气相传输法制备大尺寸单晶Bi2Se3纳米片、纳米带

doi:10.15541/jim20140087

无机材料学报 ›› 2014, Vol. 29 ›› Issue (11): 1199-1203.DOI: 10.15541/jim20140087 CSTR: 32189.14.10.15541/jim20140087

气相传输法制备大尺寸单晶Bi₂Se₃纳米片、纳米带

李小帅¹, 王增梅^{1, 2}, 朱鸣芳³, 王善朋², 陶绪堂², 陆骏¹, 陈兴涛¹, 徐佳乐¹

(1. 东南大学江苏省土木工程材料重点实验室, 南京211189; 2. 山东大学晶体材料国家重点实验室, 济南250100; 3. 东南大学江苏省先进金属材料高技术研究重点实验室, 南京211189)

收稿日期:2014-02-27 修回日期:2014-04-13 出版日期:2014-11-20 网络出版日期:2014-10-24
作者简介:李小帅(1990–), 男, 硕士研究生. E-mail: lixsseu@163.com
基金资助:
国家自然科学基金(51002029);山东大学晶体材料国家重点实验室开放课题(KF1107)

Synthesis of Jumbo-size Single Crystalline Bi₂Se₃Nanoplates and Nanoribbons by Vapor Transportation

LI Xiao-Shuai¹, WANG Zeng-Mei^{1, 2}, ZHU Ming-Fang³, WANG Shan-Peng², TAO Xu-Tang², LU Jun¹, CHEN Xing-Tao¹, XU Jia-Le¹

(1. Jiangsu Key Laboratory of Construction Materials, Southeast University, Nanjing 211189, China; 2. State Key Laboratory of Crystal Materials, Shandong University, Jinan, 250100, China; 3. Jiangsu Key Laboratory of Advanced Metallic Materials, Southeast University, Nanjing 211189, China)

Received:2014-02-27 Revised:2014-04-13 Published:2014-11-20 Online:2014-10-24
About author:LI Xiao-Shuai. E-mail: lixsseu@163.com
Supported by:
Natural Science Foundation of China(51002029);Opening project for State Key Laboratory of Crystal Materials, Shandong University, China(KF1107)

摘要/Abstract

摘要：

低维Bi₂Se₃纳米材料是最新研究发现的一种新型三维拓扑绝缘体材料, 在微电子器件和传感器领域具有广阔的应用前景。本研究采用气相传输法在真空石英管中合成了大尺寸单晶Bi₂Se₃纳米片、纳米带。通过XRD、EDS、Raman、SEM等手段对Bi₂Se₃纳米片、纳米带的物相结构、组成、表面形貌等进行表征。测试结果表明: 气相传输法合成的单晶Bi₂Se₃纳米片、纳米带相纯度高, 结晶性能好, 均是{001}取向; Bi₂Se₃纳米片水平尺寸大, 约为15~180 μm; Bi₂Se₃纳米带长度达860 μm, 宽度约5 μm。根据不同温度下制备的Bi₂Se₃纳米片、纳米带SEM照片及其不同方向结合能的差异, 分析了其可能的生长机制: 在较高温度下沿<001>和方向生长速度快, 生成大尺寸单晶Bi₂Se₃纳米片; 在较低温度下, 沿方向生长速度快, 生成大尺寸单晶Bi₂Se₃纳米带。这些研究结果完善了大尺寸Bi₂Se₃纳米材料的制备工艺, 有望在微电子器件领域得到商业化应用。

关键词: 气相传输法, Bi2Se3纳米片, Bi2Se3纳米带

Abstract:

Low-dimensional Bi₂Se₃nanomaterials were discovered to be new three-dimensional (3D) topological insulators (TIs) recently, which have broad application prospect in the field of microelectronic devices and sensors. Single crystalline Bi₂Se₃nanoplates (NPs) and nanoribbons (NRs) with jumbo size were synthesized in the vacuum quartz tube via vapor transportation. The crystal structure, composition and morphology of the as-prepared Bi₂Se₃NPs and NRs were analyzed by XRD, EDS, Raman and SEM. It is found that both of the two specimens are well-crystallized in the direction of {001} with a high purity. Bi₂Se₃NPs have a large lateral size of 15-180 μm, while Bi₂Se₃NRs have a large length of 860 μm and a width of about 5 μm. Besides, the probable growth mechanism is proposed based on the analysis of the SEM images of Bi₂Se₃NPs and NRs prepared at different temperatures and the binding energy difference along different directions. Bi₂Se₃ has a quicker growth speed along <001> and directions in relatively high temperature to form single crystalline NPs with large lateral size, while it grows faster along direction in lower temperature to get single crystalline NRs with large length. All these results not only improve the preparation process of Bi₂Se₃nanomaterials with jumbo size, but also promote the commercial use in the field of microelectronic devices.

Key words: vapor transportation, Bi2Se3 nanoplates, Bi2Se3 nanoribbons

中图分类号:

TB34

李小帅, 王增梅, 朱鸣芳, 王善朋, 陶绪堂, 陆骏, 陈兴涛, 徐佳乐. 气相传输法制备大尺寸单晶Bi₂Se₃纳米片、纳米带[J]. 无机材料学报, 2014, 29(11): 1199-1203.

LI Xiao-Shuai, WANG Zeng-Mei, ZHU Ming-Fang, WANG Shan-Peng, TAO Xu-Tang, LU Jun, CHEN Xing-Tao, XU Jia-Le. Synthesis of Jumbo-size Single Crystalline Bi₂Se₃Nanoplates and Nanoribbons by Vapor Transportation[J]. Journal of Inorganic Materials, 2014, 29(11): 1199-1203.

图/表 6

图1 气相传输法制备Bi2Se3纳米片、纳米带实验装置示意图

Fig. 1 Schematic of experimental setup for the synthesis of Bi2Se3 nanoplates and nanoribbons with vapor transportation Ⅰ: 700℃; Ⅱ: 350℃-450℃

图2 高温真空熔炼制备的Bi2Se3块体

Fig. 2 Bulk Bi2Se3 synthesized by vacuum melting at high temperature

图3 Bi2Se3块体、纳米片和纳米带的XRD图谱

Fig. 3 XRD patterns of bulk Bi2Se3, Bi2Se3 nanoplates and Bi2Se3 nanoribbons

图4 Bi2Se3纳米片(a)和Bi2Se3纳米带(b)的EDS图谱

Fig. 4 EDS spectra of Bi2Se3 nanoplates (a) and Bi2Se3 nanoribbons (b)

图5 Bi2Se3块体、纳米片和纳米带的Raman光谱

Fig. 5 Raman spectra of bulk Bi2Se3, Bi2Se3 nanoplates and Bi2Se3 nanoribbons

图6 不同放大倍数下Bi2Se3纳米片(a~d)、Bi2Se3纳米带(e~h)的SEM照片

Fig. 6 SEM images of Bi2Se3 nanoplates (a-d) and Bi2Se3 nanoribbons (e-h) at different magnifications

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气相传输法制备大尺寸单晶Bi₂Se₃纳米片、纳米带

Synthesis of Jumbo-size Single Crystalline Bi₂Se₃Nanoplates and Nanoribbons by Vapor Transportation

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