CN113593881A - 一种液相激光烧蚀法制备钕铁硼复合永磁体的方法 - Google Patents
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Abstract
本发明公开了一种液相激光烧蚀法制备钕铁硼复合永磁体的方法。本发明的钕铁硼复合永磁体材料的化学组成式为Nd2Fe14B/α‑Fe，所述的复合物中所涉及的元素有金属Nd、Dy、Tb、In、Nb、Fe、Co。本发明按一定化学计量比称取复合永磁体材料的原材料粉末，经过充分研磨混合之后，将原材料粉末压成块，将压制成的块在一定温条件下预烧，形成前驱体，利用激光烧蚀技术，制备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，烘干之后获得钕铁硼复合永磁体材料。该制备方法能够得到表面干净，化学活性好，其晶粒尺寸更小，具有较强的交换耦合强度，磁性能显著提高，并且制备过程简单、安全。
Description
技术领域
本发明涉及一种液相激光烧蚀法制备钕铁硼复合永磁体的方法，属于高性能磁性材料领域。
背景技术
液相激光烧蚀技术作为一种制备纳米粒子的新技术备受关注。液相激光烧蚀(Laser Ablation in Liquid，LAL)是一种简单、绿色的纳米材料制备技术，通常只需在水中或有机液相条件下进行。近年来，LAL已被用于制备一系列具有特殊形貌、微观结构的纳米材料，以及在探索新兴的，在光学、显示、探测、生物等领域的性能和应用中，实现了功能化纳米材料的一步制备。结果表明，液体激光烧蚀也适用于制备复合材料纳米粒子。与传统的纳米材料制备方法相比，液相激光烧蚀法有以下的优势:(1)它是一种“简单且干净”的合成手段，不仅制备过程简单，而且由于减少了副产物的生成，并且简化了反应的前驱物的使用，确保了最终产物很高的纯度，而且具有较高的表面活性；(2)液相激光烧蚀法在温和的条件下能够制备出高温高压的亚稳相；(3)这种制备方法几乎对所有纳米材料都有普适性，研究者可以根据材料的属性来选择所需的靶材和液体来合成纳米颗粒和结构；(4)纳米结构的相、尺寸和形状可以通过改变激光参数和外部条件来合成，而且很多反应一步就能实现，避免了繁杂的后处理。
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)。而剩磁的增强主要是靠纳米晶磁体内晶粒间的强交换耦合作用来实现的。因此，对纳米晶磁体的晶间交换耦合作用的研究已经成为提高该磁体磁性能的主要因素。
微结构计算研究表明，复合纳米晶永磁体的磁性能显著地随软磁相的晶粒尺寸、含量和晶粒形状等因素变化。当软磁相晶粒尺寸足够小时，由于晶界处的交换耦合作用，可以使纳米晶磁体的剩磁和矫顽力显著提升。同时，大量实验数据研究证明，当软磁相的含量为40％，同时晶粒为10nm且均匀分布在晶粒为10～20nm的硬磁相之间时，可以使纳米晶磁体的磁性能得到提高。
本发明采用液相激光烧蚀法，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，不仅制备过程简单，而且使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得到提高。
发明内容
本发明的目的是为克服现有技术的不足，提供一种利用液相激光烧蚀法的制备过程简单且低耗能和低温度系数以及低时耗的纳米级高性能复合永磁体的制备方法
具体制备包括如下步骤：
(1)配料阶段：按一定化学计量比称取一定量纳米复合永磁体原材料粉末，经过充分研磨混合之后，将粉末压成块；
(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：利用超声清洗剂将前驱体清洗15～30min，干燥后，放入烧杯的靶材支架上，装入异丙酮溶液没过前驱体5～10mm，将烧杯置于旋转转速为30r/min的旋转平台上，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10～20min，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3-5次，烘干之后，获得纳米级高性能复合永磁体材料。
具体的，步骤(1)所述的纳米复合永磁体化学式为Nd2Fe14B/α-Fe，所述的粉末为纯度>99.5％的金属Nd、Dy、Tb、In、Nb、Fe、Co粉末，B用FeB为原料，其中FeB中B质量分数为19.83％；Nb用NbFe为原料，NbFe中Nb质量分数为66.3％；其余采用99.99％的高纯金属原料。所述的压成块的大小为直径10～20mm，厚度为2～5mm。
具体的，步骤(2)所述的预烧条件，温度为600～800℃，时间为12～24h。
具体的，步骤(3)所述的激光器为纳秒固体激光器，激光频率为10Hz，波长为1064nm，脉宽为1～7ns，激光脉冲强度为100～350mJ/pulse，光斑直径为1～3mm，所述的清洗剂为色谱纯乙醇。
具体的，步骤(4)所述的过滤方法，采用为离心机过滤，速度为5000～15000rpm。
与快淬法相比，本发明具有如下优势：
(1)新型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；
(2)烧蚀后磁体晶界相中由于具有更干净表面和更高化学活性的纳米级稀土磁制冷材料，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；
(3)本发明，工艺过程环保简单，易操作，省时节能。
附图说明
图1液相激光烧蚀法靶材系统示意图。
图中：1.纳秒激光、2.反射镜、3.聚焦镜、4.石英玻璃盖、5.液体介质、6.靶材、7.靶材支架、8.旋转平台。
具体实施方式
为更进一步阐述本发明为实现预定发明目的所采取的技术手段及功效，以下结合附图及较佳实施例，对依据本发明的具体实施方式、结构、特征及其功效，详细说明如后。
实施例1。
实施例1：，如图1所示，采用一种液相激光烧蚀法制备Nd9Dy0.4Fe80.24InNb0.36Co3B6的方法。本发明的具体步骤如下：
(1)配料阶段：按原子比：Nd:Dy:Fe:Nb:Co:B＝9:0.4:80.24:0.36:3:6称取稀土磁性材料的原材料粉末Nd、Dy、Tb、In、Fe、Co，FeB(B质量分数为19.83％)、NbFe(Nb质量分数为66.3％)以及其他高纯金属原料经过充分研磨混合之后，将原材料粉末在15Mpa压力下压成直径为12mm，厚度为5mm的块；
(2)退火阶段：将压制成的块在680℃退火0.5h，形成前驱体；
(3)烧蚀阶段：利用超声清洗剂将前驱体清洗30min，干燥后，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30r/min的旋转平台上，采用Nd:YAG激光器三次谐波作为烧蚀激光光源，激光频率为10Hz，波长为1064nm，脉宽为1ns，激光脉冲强度为100mJ/pulse，光斑直径为3mm，将激光脉冲光束聚焦在前驱体表面烧蚀10min，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15000rpm，之后在150℃条件下烘干，获得纳米级高性能Nd2Fe14B/α-Fe复合磁体材料。
与快淬法制备的Nd9Dy0.4Fe80.24InNb0.36Co3B6的相比，所得纳米复合永磁体其矫顽力控制机理仍为成核机制，但其晶粒尺寸更小，具有较强的交换耦合强度，矫顽力、磁能积得到提升，磁性能显著提高，且制备过程更安全。
Claims (5)
1.一种液相激光烧蚀法制备钕铁硼复合永磁体的方法，其特征在于包括如下步骤：
1)配料阶段：按一定化学计量比称取一定量复合永磁体原材料粉末，经过充分研磨混合之后，将粉末压成块；
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：利用超声清洗剂将前驱体清洗15～30min，干燥后，放入烧杯的靶材支架上，装入异丙酮溶液没过前驱体5～10mm，将烧杯置于旋转转速为30r/min的旋转平台上，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10～20min，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3-5次，烘干之后，获得钕铁硼复合永磁体材料。
2.根据权利要求1所述的方法，步骤(1)所述的纳米复合永磁体化学式为Ndx1Fey1B/α-Fe，所述的粉末为纯度>99.5％的金属Nd、Dy、Tb、In、Nb、Fe、Co粉末，B用FeB为原料，其中FeB中B质量分数为19.83％；Nb用NbFe为原料，NbFe中Nb质量分数为66.3％；其余采用99.99％的高纯金属原料。所述的压成块的大小为直径10～20mm，厚度为2～5mm。
3.根据权利要求1所述的方法，步骤(2)所述的退火条件，温度为600～800℃，时间为0.1～1h。
4.根据权利要求1所述的方法，步骤(3)所述的激光器为纳秒固体激光器，激光频率为10Hz，波长为1064nm，脉宽为1～7ns，激光脉冲强度为100～350mJ/pulse，光斑直径为1～3mm，所述的清洗剂为色谱纯乙醇。
5.根据权利要求1所述的方法，步骤(4)所述的过滤，采用为离心机过滤，速度为5000～15000rpm。
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| US20150348685A1 (en) * | 2012-12-24 | 2015-12-03 | Beijing Zhong Ke San Huan Hi-Tech Co.,Ltd | Nd-Fe-B SINTERED MAGNET AND METHODS FOR MANUFACTURING THE SAME |
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