Sb2Te3纳米片的水热合成与表征

doi:10.7503/cjcu20150808

摘要/Abstract

摘要：

在水热条件下, 以乙醇胺为还原剂, 实现了亚碲酸根(Te $O 3 2 -$ )的分步还原, 并以新生成的单质Te纳米棒为碲源, 原位一步法合成出六方相Sb₂Te₃纳米片. 采用X射线粉末衍射仪(XRD)、场发射扫描电子显微镜(FESEM)和透射电子显微镜(TEM)等对产物的物相、形貌及组成进行了表征. 结果表明, 产物Sb₂Te₃为六方纳米片, 厚度约为100~200 nm, 直径约为0.6~1.5 μm, 形貌均一, 分散性良好. 适宜的合成条件是水/乙醇胺体积比为8∶12, 180 ℃下反应24 h. 依据部分实验结果以及单质Te和六方相Sb₂Te₃晶体结构的比较, 证明了Sb₂Te₃主要以外延方式在单质Te纳米棒表面生长, 且两者的晶面取向为(003)Te//(003) Sb₂Te₃, [110]Te//[110]Sb₂Te₃.

关键词: 水热合成, Sb2Te3纳米片, 形貌, 反应机制

Abstract:

Under hydrothermal conditions and with ethanolamine acting as the reducing agent, fractional reduction of Te $O 3 2 -$ was realized, and Sb₂Te₃ nanoplates were synthesized in situ with the newly generated Te nanorods acting as tellurium source. The as-prepared product was characterized by X-ray powder diffractometer(XRD), field emission scanning electron microscope(SEM), and transmission electron microscope(TEM). Results showed that the product presents the hexastyle nanoplate structure with the thickness of about 100—200 nm and the diameter of about 0.6—1.5 μm, and has a uniform morphology and good dispersibility. The suitable conditions were that the volume ratio of water to ethanolamine was 8∶12, and the reaction lasted for 24 h at 180 ℃. By comparing the crystal structures of the elemental Te and hexagonal Sb₂Te₃ as well as some experimental results, that the hexagonal phase Sb₂Te₃ grew epitaxially on the lateral sides of newly generated Te nanorods was discussed preliminarily, and their crystal orientations were (003)Te//(003)Sb₂Te₃, and [110]Te//[110]Sb₂Te₃.

Key words: Hydrothermal synthesis, Sb2Te3 nanoplates, Morphology, Reaction mechanism

中图分类号:

O614

TrendMD:

柴臻臻, 郑文君. Sb₂Te₃纳米片的水热合成与表征. 高等学校化学学报, 2016, 37(3): 435.

CHAI Zhenzhen, ZHENG Wenjun. Hydrothermal Synthesis and Characterization of Sb₂Te₃ Nanoplates^†. Chem. J. Chinese Universities, 2016, 37(3): 435.

图/表 8

Fig.1 SEM images with different magnifications(A—C) and XRD pattern(D) of the Sb2Te3

Fig.2 EDS spectrum of the Sb2Te3 nanoplates synthesized at 180 ℃ for 24 h

Fig.3 TEM images(A, B), HRTEM image(C) of the Sb2Te3 nanoplates synthesized at 180 ℃ for 24 h and the atomic arrangement of Sb2Te3 [001] crystal zonal direction(D)The inset in (C) shows the corresponding SAED pattern.

Fig.4 SEM images of the products synthesized at 180 ℃ for different reaction timeReaction time/h: (A) 1; (B) 2; (C) 4; (D) 8; (E) 12; (F) 16.

Fig.5 XRD patterns of products synthesized at 180 ℃ for different reaction timeReaction time/h: a. 1; b. 2; c. 4; d. 8; e. 12; f. 16.

Fig.6 Atomic arrangements along c axis of hexagonal Sb2Te3(A) and hexagonal Te(B), the atomic arrangements and selected interatomic distances of (110) lattice planes of hexa-gonal Te(C) and hexagonal Sb2Te3(D)The blue balls and the yellow brown balls represent Te1 and Te2 atoms, respectively, and the pink ones are on behalf of Sb atoms.

Fig.7 SEM images indicating the influence of the volume ratio of H2O/MEA on the morphologies and phases evolutionThe synthesis was carried out at 180 ℃ for 24 h. V(H2O)/V(MEA): (A) 20∶0; (B) 0∶20; (C) 15∶5; (D) 12∶8; (E) 10∶10; (F) 8∶12; (G) 5∶15.

Fig.8 XRD patterns indicating the influence of the volume ratio of H2O/MEA on the morpho-logies and phases evolution

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Sb₂Te₃纳米片的水热合成与表征

Hydrothermal Synthesis and Characterization of Sb₂Te₃ Nanoplates^†

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