拓扑半金属及磁性拓扑材料的单晶生长

王欢; 何春娟; 徐升; 王义炎; 曾祥雨; 林浚发; 王小艳; 巩静; 马小平; 韩坤; 王乙婷; 夏天龙

doi:10.7498/aps.72.20221574

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摘要

拓扑材料因具有新奇物理特性受到广泛关注, 这些材料一方面为基础物理研究提供了新的平台, 另一方面在以拓扑物理为基础发展的器件研究方向上展现出潜在应用价值. 凝聚态领域对于拓扑材料相关物理问题的研究主要通过两种方式开展: 一是在已知的拓扑材料中不断挖掘新的实验现象和物理问题; 二是不断预言和探索发现新型拓扑材料体系并开展合成. 无论哪种方式, 高质量单晶的获得都至关重要, 它为角分辨光电子能谱、扫描隧道显微谱和磁场下的量子振荡等实验研究提供了前提保障. 本文总结了拓扑材料的分类和发展, 基于本研究组近些年开展的工作介绍了助溶剂法、气相输运法这两种拓扑材料单晶生长中常用的方法, 并详细介绍了拓扑物性研究领域几类典型的拓扑材料及其生长方法, 如拓扑绝缘体/拓扑半金属、高陈数手性拓扑半金属和磁性拓扑材料等.

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Abstract

Topological materials have attracted much attention due to their novel physical properties. These materials can not only serve as a platform for studying the fundamental physics, but also demonstrate a significant potential application in electronics, and they are studied usually in two ways. One is to constantly explore new experimental phenomena and physical problems in existing topological materials, and the other is to predict and discover new topological material systems and carry out synthesis for further studies. In a word, high-quality crystals are very important for studying quantum oscillations, angle resolved photoemission spectra or scanning tunneling microscopy. In this work, the classifications and developments of topological materials, including topological insulators, topological semimetals, and magnetic topological materials, are introduced. As usually employed growth methods in growing topological materials, flux and vapour transport methods are introduced in detail. Other growth methods, such as Bridgman, float-zone, vapour deposition and molecular beam epitaxy methods, are also briefly mentioned. Then the details about the crystal growth of some typical topological materials, including topological insulators/semimetals, high Chern number chiral topological semimetals and magnetic topological materials, are elaborated. Meanwhile, the identification of crystal quality is also briefly introduced, including the analysis of crystal composition and structure, which are greatly important.

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作者及机构信息

1.
中国人民大学物理系, 北京　100872

2.
中国人民大学, 光电功能材料与微纳器件北京市重点实验室, 北京　100872

3.
浙江大学物理学系, 浙江省量子技术与器件重点实验室, 杭州　310027

4.
安徽大学物质科学与信息技术研究院, 合肥　230601

5.
中国人民大学, 中子散射重点实验室, 北京　100872

通信作者: 夏天龙, tlxia@ruc.edu.cn

基金项目: 国家重点研发计划(批准号: 2019YFA0308602)、国家自然科学基金(批准号: 12074425, 11874422)、中央高校基本科研业务费(批准号: 18XNLG14, 19XNLG18)和中国人民大学2020年度拔尖创新人才培育计划资助的课题

Authors and contacts

1.
Department of Physics, Renmin University of China, Beijing 100872, China

2.
Beijing Key Laboratory of Opto-electronic Functional Materials & Micro-nano Devices of Beijing, Renmin University of China, Beijing 100872, China

3.
Key Laboratory of Quantum Technology and Device of Zhejiang Province , Department of Physics, Zhejiang University, Hangzhou 310027, China

4.
Institute of Physical Science and Information Technology, Anhui University, Hefei 230601, China

5.
Key Laboratory for Neutron Scattering, Renmin University of China, Beijing 100872, China

Corresponding author: Xia Tian-Long, tlxia@ruc.edu.cn

Funds: Project supported by the National Key R&D Program of China (Grant No. 2019YFA0308602), the National Natural Science Foundation of China (Grant Nos. 12074425, 11874422), the Fundamental Research Fund for the Central Universities, China (Grant Nos. 18XNLG14, 19XNLG18), and the Outstanding Innovative Talents Cultivation Funded Programs 2020 of Renmin University of China

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施引文献

图 1 Ba-Ga元素二元相图^[143], 其中插图为自助溶方法生长的BaGa₂及BaGa₄单晶

Fig. 1. Ba-Ga binary phase diagram. Insets are typical grown single crystal of BaGa₂ and BaGa₄, respectively

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图 2 Pt-Bi元素二元相图^[148], 其中插图为所生长的不同结构的PtBi₂单晶

Fig. 2. Pt-Bi binary phase diagram. Insets are typical grown single crystal of PtBi₂ with different structures

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图 3 (a) 常用石英管类型; (b) 常用石英堵头与坩埚类型; (c) 封管后的样品离心前后对比示意图

Fig. 3. (a) Different types of quartz tube frequently used; (b) different types of quartz plug and crucible frequently used; (c) sealed sample before and after centrifugation

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图 4 物理气相输运以及化学气相输运过程示意图, 以(T(S) > T(C)) 为例

Fig. 4. Physical vapour transport and chemical vapour transport. Take the case (T(S) > T(C)) as an example

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图 5 Pd-Te元素二元相图^[156], 插图为生长出的PdTe₂单晶

Fig. 5. Pd-Te binary phase diagram. Inset is the typical grown single crystal of PdTe₂

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图 6 (a) Cd-As元素二元相图^[164]; (b) 助溶剂方法生长出的单晶; (c) 气相输运方法生长的单晶

Fig. 6. (a) Cd-As binary phase diagram; (b) the single crystal grown from the flux method; (c) the single crystal grown from the vapour transport method

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图 7 通过气相输运方法得到的(a) NbAs₂和(b) TaAs₂单晶样品

Fig. 7. Single crystals of (a) NbAs₂ and (b) TaAs₂ grown from the vapour transport method

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图 8 助溶剂方法生长出的(a) RuAs₂, (b) IrAs₂, (c) CoAs₂单晶

Fig. 8. Single crystals of (a) RuAs₂, (b) IrAs₂ and (c) CoAs₂ grown by flux method

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图 9 (a) YSb, (b) TmSb, (c) HoSb, (d) DyBi单晶图片

Fig. 9. Photos of single crystal (a) YSb, (b) TmSb, (c) HoSb and (d) DyBi

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图 10 (a) Co-Te^[177]和(b) Si-Te^[178]二元相图; (c), (d) 通过化学气相输运方法得到的CoSi单晶; (e) 助溶剂方法生长的CoSi单晶

Fig. 10. Binary phase diagram of (a) Co-Te^[177] and (b) Si-Te^[178]. The single crystal of CoSi grown from the vapour transport (c), (d) and flux method (e)

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图 11 (a) Co-Sb^[179], (b) Sb-Si^[180], (c) Co-Sn^[181] 与(d) Si-Sn^[182]元素二元相图. (b)中插图与 (d)中插图分别为用Sb和Sn作为助溶剂生长的CoSi单晶

Fig. 11. (a) Co-Sb^[179], (b) Sb-Si^[180], (c) Co-Sn^[181] and (d) Si-Sn^[182] binary phase diagram. Insets in panels (b) and (d) are the single crystal of CoSi grown from the Sb and Sn flux

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图 12 (a) Bi-Rh^[183]及(b) Bi-Sn^[184]元素的二元相图, 插图为典型的RhSn单晶; (c) 同一块单晶中不同晶面的单晶XRD衍射图谱

Fig. 12. (a) Bi-Rh^[183] and (b) Bi-Sn^[184] binary phase diagram. Inset is the single crystal of RhSn grown from flux method. (c) Single-crystal XRD pattern of RhSn with different crystal faces

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图 13 (a) Bi-Pt^[148]以及(b) Bi-Ga^[185]元素的二元相图, 插图为助溶剂方法生长出的PtGa单晶

Fig. 13. (a) Pt-Bi^[148] and (b) Bi-Ga^[185] binary phase diagram. Insets are the single crystals of PtGa grown from flux method

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图 14 (a) Bi-Pd^[186]以及(b) Bi-Ga^[185]元素的二元相图; (c), (d) 不同晶面的单晶XRD衍射图谱

Fig. 14. (a) Bi-Pd^[186] and (b) Bi-Ga^[185] binary phase diagram; (c), (d) single-crystal XRD patterns of PdGa with different crystal faces

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图 15 (a) YbMnSb₂与 (b) EuMnSb₂单晶照片及单晶X射线衍射谱图

Fig. 15. Photos and XRD sprctras of single crystal (a) YbMnSb₂ and (b) EuMnSb₂

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图 16 (a) Al-Eu^[200]以及(b) Al-B^[201]元素二元相图; (c), (d) 典型的EuB₆单晶样品

Fig. 16. (a) Al-Eu^[200] and (b) Al-B^[201] binary phase diagram; (c), (d) typical grown single crystals of EuB₆

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图 17 (a) Al-Sm^[203]以及(b) Al-B^[201]元素二元相图, 插图为典型的SmB₆单晶样品

Fig. 17. (a) Al-Sm^[203] and (b) Al-B^[201] binary phase diagram. Insets are typical grown single crystals of SmB₆

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图 18 (a) Co₃Sn₂S₂与 (b) Co₃In₂S₂单晶样品

Fig. 18. Single crystals of (a) Co₃Sn₂S₂ and (b) Co₃In₂S₂

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图 19 (a) Fe-Sn^[209]元素二元相图, 插图为自助溶剂方法生长的Fe₃Sn₂单晶样品; (b) 气相输运方法生长的Fe₃Sn₂单晶样品

Fig. 19. (a) Fe-Sn^[209] binary phase diagram. Inset is the single crystal of Fe₃Sn₂ grown from the flux method. (b) The single crystals grown from the vapour transport

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图 20 (a) MnBi₂Te₄, (b) MnBi₄Te₇, (c) MnBi₆Te₁₀与(d) MnBi₈Te₁₃的晶体图以及相应的单晶X射线衍射图谱

Fig. 20. Single-crystal XRD patterns of (a) MnBi₂Te₄, (b) MnBi₄Te₇, (c) MnBi₆Te₁₀ and (d) MnBi₈Te₁₃. Insets are corresponding photos of single crystals

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图 21 (a) Eu-In^[229]元素二元相图; (b) As-In^[230]元素二元相图, 其中插图为生长的EuIn₂As₂单晶

Fig. 21. (a) Eu-In^[229] and (b) As-In^[230] binary phase diagram. Inset is the grown single crystals

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表 1 常用的金属助溶剂性质

Table 1. Properties of the frequently-used fluxes.

	熔点/℃	沸点/℃	可溶于酸或碱溶液	密度/(g·cm^-3)	毒性
Al	660.3	2327	硫酸/硝酸/盐酸/氢氧化钠/氢氧化钾	2.70	无
Ga	29.8	2400	盐酸/硫酸	5.90	无
In	156.6	2000	硝酸/盐酸/硫酸	7.31	无
Sn	231.9	2270	盐酸/硝酸/碱溶液	7.28	无
Pb	327.5	1740	硫酸/硝酸/有机酸溶液/碱溶液	11.34	有
Sb	630.6	1635	硫酸	6.69	无
Bi	271.3	1500	硝酸	9.78	无
Te	449.5	989.8	硝酸/盐酸/氢氧化钾	6.24	无
Cd	321.2	765	盐酸	8.65	有

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表 2 常用的输运剂性质

Table 2. Properties of the frequently-used transport agents

	熔点/℃	沸点/℃	稳定性	可溶于溶液	形貌	储存
I₂	113	184	易挥发/易升华	乙醇	紫红色颗粒	密封干燥
TeCl₄	224	380	易潮解	水/盐酸	白色粉末	密封干燥
BiCl₃	230	447	易潮解	水/盐酸	白色粉末	密封干燥
BiBr₃	218	441	易潮解	水/稀盐酸/丙酮	黄色粉末	密封干燥
TeBr₄	380	420	易潮解	水/氢氧化钠	黄色粉末	避光/密封
SnI₄	144.5	364	/	乙醇	橘黄色粉末	密封干燥
TeI₄	280	118 (升华点)	灼热易分解	乙醇/丙酮	灰色粉末	密封干燥

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表 3 不同生长方法的优缺点及适用范围

Table 3. Advantages and disadvantages of different growth methods and their application scope

	优点	缺点	适用范围
熔融重结晶法	1. 不需要加入其他试剂如助溶剂或输运剂, 损耗少且不引入杂质; 2. 不需要额外处理其他溶剂的分离或回收, 操作简单.	适用性不强	适合生长具有低熔点的目标材料
助溶剂法	1. 适用性强, 几乎对于所有材料只要找到合适的助溶剂都可以将其以单晶形式生长出来; 2. 生长温度低, 适合熔点很高的化合物; 3. 生长出的晶体均匀完整.	1. 生长周期长; 2. 许多助溶剂都有不同程度的毒性处理后的助溶剂或含有助溶剂的溶液具有腐蚀性还会产生污染, 要做好分类并小心处理; 3. 使用坩埚, 可能会影响品体成核与生长取向.	适合生长本身熔点较高的化合物
气相输运法	1. 可以实现常压下难以合成的化合物; 2. 可以合成难以通过固-固, 固-液反应合成的化合物; 3. 温度调节灵活, 可以直接调控晶体生长时所需的应力, 饱和度等参量, 进而影响晶体的生长速度.	1. 产量较低; 2. 需要精准掌控输运剂的浓度和低沸点反应物的总量, 否则容易因为管内压强过大造成爆管; 3. 有些气相输运法需要通惰性气体或氢气, 操作复杂, 有一定的危险; 4. 管壁会限制晶体生长方向, 与管壁接触的晶面呈曲面.	适合生长反应物中沸点较低的化合物或其它难以通过固-固、固-液合成的化合物

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拓扑半金属及磁性拓扑材料的单晶生长

1. 中国人民大学物理系, 北京　100872

2. 中国人民大学, 光电功能材料与微纳器件北京市重点实验室, 北京　100872

3. 浙江大学物理学系, 浙江省量子技术与器件重点实验室, 杭州　310027

4. 安徽大学物质科学与信息技术研究院, 合肥　230601

5. 中国人民大学, 中子散射重点实验室, 北京　100872

通信作者: 夏天龙, tlxia@ruc.edu.cn

基金项目: 国家重点研发计划(批准号: 2019YFA0308602)、国家自然科学基金(批准号: 12074425, 11874422)、中央高校基本科研业务费(批准号: 18XNLG14, 19XNLG18)和中国人民大学2020年度拔尖创新人才培育计划资助的课题

收稿日期: 2022-08-04

修回日期: 2022-11-04

上网日期: 2023-01-16

刊出日期: 2023-02-05

摘要: 拓扑材料因具有新奇物理特性受到广泛关注, 这些材料一方面为基础物理研究提供了新的平台, 另一方面在以拓扑物理为基础发展的器件研究方向上展现出潜在应用价值. 凝聚态领域对于拓扑材料相关物理问题的研究主要通过两种方式开展: 一是在已知的拓扑材料中不断挖掘新的实验现象和物理问题; 二是不断预言和探索发现新型拓扑材料体系并开展合成. 无论哪种方式, 高质量单晶的获得都至关重要, 它为角分辨光电子能谱、扫描隧道显微谱和磁场下的量子振荡等实验研究提供了前提保障. 本文总结了拓扑材料的分类和发展, 基于本研究组近些年开展的工作介绍了助溶剂法、气相输运法这两种拓扑材料单晶生长中常用的方法, 并详细介绍了拓扑物性研究领域几类典型的拓扑材料及其生长方法, 如拓扑绝缘体/拓扑半金属、高陈数手性拓扑半金属和磁性拓扑材料等.

关键词:

Single crystal growth of topological semimetals and magnetic topological materials

1.
Department of Physics, Renmin University of China, Beijing 100872, China

2.
Beijing Key Laboratory of Opto-electronic Functional Materials & Micro-nano Devices of Beijing, Renmin University of China, Beijing 100872, China

3.
Key Laboratory of Quantum Technology and Device of Zhejiang Province , Department of Physics, Zhejiang University, Hangzhou 310027, China

4.
Institute of Physical Science and Information Technology, Anhui University, Hefei 230601, China

5.
Key Laboratory for Neutron Scattering, Renmin University of China, Beijing 100872, China

Corresponding author: Xia Tian-Long, tlxia@ruc.edu.cn

Fund Project: Project supported by the National Key R&D Program of China (Grant No. 2019YFA0308602), the National Natural Science Foundation of China (Grant Nos. 12074425, 11874422), the Fundamental Research Fund for the Central Universities, China (Grant Nos. 18XNLG14, 19XNLG18), and the Outstanding Innovative Talents Cultivation Funded Programs 2020 of Renmin University of China

Received Date: 04 August 2022

Accepted Date: 04 November 2022

Available Online: 16 January 2023

Published Online: 05 February 2023

Abstract: Topological materials have attracted much attention due to their novel physical properties. These materials can not only serve as a platform for studying the fundamental physics, but also demonstrate a significant potential application in electronics, and they are studied usually in two ways. One is to constantly explore new experimental phenomena and physical problems in existing topological materials, and the other is to predict and discover new topological material systems and carry out synthesis for further studies. In a word, high-quality crystals are very important for studying quantum oscillations, angle resolved photoemission spectra or scanning tunneling microscopy. In this work, the classifications and developments of topological materials, including topological insulators, topological semimetals, and magnetic topological materials, are introduced. As usually employed growth methods in growing topological materials, flux and vapour transport methods are introduced in detail. Other growth methods, such as Bridgman, float-zone, vapour deposition and molecular beam epitaxy methods, are also briefly mentioned. Then the details about the crystal growth of some typical topological materials, including topological insulators/semimetals, high Chern number chiral topological semimetals and magnetic topological materials, are elaborated. Meanwhile, the identification of crystal quality is also briefly introduced, including the analysis of crystal composition and structure, which are greatly important.

Keywords:

熔点/℃

沸点/℃

可溶于酸或碱溶液

密度/(g·cm^-3)

毒性

660.3

2327

硫酸/硝酸/盐酸/氢氧化钠/氢氧化钾

2.70

无

29.8

2400

盐酸/硫酸

5.90

无

156.6

2000

硝酸/盐酸/硫酸

7.31

无

231.9

2270

盐酸/硝酸/碱溶液

7.28

无

327.5

1740

硫酸/硝酸/有机酸溶液/碱溶液

11.34

有

630.6

1635

硫酸

6.69

无

271.3

1500

硝酸

9.78

无

449.5

989.8

硝酸/盐酸/氢氧化钾

6.24

无

321.2

765

盐酸

8.65

有

熔点/℃

沸点/℃

稳定性

可溶于溶液

形貌

储存

I₂

113

184

易挥发/易升华

乙醇

紫红色颗粒

密封干燥

TeCl₄

224

380

易潮解

水/盐酸

白色粉末

密封干燥

BiCl₃

230

447

易潮解

水/盐酸

白色粉末

密封干燥

BiBr₃

218

441

易潮解

水/稀盐酸/丙酮

黄色粉末

密封干燥

TeBr₄

380

420

易潮解

水/氢氧化钠

黄色粉末

避光/密封

SnI₄

144.5

364

乙醇

橘黄色粉末

密封干燥

TeI₄

280

118 (升华点)

灼热易分解

乙醇/丙酮

灰色粉末

密封干燥

优点

缺点

适用范围

熔融重结晶法

1. 不需要加入其他试剂如助溶剂或输运剂, 损耗少且不引入杂质;
2. 不需要额外处理其他溶剂的分离或回收, 操作简单.

适用性不强

适合生长具有低熔点的目标材料

助溶
剂法

1. 适用性强, 几乎对于所有材料只要找到合适的助溶剂都可以将其以单晶形式生长出来;
2. 生长温度低, 适合熔点很高的化合物;
3. 生长出的晶体均匀完整.

1. 生长周期长;
2. 许多助溶剂都有不同程度的毒性处理后的助溶剂或含有助溶剂的溶液具有腐蚀性还会产生污染, 要做好分类并小心处理;
3. 使用坩埚, 可能会影响品体成核与生长取向.

适合生长本身熔点较高的化合物

气相输运法

1. 可以实现常压下难以合成的化合物;
2. 可以合成难以通过固-固, 固-液反应合成的化合物;
3. 温度调节灵活, 可以直接调控晶体生长时所需的应力, 饱和度等参量, 进而影响晶体的生长速度.

1. 产量较低;
2. 需要精准掌控输运剂的浓度和低沸点反应物的总量, 否则容易因为管内压强过大造成爆管;
3. 有些气相输运法需要通惰性气体或氢气, 操作复杂, 有一定的危险;
4. 管壁会限制晶体生长方向, 与管壁接触的晶面呈曲面.

适合生长反应物中沸点较低的化合物或其它难以通过固-固、固-液合成的化合物

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