Zintl相Mg3X2(X=Sb, Bi)基晶体生长及热电性能研究进展

doi:10.15541/jim20220356

无机材料学报 ›› 2023, Vol. 38 ›› Issue (3): 270-279.DOI: 10.15541/jim20220356 CSTR: 32189.14.10.15541/jim20220356

Zintl相Mg₃X₂(X=Sb, Bi)基晶体生长及热电性能研究进展

林思琪¹^,²^,³(), 李艾燃⁴, 付晨光⁴, 李荣斌¹, 金敏¹^,³()

1.上海电机学院材料学院, 上海 201306
2.同济大学材料科学与工程学院, 上海201804
3.山东大学晶体材料国家重点实验室, 济南 250100
4.浙江大学材料科学与工程学院, 杭州 310027

收稿日期:2022-06-24 修回日期:2022-08-09 出版日期:2023-03-20 网络出版日期:2022-10-28
通讯作者: 金敏, 教授. E-mail: jmaish@aliyun.com
作者简介:林思琪(1992-), 女, 博士, 副教授. E-mail: linsiqi0811@163.com
基金资助:
国家自然科学基金(52001231);国家自然科学基金(52272006);上海市教委曙光计划

Crystal Growth and Thermoelectric Properties of Zintl Phase Mg₃X₂ (X=Sb, Bi) Based Materials: a Review

LIN Siqi¹^,²^,³(), LI Airan⁴, FU Chenguang⁴, LI Rongbing¹, JIN Min¹^,³()

1. College of Materials, Shanghai Dianji University, Shanghai 201306, China
2. School of Materials Science and Engineering, Tongji University, Shanghai 201804, China
3. State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100, China
4. School of Materials Science and Engineering, Zhejiang University, Hangzhou 310027, China

Received:2022-06-24 Revised:2022-08-09 Published:2023-03-20 Online:2022-10-28
Contact: JIN Min, professor. E-mail: jmaish@aliyun.com
About author:LIN Siqi (1992-), female, PhD, associate professor. E-mail: linsiqi0811@163.com
Supported by:
National Natural Science Foundation of China(52001231);National Natural Science Foundation of China(52272006);Shuguang Program of Shanghai Education Development Foundation and Shanghai Municipal Education Commission

摘要/Abstract

摘要：

Zintl相Mg₃X₂(X= Sb, Bi)基热电材料以其无毒性、价格低及性能高等优点而备受关注。与多晶相比, Mg₃X₂晶体在揭示材料本征热电性能、各向异性性质及电声输运调控策略等方面极具研究价值。本文系统归纳与总结近年Mg₃X₂基晶体的生长及热电性能发展现状。针对Mg₃X₂晶体生长过程中Mg元素易挥发和活泼金属性的难点, 多种技术如合适的温度冷却法、定向凝固法、助熔剂法、助熔剂坩埚下降法等被开发运用于生长Mg₃X₂晶体, 其中助熔剂坩埚下降法在获得大尺寸块状晶体方面更有竞争力。n型和p型Mg₃Sb₂晶体都呈现出各向异性的热电性能。调控晶体生长速度、Mg元素自补偿含量、杂质元素掺杂与固溶含量等手段, 都会影响Mg₃X₂晶体的电学性能和热学性能。目前p型和n型Mg₃Sb₂基晶体的最高ZT值可分别达到0.68和0.82。本文综述了Zintl相Mg₃X₂基晶体生长与热电性能的研究进展, 发现助熔剂坩埚下降法是制备大尺寸Mg₃X₂基晶体的关键, 通过元素掺杂及固溶方法调控载流子浓度和能带结构可以进一步提高Mg₃X₂基晶体性能。该生长方法和研究思路对将来Mg₃X₂基晶体制备与热电性能深入研究具有重要指导意义。

关键词: Zintl相, Mg₃X₂, 晶体生长, 热电性能, 综述

Abstract:

Zintl phase Mg₃X₂ (X=Sb, Bi) based thermoelectric materials have attracted much attention because of their non-toxic, low cost and high performance. Compared with polycrystalline materials, the Mg₃X₂ crystals are of great value in revealing material’s intrinsic and anisotropic thermoelectric properties, as well as providing effective strategies for enhancing electrical and thermal transport properties. Therefore, the recent progress of single crystal growth and thermoelectric properties for Mg₃X₂ crystals are systematically summarizes in this paper. Due to the volatility and causticity of Mg element, several different methods such as slow cooling method, directional solidification method, flux method, and flux Bridgman method are widely used for synthesizing Mg₃X₂ crystals, in which the flux Bridgman method is more competitive to prepare large size bulk crystals. Researchers found that both n-type and p-type Mg₃Sb₂ crystals show an anisotropy thermoelectric transport property. The crystal growth rate, the concentration of self-doped Mg element, the concentration of impurity doping or alloying elements have a great impact on both electrical and thermal transport properties for Mg₃Sb₂ crystals. So far, the p-type and n-type Mg₃Sb₂ crystals with ZT value of 0.68 and 0.82 are achieved, respectively. This paper reviews the recent progress of growth and thermoelectrics properties of Zintl phase Mg₃X₂-based crystals, revealing that the flux Bridgman method is the most effective method to produce large-sized Mg₃X₂-based crystals. Tuning chemical composition of Mg₃X₂-based crystal by doping and forming solid solution for optimal carrier concentration and band structure engineering is expected to further improve the thermoelectric performance of Mg₃X₂-based crystal. The above-mentioned growth method and research strategies provide a significant guidance for the in-depth understanding of the Mg₃X₂-based crystal in the future.

Key words: Zintl phase, Mg₃X₂, crystal growth, thermoelectric property, review

中图分类号:

TQ174

林思琪, 李艾燃, 付晨光, 李荣斌, 金敏. Zintl相Mg₃X₂(X=Sb, Bi)基晶体生长及热电性能研究进展[J]. 无机材料学报, 2023, 38(3): 270-279.

LIN Siqi, LI Airan, FU Chenguang, LI Rongbing, JIN Min. Crystal Growth and Thermoelectric Properties of Zintl Phase Mg₃X₂ (X=Sb, Bi) Based Materials: a Review[J]. Journal of Inorganic Materials, 2023, 38(3): 270-279.

图/表 8

图1 Mg3X2(X=Sb, Bi)晶体结构图[33]

Fig. 1 Crystal structure of Mg3X2 (X=Sb, Bi)[33]

图2 Mg3X2化合物相图[46-47]

Fig. 2 Phase diagram of Mg3X2 compounds[46-47] (a) Mg-Sb and (b) Mg-Bi binary phase diagram

图3 温度冷却法生长的Mg3Sb2晶体

Fig. 3 MgSb2 crystals grown by slow cooling method (a) XRD patterns of Mg3-xMnxSb2 crystal powder grown by slow cooling method; (b) XRD patterns of (001) cleavage plane; (c) Morphology of as grown Mg3-xMnxSb2 crystal; (d) SEM image of cleavage plane[48]; (e) Ag-doped Mg3Sb2 crystal grown by modified slow cooling method[50]

图4 定向凝固法生长Mg3Sb2晶体[51]

Fig. 4 MgSb2 crystals grown by directional solidification method[51] (a) Ag-doped Mg3Sb2 crystal growth diagram; (b) The as-grown crystal1. The graphite; 2. Raw materials; 3. Melting zone; 4. Graphite heater; 5. Induction coil; 6. Boron nitride baffle; 7. Solidified crystal; 8. Seed crystal

图5 助熔剂法生长Mg3Sb2-xBix晶体

Fig. 5 Mg3Sb2-xBix crystals grown by flux method (a) Sb flux grown Mg3Sb2[53]; (b) Te-doped Mg3Sb2 crystals[54]; (c) Mg flux grown Mg3Bi1.25Sb0.75 crystal[55]

图6 助熔剂法生长Mg3Sb2晶体[56]

Fig. 6 MgSb2 crystal grown by flux method[56] (a) Schematic diagram of Y-doped Mg3Sb2 crystal growth by flux Bridgman method; (b) As grown crystal; (c) Mg3Sb2 single crystal with the size of 8 mm×10 mm×25 mm

图7 Mg3Sb2-xBix晶体热电性能

Fig. 7 Thermoelectric properties of Mg3Sb2-xBix crystals (a) Thermoelectric properties of Mg3Sb2 crystals grown by modified temperature cooling method[50]; (b) Sb/Bi flux Bridgman method[56]; (c) Directional solidification method[51]; (d) Sb flux method[54]; (e) Mg flux method[55]

表1 不同方法生长Mg3X2晶体及热电性能研究结果统计

Table 1 Growth results of Mg3X2 crystal by different methods and their thermoelectric properties

Method	Composition	Type	Shape and size	ZT_max	Year	Ref.
Temperature cooling	Mn-doped Mg₃Sb₂	n	Flake, 6-7 mm	0.11 (//ab plane, 500 K)	2014	[48]
	Mg₃Sb_2-_xBi_x	p	Flake, 6-7 mm	0.006 (//ab plane, 300 K)	2015	[49]
	Ag-doped Mg₃Sb₂	p	Bulk, 3 mm×6 mm×10 mm	0.03 (//ab plane, 300 K) 0.12 (┴ab plane, 300 K)	2021	[50]
Flux method	Mg₃Sb₂ (Sb Flux)	p	Flake, 6-7 mm	-	2018	[53]
	Mg₃Bi₂ (Bi Flux)	p	Flake, 6-7 mm	-	2018	[53]
	Y-doped Mg₃Sb₂(Mg Flux)	n	Flake, 3-8 mm	-	2020	[55]
	Y-doped Mg₃Bi₂(Mg Flux)	n/p	Flake, 3-8 mm	-	2020	[55]
	Y-doped Mg₃Bi_1.25Sb_0.75(Mg Flux)	n	Flake, 3-10 mm	0.82 (//ab plane, 325 K)	2020	[55]
	Te-doped Mg₃Sb₂ (Sb Flux)	n	Flake, 5-10 mm	0.78 (//ab plane, 600 K)	2020	[54]
Directional solidification	Ag-doped Mg₃Sb₂	p	Ingot, ϕ 10 mm×50 mm	0.62 (//ab plane, 800 K) 0.68 (┴ab plane, 800 K)	2020	[51]
Flux Bridgman	Y-doped Mg₃Sb₂(Sb/Bi Flux)	n	Bulk, 8 mm×10 mm×25 mm	0.60 (//ab plane, 700 K) 0.48 (┴ab plane, 700 K)	2021	[56]

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Zintl相Mg₃X₂(X=Sb, Bi)基晶体生长及热电性能研究进展

Crystal Growth and Thermoelectric Properties of Zintl Phase Mg₃X₂ (X=Sb, Bi) Based Materials: a Review

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