高性能Sm2Fe17N x 粉体制备的研究进展

doi:10.11901/1005.3093.2021.279

材料研究学报

2022, Vol. 36

Issue (5): 321-331 DOI: 10.11901/1005.3093.2021.279

综述

本期目录 | 过刊浏览

高性能Sm₂Fe₁₇N _x 粉体制备的研究进展

何颖¹, 李超群¹, 陈小立¹, 龙芝梅¹, 赖嘉琪¹, 邵斌¹^,²(

), 马毅龙¹^,²(

), 陈登明¹^,², 董季玲¹^,²

^1.重庆科技学院冶金与材料工程学院重庆 401331
^2.纳微复合材料与器件重庆市重点实验室重庆 401331

Recent Development for Preparation Processes of Sm₂Fe₁₇N _x Powders with High Magnetic Properties

HE Ying¹, LI Chaoqun¹, CHEN Xiaoli¹, LONG Zhimei¹, LAI Jiaqi¹, SHAO Bin¹^,²(

), MA Yilong¹^,²(

), CHEN Dengming¹^,², DONG Jiling¹^,²

^1.School of Metallurgy and Material Engineering, Chongqing University of Science and Technology, Chongqing 401331, China
^2.Chongqing Key Laboratory of Nano-Micro Composites and Devices, Chongqing 401331, China

引用本文:

何颖, 李超群, 陈小立, 龙芝梅, 赖嘉琪, 邵斌, 马毅龙, 陈登明, 董季玲. 高性能Sm₂Fe₁₇N _x 粉体制备的研究进展[J]. 材料研究学报, 2022, 36(5): 321-331.
Ying HE, Chaoqun LI, Xiaoli CHEN, Zhimei LONG, Jiaqi LAI, Bin SHAO, Yilong MA, Dengming CHEN, Jiling DONG. Recent Development for Preparation Processes of Sm₂Fe₁₇N _x Powders with High Magnetic Properties[J]. Chinese Journal of Materials Research, 2022, 36(5): 321-331.

全文: PDF(12208 KB) HTML

摘要:

新能源汽车的高速发展,需要能稳定工作在120℃~200℃温度区间的永磁材料。居里温度为476℃、各向异性场为14.7 T的Sm₂Fe₁₇N₃,具有优良的本征磁性能,可应用在这个温度区间。为了提高Sm₂Fe₁₇N₃粉体的磁性能,必须将颗粒的粒径减小到临界单畴尺寸以实现高各向异性场；同时,还要避免颗粒尺寸减小产生的表面氧化,以保证高剩磁和最大磁能积。粉体破碎、机械合金化、甩带、薄带连铸、还原扩散以及表面镀覆等多种制备工艺,可用于制备高性能Sm₂Fe₁₇N₃。目前,实验室制备的Sm₂Fe₁₇N₃粉体的矫顽力和最大磁能积已经达到28.1 kOe和43.6 MGOe。本文评述近年来Sm₂Fe₁₇N₃粉体制备的研究成果,包括对制备机理的系统总结并提出仍待解决的关键问题：Sm₂Fe₁₇N₃粉体的矫顽力、剩磁等与其颗粒尺寸的量化规律以及与颗粒磁畴结构的关联机制；对NH₃/H₂混合气体中H₂对提高氮化效率的作用机制仍需探索；进一步开发在低氧环境下的颗粒粒径均匀化、控制形貌的二次破碎技术；对于还原扩散法,开发适合规模化应用的新前驱体及其制备方法以及快速去除钙副产物的水洗技术等。

关键词 ：评述, 金属材料, Sm₂Fe₁₇N _x, 永磁, 制备方法

Abstract：

The rapid development of new energy vehicles requires permanent magnet materials that can work stably in the temperature range of 120℃~200℃. Sm₂Fe₁₇N₃ with Curie temperature of 476℃ and anisotropic field of 14.7 T has excellent intrinsic magnetic properties, and can be used in this temperature range. In order to improve the magnetic properties of Sm₂Fe₁₇N₃ powder, the particle size of which should be reduced to the critical size close to a single domain, so that to gain high anisotropic field; Meanwhile, surface oxidation caused by particle size reduction should be avoided to ensure high remanence magnetism and maximum magnetic energy product. High performance Sm₂Fe₁₇N₃ can be prepared by powder crushing, mechanical alloying, strip casting, thin strip continuous casting, reduction diffusion and surface plating. At the present, the coercivity and maximum magnetic energy product of Sm₂Fe₁₇N₃ powder prepared in laboratory have reached 28.1 kOe and 43.6 MGOe respectively. In this paper, the research results on the preparation of Sm₂Fe₁₇N₃ powders in recent years are reviewed, including preparation methods and the relevant mechanism, and key problems that remain to be solved, namely the relation of the coercivity and remanence of Sm₂Fe₁₇N₃ powder with the particle size, as well as with the particle magnetic domain structure；the mechanism related with the enhanced effect H₂ within the gas mixture NH₃/H₂ on the nitriding efficiency of the powder still needs to be revealed; further the secondary crushing technique in low oxygen pressures, which can prepare particles with uniform distribution of particle size, while adjust their morphology, remains to be developed; for the present reduction diffusion method, new precursors, and their preparation methods suitable for massive production, and water washing technology for rapid removal of calcium by-products were also needed to develop.

Key words： review metallic material Sm₂Fe₁₇N _x magnetic properties preparation methods

收稿日期: 2021-04-29

ZTFLH:

TM27

基金资助:重庆科技学院研究生创新计划(YKJCX2020215);重庆市自然科学基金(cstc2019jcyj-msxmX0162);重庆市教委科学技术研究重大项目(KJZD-M201801501);重庆市高校创新研究团队(CXQT19031)

作者简介: 何颖,女,1995年生,硕士

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表1 Nd2Fe14B和Sm2Fe17N3的磁性能[16~19]

图1 Sm2Fe17N3和(NdDy)FeB的(BH)max与工作温度的关系[20]

图2 Sm2Fe17N x 粉末球磨前后的比特花样、矫顽力以及含氧量随球磨时间的变化[35]

图3 在低温和室温下球磨不同时间Sm2Fe17N x 粉体的XRD谱、SEM照片和磁滞回线[38]

图4 用球磨结合等离子放电技术机械合金化制备Sm2Fe17的示意图和氮化后Sm2Fe17N x 样品的退磁曲线[44]

图5 用薄带连铸结合球磨破碎技术制备Sm2(FeCu)17N x

图6 还原扩散法制备流程、还原扩散后(未氮化)块体照片、直接氮化后的照片以及水洗后Sm2Fe17N3粉体的SEM照片[50]

图7 分别用溶胶凝胶法[29]、共沉淀法[10]、水热法[54]和溶剂热解法[56]制备前驱体,再进行还原扩散后的Sm2Fe17N x 的SEM照片和磁化曲线

图8 还原扩散法的新制备流程(缓慢氧化处理)以及样品的SR-XRD谱和退磁曲线[11]

图9 氮原子扩散机制和由Sm2Fe17N x (NP, x<3)向Sm2Fe17N3(FN)相转变引起的晶粒生长机制下的氮元素分布示意图[62]

图10 Sm2Fe17N x /Sm2(Fe,Mn)17N x 核壳粉的制备流程图和示意图、Mn扩散Sm-Fe粉末的截面扫描电镜和元素映射图、Mn扩散Sm-Fe-N核壳粉、无Mn扩散Sm-Fe-N粉热处理前后的退磁曲线[63]以及锌包覆Sm2Fe17N3粉体矫顽力随锌层平均厚度的增加速率[66]

表2 用不同方法制备Sm2Fe17N x 的氮化条件和性能

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