CN113593878A - 一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法 - Google Patents

一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法 Download PDF

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CN113593878A
CN113593878A CN202110763009.8A CN202110763009A CN113593878A CN 113593878 A CN113593878 A CN 113593878A CN 202110763009 A CN202110763009 A CN 202110763009A CN 113593878 A CN113593878 A CN 113593878A
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吴琼
杨杭福
葛洪良
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China Jiliang University
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Abstract

本发明公开了一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，包括以下步骤：按一定化学计量比称取原材料，研磨混合之后，将粉末压制成块；将压制成的块在一定温度条件下预烧，形成前驱体；清洗前驱体，干燥后，作为靶材，放入烧杯的靶材支架上，装入异丙酮溶液没过前驱体5~10mm，将烧杯置于旋转平台上，采用Nd:YAG激光器三次谐波作为烧蚀激光光源，将激光脉冲光束聚焦在前驱体表面烧蚀，生成含纳米级颗粒沉淀物的混合溶液；将混合溶液的沉淀物过滤，并反复清洗，烘干之后，获得纳米级高性能复合永磁体材料。本发明制备得到的复合纳米晶永磁体表面干净，化学活性好，同时有效抑制结构畸形，提高纳米晶磁体的磁性能。

Description

一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法
技术领域
本发明具体涉及一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法。
背景技术
复合纳米晶磁性材料是近年来开发的一种新型双相永磁材料。它是由高磁晶各向异性的硬磁相和高饱和磁化强度的软磁相在纳米尺度上产生强烈的磁交换耦合作用，使磁体呈现明显的剩磁增强效应（Mr/Ms>0.5）。目前对高性能的复合纳米晶磁性材料的研究较少，因此，需要提供一种高性能的复合纳米晶磁性材料的制备方法。
发明内容
针对上述情况，为克服现有技术的缺陷，本发明提供一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法。
为了实现上述目的，本发明提供以下技术方案：
一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，包括以下步骤：
（1）配料阶段：按一定化学计量比称取原材料，研磨混合之后，将粉末压制成块；
（2）预烧阶段：将压制成的块在一定温度条件下预烧，形成前驱体；
（3）烧蚀阶段：清洗前驱体，80-120oC干燥后，作为靶材，放入烧杯的靶材支架上，装入异丙酮溶液没过前驱体5~10mm，将烧杯置于旋转平台上，采用Nd:YAG激光器三次谐波作为烧蚀激光光源，将激光脉冲光束聚焦在前驱体表面烧蚀，生成含纳米级颗粒沉淀物的混合溶液；
（4）分离阶段：将混合溶液的沉淀物过滤，并反复清洗，烘干之后，获得纳米级高性能复合永磁体材料。进一步地，步骤（1）中，所述原材料包括金属Nd、Dy、Tb、In、Fe、Co粉末，NbFe粉末，FeB粉末和感应熔炼的MnBi粉末，其中FeB粉末中B质量分数为19.83%；NbFe粉末中Nb质量分数为66.3%；MnBi粉末中Mn与Bi的元素质量比例为54∶46。
进一步地，步骤（1）中，压制成的块的长度、宽度分别为12~25mm，厚度为3~6mm。
进一步地，步骤（2）中，预烧阶段的温度为900~1100℃，预烧时间为4~6h。预烧阶段的温度设置为900~1100℃，这样利于晶界相流动，提高磁性能。
进一步地，步骤（3）中，所述Nd:YAG激光器为纳秒固体激光器，激光频率为10 Hz，波长为1064nm，脉宽为7ns，激光脉冲强度为100~250mJ/pulse，光斑直径为1mm。激光参数设置成上述数值，有利于将材料融化，并形成纳米颗粒。
进一步地，步骤（3）中，将激光脉冲光束聚焦在前驱体表面烧蚀10~20min。
进一步地，步骤（3）中，利用超声清洗剂清洗前驱体，所述超声清洗剂为乙醇。
进一步地，步骤（3）中，将烧杯置于旋转转速为20 r/min的旋转平台上。
进一步地，步骤（4）中，采用为离心机过滤，离心速度为5000~15000rpm。
进一步地，步骤（4）中，烘干温度为150 oC。
本发明的有益效果是：
（1）本发明的复合永磁体材料的化学组成为Nd2Fe14B/MnBi，本发明制备方法，其可在室温下产生高温高压等的极端的环境，通过在高溫高压的极端环境中，来自于靶材和溶液介质的粒子会发生各种反应，而且液体的冷却效果好，能实现高温等离子体的快速冷却，制备得到的复合纳米晶永磁体表面干净，化学活性好，同时有效抑制结构畸形，提高纳米晶磁体的磁性能。大小为纳米级的纳米复合永磁体材料，其晶粒尺寸更均匀，综合磁性能更高。
（2）本发明的激光液相烧蚀纳米复合永磁体材料制备法更简洁，环境更易控制，液体的冷却效果好，能实现高温等离子体的快速冷却，保护了纳米复合永磁体材料，得到分布均匀的纳米微晶结构。
（3）本发明中，烧蚀后磁体晶界相中具有更干净的表面和更高的化学活性，复合相在纳米晶尺度上将产生强烈的交换耦合作用，将得到较高的理论最大磁能积。
附图说明
图1是本发明制备方法示意图。
图2是本发明制备得到的Nd2Fe14B/MnBi复合磁性材料的TEM图。
具体实施方式
以下结合附图对本发明的技术方案做进一步详细说明，应当指出的是，具体实施方式只是对本发明的详细说明，不应视为对本发明的限定。
实施例1
一种液相激光烧蚀法制备纳米级复合磁体材料的方法包括以下步骤：
（1）配料阶段：原子个数比为Nd：Dy：Fe：Nb：Co：B=9：0.4：80.24：0.36：3：6，将原子个数比，换算成质量比，然后称取金属粉末材料Nd、Dy、Tb、In、Fe、Co、FeB（FeB中B质量分数为19.83%）和NbFe（NbFe中Nb质量分数为66.3%），再加入成品的MnBi（Mn和Bi的原子个数比为54:46）粉末经过充分研磨混合之后，将原材料粉末在15Mpa压力下压成长度为15mm，宽度为15mm，厚度为4mm的块；
（2）预烧阶段：将压制成的块在1050 oC预烧4h，形成前驱体；
（3）烧蚀阶段：前驱体温度降到室温，利用超声清洗剂将前驱体清洗30min，80oC干燥5h后，放入烧杯的靶材支架上，装入异丙酮没过前驱体7mm，将烧杯置于旋转转速为20 r/min的磁力搅拌器上，采用Nd:YAG激光器三次谐波作为烧蚀激光光源，激光频率为10 Hz，波长为1064nm，脉宽为7ns，激光脉冲强度为100 mJ/pulse，光斑直径为1 mm，将激光脉冲光束聚焦在前驱体表面烧蚀20 min，生成含纳米级颗粒沉淀物的混合溶液；
（4）分离阶段：将混合溶液的沉淀物采用离心机过滤，并反复清洗5次，离心机速率为10000rpm，离心1h，之后在150 oC条件下烘干4h，获得纳米级高性能Nd2Fe14B/MnBi复合磁性材料，其结构形貌如图2所示。
与快淬法制备的材料相比，本发明所制得的纳米复合永磁体的矫顽力控制机理仍为成核机制，但其晶粒尺寸更小，平均颗粒大小为9nm~180nm, 磁能积为18.6MGOe，相比于高能球磨得到的材料磁能积（14.2MGOe），提高了30.1%，综合磁性能显著提高。
实施例2
一种液相激光烧蚀法制备纳米级复合磁体材料的方法包括以下步骤：
（1）配料阶段：原子比：Nd：Dy：Fe：Nb：Co：B=9：0.4：80.24：0.36：3：6，将原子个数比，换算成质量比，然后称取金属粉末材料Nd、Dy、Tb、In、Fe、Co、FeB（FeB中B质量分数为19.83%）和NbFe（NbFe中Nb质量分数为66.3%），再加入成品的MnBi（Mn和Bi的原子个数比为54:46）粉末经过充分研磨混合之后，将原材料粉末在15Mpa压力下压成长度为12mm，宽度为15mm，厚度为6mm的块；
（2）预烧阶段：将压制成的块在1050 oC预烧4h，形成前驱体；
（3）烧蚀阶段：前驱体温度降到室温，利用超声清洗剂将前驱体清洗30min， 110oC干燥3h后，放入烧杯的靶材支架上，装入异丙酮没过前驱体10mm，将烧杯置于旋转转速为20r/min的磁力搅拌器上，采用Nd:YAG激光器三次谐波作为烧蚀激光光源，激光频率为10 Hz，波长为1064nm，脉宽为7ns，激光脉冲强度为150 mJ/pulse，光斑直径为1 mm，将激光脉冲光束聚焦在前驱体表面烧蚀15 min，生成含纳米级颗粒沉淀物的混合溶液；
（4）分离阶段：将混合溶液的沉淀物采用离心机过滤，并反复清洗5次，离心机速率为12000rpm，离心1h，之后在150 oC条件下烘干3h，获得纳米级高性能Nd2Fe14B/MnBi复合磁性材料。
本实施例所制得的纳米复合永磁体的矫顽力控制机理仍为成核机制，其晶粒尺寸小，平均颗粒大小为50nm~150nm, 磁能积为20.4MGOe，综合磁性能显著提高。
显然，所描述的实施例仅仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。

Claims (10)

1.一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，包括以下步骤：
（1）配料阶段：按一定化学计量比称取原材料，研磨混合之后，将粉末压制成块；
（2）预烧阶段：将压制成的块在一定温度条件下预烧，形成前驱体；
（3）烧蚀阶段：清洗前驱体，干燥后，作为靶材，放入烧杯的靶材支架上，装入异丙酮溶液没过前驱体5~10mm，将烧杯置于旋转平台上，采用Nd:YAG激光器三次谐波作为烧蚀激光光源，将激光脉冲光束聚焦在前驱体表面烧蚀，生成含纳米级颗粒沉淀物的混合溶液；
（4）分离阶段：将混合溶液的沉淀物过滤，并反复清洗，烘干之后，获得纳米级高性能复合永磁体材料。
2.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（1）中，所述原材料包括金属Nd、Dy、Tb、In、Fe、Co粉末，NbFe粉末，FeB粉末和感应熔炼的MnBi粉末，其中FeB粉末中B质量分数为19.83%；NbFe粉末中Nb质量分数为66.3%；MnBi粉末中Mn与Bi的元素质量比例为54∶46。
3.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（1）中，压制成的块的长度、宽度分别为12~25mm，厚度为3~6mm。
4.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（2）中，预烧阶段的温度为900~1100℃，预烧时间为4~6h。
5.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（3）中，所述Nd:YAG激光器为纳秒固体激光器，激光频率为10 Hz，波长为1064nm，脉宽为7ns，激光脉冲强度为100~250mJ/pulse，光斑直径为1mm。
6.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（3）中，将激光脉冲光束聚焦在前驱体表面烧蚀10~20min。
7.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（3）中，利用超声清洗剂清洗前驱体，所述超声清洗剂为乙醇。
8.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（3）中，将烧杯置于旋转转速为20 r/min的旋转平台上。
9.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（4）中，采用为离心机过滤，离心速度为5000~15000rpm。
10.根据权利要求1所述的一种制备纳米级高性能Nd2Fe14B/MnBi复合磁体材料的方法，其特征是，步骤（4）中，烘干温度为150 oC。
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