M位与A位双固溶MAX相的磁学性能研究

doi:10.15541/jim20210126

无机材料学报 ›› 2021, Vol. 36 ›› Issue (12): 1247-1255.DOI: 10.15541/jim20210126

所属专题： MXene材料专辑(2020~2021)；【信息功能】Max层状材料、MXene及其他二维材料

M位与A位双固溶MAX相的磁学性能研究

张霄¹^,²^,³(), 李友兵²^,³, 陈科²^,³, 丁浩明²^,³, 陈露²^,³, 李勉²^,³, 史蓉蓉¹(), 柴之芳²^,³, 黄庆²^,³()

1.兰州大学物理科学与技术学院, 磁学与磁性材料教育部重点实验室, 光转换材料与技术国家地方联合工程实验室, 兰州 730000
2.中国科学院宁波材料技术与工程研究所, 先进能源材料工程实验室, 宁波 315201
3.宁波材料所杭州湾研究院, 宁波 315336

收稿日期:2021-03-03 修回日期:2021-03-24 出版日期:2021-12-20 网络出版日期:2021-06-01
通讯作者: 史蓉蓉, 副教授. E-mail: shirr@lzu.edu.cn;黄庆, 研究员. E-mail: huangqing@nimte.ac.cn
作者简介:张霄(1996-), 男, 硕士研究生. E-mail: zhangxiao18@lzu.edu.cn
基金资助:
国家自然科学基金(21671195);国家自然科学基金(51902319);国家自然科学基金(91426304);中国博士后科学基金(2020M680082);中国科学院国际伙伴计划(174433KYSB20190019);浙江省领军型创新创业团队(2019R01003)

Tailoring MAX Phase Magnetic Property Based on M-site and A-site Double Solid Solution

ZHANG Xiao¹^,²^,³(), LI Youbing²^,³, CHEN Ke²^,³, DING Haoming²^,³, CHEN Lu²^,³, LI Mian²^,³, SHI Rongrong¹(), CHAI Zhifang²^,³, HUANG Qing²^,³()

1. State and Local Joint Engineering Laboratory of Light-conversion Materials and Technology, Key Laboratory for Magnetism and Magnetic Materials of the Ministry of Education, School of Physical Science and Technology, Lanzhou University, Lanzhou 730000, China
2. Engineering Laboratory of Advanced Energy Materials, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
3. Qianwan Institute of CNiTECH, Ningbo 315336, China

Received:2021-03-03 Revised:2021-03-24 Published:2021-12-20 Online:2021-06-01
Contact: SHI Rongrong, associate professor. E-mail: shirr@lzu.edu.cn;HUANG Qing, professor. E-mail: huangqing@nimte.ac.cn
About author:ZHANG Xiao(1996-), male, Master candidate. E-mail: zhangxiao18@lzu.edu.cn
Supported by:
National Natural Science Foundation of China(21671195);National Natural Science Foundation of China(51902319);National Natural Science Foundation of China(91426304);China Postdoctoral Science Foundation(2020M680082);International Partnership Program of Chinese Academy of Sciences(174433KYSB20190019);Leading Innovative and Entrepreneur Team Introduction Program of Zhejiang(2019R01003)

摘要/Abstract

摘要：

三元层状化合物MAX相兼具金属与陶瓷优良的力学性质, 通常被认为是一类高安全结构材料。有研究显示, 通过熔盐法可以将副族元素插入到MAX相A位层间, 获得具有铁磁性能的V₂(Sn, A)C (A =Fe、Co、Ni和Mn)材料。因而, 如何构建新的MAX相结构并对实现其磁性调控备受关注。本研究通过MAX相M位和A位双固溶的方式设计了四种新型MAX相(V, Nb)₂(Sn, A)C (A =Fe、Co、Ni和Mn)。XRD、SEM、EDS结合TEM分析证实了上述新相的合成。超导量子磁强计(Superconducting quantum interference device magnetometer, SQUID)测试磁学性能发现, M位固溶后的MAX相的居里温度与其四方率(c/a)、元素组成有关。(V, Nb)₂(Sn, Fe)C、(V, Nb)₂(Sn, Ni)C、(V, Nb)₂(Sn, Mn)C相较于M位固溶Nb元素之前的V₂(Sn, A)C相, 其矫顽力H_c和剩余磁化强度M_r减小, 饱和磁化强度M_s增大。而V₂(Sn, Co)C在M位固溶Nb元素之后磁性变化均与前述MAX相相反。通过以上结果, 揭示了M/A位双固溶对MAX相磁性的影响规律, 为调控MAX相磁性提供了新的思路。

关键词: MAX相, 双固溶, 磁性

Abstract:

The three-dimensional layered compound MAX phase has excellent mechanical property of both metals and ceramics, which is generally considered as a kind of high safety structural materials. In recent reports, V₂(Sn, A)C (A = Fe, Co, Ni and Mn) materials showed that antiferromagnetic property can be obtained by inserting the subgroup elements into A layer of MAX phase by molten salt method. However, how to further regulate magnetic properties of MAX phase through design of its crystal structure has attracted the attention of scholars in the field of spintronics and other fields. In this work, four new MAX phases of (V, Nb)₂(Sn, A)C (A = Fe, Co, Ni and Mn) were synthesized based on M/A double solid solution by molten salt method, and proved to be synthesized successfully. Magnetic property of the MAX phases was checked by SQUID (superconducting quantum interference device magnetometer). It is found that the change of Curie temperature is correlated with tetragonal ratio (c/a) and elemental composition. Changes of lattice parameters, tetragonal rate and magnetic results before and after introducing Nb element into M site were further compared. Besides, the H_c and M_r of (V, Nb)₂(Sn, Fe)C, (V, Nb)₂(Sn, Ni)C, and (V, Nb)₂(Sn, Mn)C decreased and the M_r increased compared with V₂(Sn, A)C (A = Fe, Ni, Mn) before introducing Nb element into M site. All these results were opposite after introducing Nb element into M site of V₂(Sn, Co)C which reveals the influence of M/A-site doble solid solution to the magnetic property of MAX phase, and provides a new way for tailoring magnetic property of MAX phase.

Key words: MAX phase, double solid solution, magnetic property

中图分类号:

TQ174

张霄, 李友兵, 陈科, 丁浩明, 陈露, 李勉, 史蓉蓉, 柴之芳, 黄庆. M位与A位双固溶MAX相的磁学性能研究[J]. 无机材料学报, 2021, 36(12): 1247-1255.

ZHANG Xiao, LI Youbing, CHEN Ke, DING Haoming, CHEN Lu, LI Mian, SHI Rongrong, CHAI Zhifang, HUANG Qing. Tailoring MAX Phase Magnetic Property Based on M-site and A-site Double Solid Solution[J]. Journal of Inorganic Materials, 2021, 36(12): 1247-1255.

图/表 6

图1 酸处理后的(V, Nb)2(Sn, Fe)C表征结果

Fig. 1 Characterization results of (V, Nb)2(Sn, Fe)C after acid treatment (a) XRD pattern; (b) SEM image; (c) Corresponding energy-dispersive spectroscopy analysis; (d) Elemental mapping scanning on one particle; (e) Selected area electron diffraction pattern, showing the electron beam being paralleled to the [1$\bar{1}$00] direction; (f) HR-TEM image

图2 (a) (V, Nb)2(Sn, Co)C、(c) (V, Nb)2(Sn, Ni)C和(e) (V, Nb)2(Sn, Mn)C酸处理后的XRD谱图;(b) (V, Nb)2(Sn, Co)C、(d) (V, Nb)2(Sn, Ni)C、(f) (V, Nb)2(Sn, Mn)C元素分布图

Fig. 2 XRD patterns of (a) (V, Nb)2(Sn, Co)C, (c) (V, Nb)2(Sn, Ni)C, and (e) (V, Nb)2(Sn, Mn)C after acid treatment; SEM-EDS elemental mappings of (b) (V, Nb)2(Sn, Co)C, (d) (V, Nb)2(Sn, Ni)C, and (f) (V, Nb)2(Sn, Mn)C after acid treatment

表1 晶格参数和MAX相中元素的原子百分比

Table 1 Lattice parameters and atomic percentage of element in MAX phases

MAX phase	Lattice parameter			Element percentage/%				Nb element in M site/%	Magnetic element in A site/%
MAX phase	a/nm	c/nm	c/a	V	Nb	Sn	A	Nb element in M site/%	Magnetic element in A site/%
V₂(Sn, Fe)C^[23]	0.2984	1.3345	4.4718	66.84	-	22.05	11.11	-	33.50
(V, Nb)₂(Sn, Fe)C	0.3014	1.3447	4.4622	54.32	13.38	25.03	7.27	19.76	22.51
V₂(Sn, Co)C^[23]	0.2989	1.3409	4.4864	66.36	-	22.44	11.19	-	33.28
(V, Nb)₂(Sn, Co)C	0.3016	1.3419	4.4493	56.41	11.23	24.60	7.76	16.60	23.98
V₂(Sn, Ni)C^[23]	0.2985	1.3357	4.4751	67.47	-	24.36	8.16	-	25.10
(V, Nb)₂(Sn, Ni)C	0.3021	1.3413	4.4402	56.87	13.00	21.66	8.47	18.61	28.10
V₂(Sn, Mn)C^[23]	0.2982	1.3403	4.4941	66.19	-	23.07	10.74	-	31.76
(V, Nb)₂(Sn, Mn)C	0.3026	1.3509	4.4646	57.10	10.84	23.50	8.56	15.96	26.70

图3 在0.1 T下, V2(Sn, A)C和(V, Nb)2(Sn, A)C (A = Fe, Co, Ni和Mn)在2~100 K范围内随温度变化的磁化M-T曲线

Fig. 3 Temperature dependent magnetization M-T curves for (a) V2(Sn, A)C and (b) V2(Sn, A)C (A = Fe, Co, Ni and Mn) at 0.1 T in the range of 2-100 K

图4 V2(Sn, A)C和(V, Nb)2(Sn, A)C(A=Fe、Co、Ni和Mn)在-1~1 T范围内的磁滞回线

Fig. 4 Magnetic hysteresis loops of V2(Sn, A)C and V2(Sn, A)C (A=Fe, Co, Ni and Mn) at different temperatures in the range from -1 to 1 T, respectively Colourful figures are available on website

表2 V2(Sn, A)C与(V, Nb)2(Sn, A)C(A = Fe、Co、Ni和Mn)的磁性参数

Table 2 Magnetic parameters of V2(Sn, A)C and (V, Nb)2(Sn, A)C (A = Fe, Co, Ni and Mn)

MAX phase	T_C	2 K			20 K			40 K
MAX phase	T_C	H_c	M_r	M_s	H_c	M_r	M_s	H_c	M_r	M_s
V₂(Sn, Fe)C	63	458	0.59	1.73	305	0.42	1.53	152	0.18	1.08
(V, Nb)₂(Sn, Fe)C	63	238	0.48	1.79	174	0.37	1.67	73	0.14	1.24
V₂(Sn, Co)C	66	314	0.34	1.19	224	0.26	1.05	113	0.12	0.79
(V, Nb)₂(Sn, Co)C	53	378	0.49	1.11	240	0.33	1.00	134	0.17	0.71
V₂(Sn, Ni)C	60	276	0.30	1.54	191	0.23	1.42	94	0.10	1.12
(V, Nb)₂(Sn, Ni)C	53	140	0.29	2.07	96	0.19	1.83	45	0.07	1.34
V₂(Sn, Mn)C	56	780	0.26	0.98	545	0.21	0.84	206	0.07	0.63
(V, Nb)₂(Sn, Mn)C	57	117	0.06	0.97	75	0.04	0.90	32	0.01	0.67

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M位与A位双固溶MAX相的磁学性能研究

Tailoring MAX Phase Magnetic Property Based on M-site and A-site Double Solid Solution

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