得到Sm2Fe17Nx合金粉。Sm2Fe17Nx磁体一般采用先制备出Sm2Fe17Nx粉末然后制作成粘结磁体，粘结磁体是将磁粉与粘结剂和其它添加剂按一定比例均匀复合，然后用压制、注射、挤出和压延成型等方法制作而成。粘结磁体具有形状复杂、尺寸精度高的优点，然而由于其各向同性的特点，其磁性能较低。
专利(CN 102737801 B)和专利(CN 105355354 A)公开了一种Sm-Fe-N各向异性磁粉的制备方法，即通过快速凝固工艺得到细小Sm2Fe17柱状晶近一致取向的速凝铸片，之后通过破碎并氮化得到各向异性Sm2Fe17Nx磁粉。尽管各向异性Sm2Fe17Nx磁粉的成功制备为制备各向异性Sm2Fe17Nx磁体提供了可能，然而由于Sm2Fe17Nx化合物在600℃以上会发生不可逆分解，形成α-Fe和Sm-N化合物，这也就是目前只有Sm2Fe17Nx粘结永磁体而无Sm2Fe17Nx烧结永磁体的主要原因。如前所述粘结磁体是各向同性的，性能远低于各向异性磁体。
发明内容
本发明目的在于解决Sm2Fe17Nx化合物在600℃以上会发生不可逆分解，形成α-Fe和Sm-N化合物，无法在高于600℃的温度下烧结得到Sm2Fe17Nx各向异性永磁体的问题。
一种高性能各向异性Sm-Fe-N永磁体的制备方法，其特征在于：将各向异性Sm2Fe17Nx合金粉和少量低熔点金属/合金粉混合或者是在各向异性Sm2Fe17Nx合金粉的表面包覆一薄层低熔点金属/合金粉，之后在磁场下取向压型，而后在480—520℃左右温度下热压烧结致密化，得到高性能各向异性Sm-Fe-N永磁体；该低熔点金属/合金成份由R-M,R-N,R-(M,N)或N-N组成，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；低熔点金属/合金熔点范围300－450℃，在烧结温度下熔化为液态，实现液相烧结；
具体工艺步骤为：
1)将各向异性Sm2Fe17Nx合金粉和少量低熔点金属/合金粉混合或者是在各向异性Sm2Fe17Nx合金粉的表面包覆一薄层低熔点金属/合金膜；
2)经过混合或表面包覆处理的Sm2Fe17Nx粉末在1.8－2.5T的磁场下取向压型；
3)低温热压烧结致密化，得到高性能各向异性Sm-Fe-N永磁体。
工艺步骤1)中，在各向异性Sm2Fe17Nx合金粉中添加3－8％重量分数的低熔点金属/合金粉或者在各向异性Sm2Fe17Nx合金粉的表面包覆一层厚度为10－100nm的低熔点金属/合金膜。
工艺步骤3)中，热压烧结的压力为10-200MPa，时间0.5－2h。
虽然Sm2Fe17Nx的各向异性场为14T(远高于Nd-Fe-B的7T左右)，饱和磁化强度达1.54T，(BH)max可达472.0kJ/m3，完全可与Nd-Fe-B相媲美，居里温度为470℃，比Nd-Fe-B永磁体高160℃，并且其耐腐蚀性、热稳定性、抗氧化性也更优于Nd-Fe-B永磁材料。并且Sm2Fe17Nx各向异性粉的成功制备为各向异性Sm2Fe17Nx磁体的成功制备奠定了良好的基础，而各向异性Sm2Fe17Nx磁体的性能是要远优于各向同性Sm2Fe17Nx粘结磁体的。然而遗憾的是，Sm2Fe17Nx化合物在600℃以上会发生不可逆分解，形成α-Fe和Sm-N化合物，也就是只要超过600℃，Sm2Fe17Nx化合物就不复存在。不过可喜的是，通过在Sm2Fe17Nx各向异性粉中引入低熔点金属/合金，在磁场中取向压制成型，而后在480－520℃温度下低温烧结，常规的低温烧结很难使磁体烧结致密，为了克服低温烧结不易致密化的问题，需要同时施加10－200MPa的压力，进一步促进其致密化，从而真正实现低温烧结致密化，最终得到高性能各向异性Sm2Fe17Nx磁体。低熔点金属/合金在烧结温度下熔化为液态，一方面起助烧剂实现致密化的作用，另一方面还作为非磁性晶界相，为获得高磁性能特别是高矫顽力的各向异性Sm2Fe17Nx磁体起至关重要的作用。
本发明的优点是：
1)可以制备各向异性Sm2Fe17Nx磁体；
2)各向异性Sm2Fe17Nx磁体磁性能远高于各向同性Sm2Fe17Nx粘结磁体。
具体实施方式
实施例1：
用稀土Sm、工业纯铁、金属Cu和Al为原料，按Sm11.5Fe87.5Al0.4Cu0.6配料，考虑到Sm容易挥发，多加15％的烧损量，用真空感应炉熔炼合金。利用速凝铸片工艺制备厚度为0.2－0.4mm的合金薄带，用XRD分析证明主要形成了Sm2Fe17相，对薄带截面的电镜观察可见形成了厚度为2－6μm为片状晶，晶界富Al和Cu。将铸片在750℃真空热处理1.5小时后空冷，将铸片破碎成200μm左右的颗粒；再在480℃氮化6小时，通过气-固反应氮化成Sm2Fe17Nx；再经球磨破碎成粒度为3-5微米，得到各向异性Sm2Fe17Nx磁粉。在Sm2Fe17Nx磁粉中添加重量分数5％、粒度为0.1－1μm的Pr83Co2Cu15粉，混合均匀。将混合粉在2.0T磁场下取向压型并冷等静压，随后在500℃、100MPa下真空热压烧结0.5h，得到高致密各向异性Sm2Fe17Nx磁体。
实施例2：
用稀土Sm、工业纯铁为原料，按Sm10.5Fe89.50配料，考虑到Sm容易挥发，多加15％的烧损量，用真空感应炉熔炼Sm-Fe合金。利用速凝铸片工艺制备厚度为0.2－0.4mm的合金薄带，用XRD分析证明主要形成了Sm2Fe17相，对薄带截面的电镜观察可见形成了厚度为2－6μm为片状晶。将铸片在750℃真空热处理1.5小时后空冷，将铸片破碎成200μm左右的颗粒；再在480℃氮化6小时，通过气-固反应氮化成Sm2Fe17Nx；再经球磨破碎成粒度为3-5微米的各向异性Sm2Fe17Nx磁粉。通过气相沉积的方法在Sm2Fe17Nx磁粉表面沉积厚度为50nm的Zn80Al20(质量分数)薄层。将表面包覆的Sm2Fe17Nx粉在2.0T磁场下取向压型并冷等静压，随后在500℃、50MPa下真空烧结1h，得到高致密各向异性Sm2Fe17Nx磁体。

Claims (1)

1.一种高性能各向异性Sm‐Fe‐N永磁体的制备方法，其特征在于：将各向异性Sm2Fe17Nx合金粉和少量低熔点金属/合金粉混合或者是在各向异性Sm2Fe17Nx合金粉的表面包覆一薄层低熔点金属/合金膜，之后在磁场下取向压型，而后在480—520℃的温度下热压烧结致密化，得到高性能各向异性Sm‐Fe‐N永磁体；该低熔点金属/合金成份由R‐M,R‐N,R‐(M,N)或N‐N组成，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；低熔点金属/合金熔点范围300－450℃，在烧结温度下熔化为液态，实现液相烧结；
具体工艺步骤为：
1)将各向异性Sm2Fe17Nx合金粉和少量低熔点金属/合金粉混合或者是在各向异性Sm2Fe17Nx合金粉的表面包覆一薄层低熔点金属/合金膜；
2)经过混合或表面包覆处理的各向异性Sm2Fe17Nx粉末在1.8－2.5T的磁场下取向压型；
3)低温热压烧结致密化，得到高性能各向异性Sm‐Fe‐N永磁体；
工艺步骤1)中，在各向异性Sm2Fe17Nx合金粉中添加3－8％重量分数的低熔点金属/合金粉或者在各向异性Sm2Fe17Nx合金粉的表面包覆一层厚度为10－100nm的低熔点金属/合金膜；
工艺步骤3)中，热压烧结的压力为10‐200MPa，时间0.5－2h。
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