CN114512326A - 一种高性能Pr基磁体的制备方法 - Google Patents

一种高性能Pr基磁体的制备方法 Download PDF

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CN114512326A
CN114512326A CN202210228458.7A CN202210228458A CN114512326A CN 114512326 A CN114512326 A CN 114512326A CN 202210228458 A CN202210228458 A CN 202210228458A CN 114512326 A CN114512326 A CN 114512326A
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泮敏翔
吴琼
杨杭福
俞能君
葛洪良
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China Jiliang University
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Abstract

本发明公开了一种高性能Pr基磁体的制备方法，属于磁性材料技术领域。该制备方法包括：采用熔体快淬法制备Pr‑Fe基合金薄带和PrCu低熔点合金薄带，并在氢气正压气氛下的高能球磨过程中加入一定比例的Fe3C粉末、纯Pr粉和正庚烷，实现Pr‑Fe基合金的歧化反应，并获得颗粒尺寸小于300 nm的混合粉末；将纳米混合粉末进行强磁场辅助下的热压和热变形技术制得压坯，随后将压坯进行激光加热技术下的热处理，实现Pr2Fe14C硬磁相的组装结合形成和扩散的均匀化，获得高性能的Pr基磁体。本发明方法工艺简单，成型容易，降低了成本，有利于高性能磁体在更多永磁器件中的应用。

Description

一种高性能Pr基磁体的制备方法
技术领域
本发明涉及磁性材料技术领域，尤其涉及一种高性能Pr基磁体的制备方法。
背景技术
作为一种重要的功能材料，磁性材料在现代社会里扮演着极为重要的角色。特别是永磁材料的生产和开发应用程度是现代国家经济发展的标志之一。Nd-Fe-B永磁材料具有较高的室温各向异性场(H A=7T) 和高的饱和磁极化强度(J s=1.6 T)，最大磁能积的理论值高达512 kJ/m3，被称为“磁王”，受到人们的普遍重视。另外，与 Nd2Fe14B磁体具有相同的晶体结构的RE2Fe14C（RE=Pr、Nd）也具有很好的内禀磁性。虽然RE2Fe14C的饱和磁化强度和居里温度比其硼化物略低，但是RE2Fe14C具有更高的磁晶各向异性，因此可以获得更大的矫顽力，具有代替包含重稀土Tb和Dy的Nd2Fe14B成为高矫顽力永磁体的潜力。
为此，本发明采用Pr2Fe14C相自组装合成生长和低熔点稀土元素相扩散制备高性能Pr2Fe14C永磁体的方式，在制备过程中，通过引入氢气正压气氛和正庚烷作为歧化辅助介质，实现Pr-Fe基合金的歧化反应，并在高能球磨的过程中，加入了一定粒度范围的Fe3C粉末和纯Pr粉，实现晶粒的细化；并在强磁场辅助下的热压和热变形及后续的激光下的热处理过程中，实现硬磁相的自组装合成和低熔点合金中稀土原子扩散的均匀化，从而显著提升Pr2Fe14C永磁体的矫顽力和磁能积。
发明内容
针对现有技术中存在的问题，本发明目的在于提供一种高性能Pr基磁体的制备方法。
本发明的高性能Pr基磁体的制备方法，包括如下步骤：
（1）采用熔体快淬法制备Pr-Fe基合金薄带，铜辊转速为5~40 m/s；其中，所述的Pr-Fe基合金为为按原子百分比的PraFebTM100-a-b，式中5≤a≤15，75≤b≤85，其余TM，TM为B，Ti，Co，Zr中的一种或几种；
（2）采用熔体快淬法制备按原子百分比的PrxCu100-x低熔点合金薄带，式中5≤x≤30，铜辊转速为5~25 m/s；
（3）将粒度范围为300~800目的Fe3C粉末和粒度范围为500~900目的纯Pr粉末与步骤（1）和步骤（2）获得的Pr-Fe基合金和PrCu低熔点合金按一定质量比例混合后放到高能球磨罐中，并加入10~30 mL的正庚烷作为歧化辅助介质，在氢气正压气氛下高能球磨1~15 h，实现Pr-Fe基合金的歧化反应，生成PrH2±x、Fe7C3和α-Fe相，最终获得颗粒尺寸小于300 nm并由Fe3C粉末、Pr粉末、Pr-Fe基粉体合金和PrCu低熔点粉体合金共同组成的混合粉末；
（4）将步骤（3）获得的纳米混合粉体进行强磁场辅助下的热压和热变形技术制得压坯；其中，所述强磁场辅助下的热压和热变形技术的磁场强度为3~7 T；热压温度为400~800 ℃，热压压力为150~500 MPa，热压时间为1~9 min；热变形温度为500~800 ℃，热变形压力为200~700 MPa，热变形时间为1~3 min，热变形量为65~85 %；
（5）将步骤（4）获得的压坯进行激光加热技术下的热处理，实现Pr2Fe14C硬磁相的组装结合形成和扩散的均匀化；所述激光加热技术的激光脉冲功率为1000~1500 W，光斑直接为1~5 mm，温度为600~850 ℃，激光脉冲持续时间为1~5 min。
进一步的，步骤（3）中所述的Pr-Fe基合金、PrCu低熔点合金、Fe3C粉末和Pr粉的质量比为1:0~0.1:0~0.1:0~0.1；所述的氢气正压气氛的正压强度为0.1~3 MPa。
与现有的技术相比，本发明具有如下优点和有益效果：本发明通过将Pr-Fe基合金、PrCu低熔点合金、Fe3C粉末和纯Pr粉按一定的比例在氢气正压气氛和正庚烷作为歧化辅助介质下进行高能球磨制备混合粉体，实现Pr-Fe基合金的歧化反应及各个粉末粒度的细化；并利用强磁场辅助下的热压和热变形及后续的激光下的热处理过程中，实现硬磁Pr2Fe14C相的自组装合成和低熔点合金中稀土原子向硬磁相Pr2Fe14C相扩散的均匀化，从而显著提升Pr2Fe14C永磁体的矫顽力和磁能积。
具体实施方式
下面将结合实施例对本发明做进一步的详细说明，但本发明并不仅仅局限于以下实施例。
实施例1
（1）采用熔体快淬法制备按原子百分比的Pr5Fe85B10合金薄带，铜辊转速为5 m/s；
（2）采用熔体快淬法制备按原子百分比的Pr5Cu95低熔点合金薄带，铜辊转速为5m/s；
（3）将Pr5Fe85B10合金、Pr5Cu95低熔点合金、粒度为300目的Fe3C粉末和粒度为900目的纯Pr粉末按质量比为1:0.03:0.09:0.03的比例混合后放到高能球磨罐中，并加入10 mL的正庚烷作为歧化辅助介质，在正压强度为0.1 MPa的氢气正压气氛下高能球磨1 h，实现Pr-Fe基合金的歧化反应，生成PrH2±x、Fe7C3和α-Fe相，最终获得颗粒尺寸小于280 nm并由Fe3C粉末、Pr粉末、Pr-Fe基粉体合金和PrCu低熔点粉体合金共同组成的混合粉末；
（4）将步骤（3）获得的纳米混合粉体进行强磁场辅助下的热压和热变形技术制得压坯；其中，所述强磁场辅助下的热压和热变形技术的磁场强度为3 T；热压温度为400 ℃，热压压力为150 MPa，热压时间为9 min；热变形温度为800 ℃，热变形压力为200 MPa，热变形时间为1 min，热变形量为85 %；
（5）将步骤（4）获得的压坯进行激光加热技术下的热处理，实现Pr2Fe14C硬磁相的组装结合形成和扩散的均匀化；所述激光加热技术的激光脉冲功率为1000 W，光斑直接为5mm，温度为850 ℃，激光脉冲持续时间为1 min，最终获得高性能Pr基磁体。
采用本发明制备的Pr基磁体经磁性能测试，剩磁为9.75 kG，矫顽力为17.9 kOe，磁能积为14.5 MGOe。
实施例2
（1）采用熔体快淬法制备按原子百分比的Pr10Fe80Ti10合金薄带，铜辊转速为25 m/s；
（2）采用熔体快淬法制备按原子百分比的Pr15Cu85低熔点合金薄带，铜辊转速为15m/s；
（3）将Pr10Fe80Ti10合金、Pr15Cu85低熔点合金、粒度为500目的Fe3C粉末和粒度为700目的纯Pr粉末按质量比为1:0.05:0.07:0.05的比例混合后放到高能球磨罐中，并加入20mL的正庚烷作为歧化辅助介质，在正压强度为2 MPa的氢气正压气氛下高能球磨7 h，实现Pr-Fe基合金的歧化反应，生成PrH2±x、Fe7C3和α-Fe相，最终获得颗粒尺寸小于200 nm并由Fe3C粉末、Pr粉末、Pr-Fe基粉体合金和PrCu低熔点粉体合金共同组成的混合粉末；
（4）将步骤（3）获得的纳米混合粉体进行强磁场辅助下的热压和热变形技术制得压坯；其中，所述强磁场辅助下的热压和热变形技术的磁场强度为5 T；热压温度为600 ℃，热压压力为300 MPa，热压时间为5 min；热变形温度为600 ℃，热变形压力为500 MPa，热变形时间为2 min，热变形量为75 %；
（5）将步骤（4）获得的压坯进行激光加热技术下的热处理，实现Pr2Fe14C硬磁相的组装结合形成和扩散的均匀化；所述激光加热技术的激光脉冲功率为1200 W，光斑直接为3mm，温度为750 ℃，激光脉冲持续时间为3 min，最终获得高性能Pr基磁体。
采用本发明制备的Pr基磁体经磁性能测试，剩磁为9.98 kG，矫顽力为19.7 kOe，磁能积为15.7 MGOe。
实施例3
（1）采用熔体快淬法制备按原子百分比的Pr15Fe82Co1.5Zr1.5合金薄带，铜辊转速为40 m/s；
（2）采用熔体快淬法制备按原子百分比的Pr30Cu70低熔点合金薄带，铜辊转速为25m/s；
（3）将Pr15Fe82Co1.5Zr1.5合金、Pr30Cu70低熔点合金、粒度为800目的Fe3C粉末和粒度为500目的纯Pr粉末按质量比为1:0.09:0.03:0.09的比例混合后放到高能球磨罐中，并加入30 mL的正庚烷作为歧化辅助介质，在正压强度为3 MPa的氢气正压气氛下高能球磨15h，实现Pr-Fe基合金的歧化反应，生成PrH2±x、Fe7C3和α-Fe相，最终获得颗粒尺寸小于150nm并由Fe3C粉末、Pr粉末、Pr-Fe基粉体合金和PrCu低熔点粉体合金共同组成的混合粉末；
（4）将步骤（3）获得的纳米混合粉体进行强磁场辅助下的热压和热变形技术制得压坯；其中，所述强磁场辅助下的热压和热变形技术的磁场强度为7 T；热压温度为800 ℃，热压压力为450 MPa，热压时间为3 min；热变形温度为500 ℃，热变形压力为700 MPa，热变形时间为3 min，热变形量为65 %；
（5）将步骤（4）获得的压坯进行激光加热技术下的热处理，实现Pr2Fe14C硬磁相的组装结合形成和扩散的均匀化；所述激光加热技术的激光脉冲功率为1500 W，光斑直接为1mm，温度为600 ℃，激光脉冲持续时间为5 min，最终获得高性能Pr基磁体。
采用本发明制备的Pr基磁体经磁性能测试，剩磁为10.99 kG，矫顽力为21.5 kOe，磁能积为16.6 MGOe。

Claims (2)

1.一种高性能Pr基磁体的制备方法，其特征在于包括如下步骤：
（1）采用熔体快淬法制备Pr-Fe基合金薄带，铜辊转速为5~40 m/s；其中，所述的Pr-Fe基合金为为按原子百分比的PraFebTM100-a-b，式中5≤a≤15，75≤b≤85，其余TM，TM为B，Ti，Co，Zr中的一种或几种；
（2）采用熔体快淬法制备按原子百分比的PrxCu100-x低熔点合金薄带，式中5≤x≤30，铜辊转速为5~25 m/s；
（3）将粒度范围为300~800目的Fe3C粉末和粒度范围为500~900目的纯Pr粉末与步骤（1）和步骤（2）获得的Pr-Fe基合金和PrCu低熔点合金按一定质量比例混合后放到高能球磨罐中，并加入10~30 mL的正庚烷作为歧化辅助介质，在氢气正压气氛下高能球磨1~15 h，实现Pr-Fe基合金的歧化反应，生成PrH2±x、Fe7C3和α-Fe相，最终获得颗粒尺寸小于300 nm并由Fe3C粉末、Pr粉末、Pr-Fe基粉体合金和PrCu低熔点粉体合金共同组成的混合粉末；
（4）将步骤（3）获得的纳米混合粉体进行强磁场辅助下的热压和热变形技术制得压坯；其中，所述强磁场辅助下的热压和热变形技术的磁场强度为3~7 T；热压温度为400~800℃，热压压力为150~500 MPa，热压时间为1~9 min；热变形温度为500~800 ℃，热变形压力为200~700 MPa，热变形时间为1~3 min，热变形量为65~85 %；
（5）将步骤（4）获得的压坯进行激光加热技术下的热处理，实现Pr2Fe14C硬磁相的组装结合形成和扩散的均匀化；所述激光加热技术的激光脉冲功率为1000~1500 W，光斑直接为1~5 mm，温度为600~850 ℃，激光脉冲持续时间为1~5 min。
2.根据权利要求1 所述的一种高性能Pr基磁体的制备方法，其特征在于：步骤（3）中所述的Pr-Fe基合金、PrCu低熔点合金、Fe3C粉末和Pr粉的质量比为1:0~0.1:0~0.1:0~0.1；所述的氢气正压气氛的正压强度为0.1~3 MPa。
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