Synthesis and Microstructure of Antimony Oxide Nanorods

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Antimony oxide nanorods were synthesized by the microemulsion method. The nanorods had diameter in the range of 50–175 nm and a length of up to several micrometers. The microstructure of the nanorods was examined by analytical transmission electron microscopy and high-resolution transmission electron microscopy (HRTEM). Large-angle tilt diffraction experiments on the normal nanorods (about 90 nm in diameter) showed that they have an orthorhombic structure. Combining the results of internal standards using the silicon single crystal, it could be concluded that the synthesized nanorod is Sb2O4. The common growth direction of the nanorods was along the long axis. HRTEM images showed it had a periodic layer structure, and some defects and a layer of amorphous on the nanorods surface were found. The formation mechanism of Sb2O4 nanorods is briefly discussed.

I. INTRODUCTION

Semiconductor one-dimensional solid nanostructures, such as nanorods and nanowires, have been extensively studied recently because of many interesting physical properties1–3 and great potential applications, such as catalysis, photocatalysis, sensors, and optical, electronic, and magnetic materials.4–6 Many methods have been used to prepare nanorods and nanowires, such as solution-liquid-solid growth, laser ablation, carbon nanotube template-mediated growth, electrochemical fabrication, and nonaqeuous solution synthesis.7–12 Antimony oxide is useful as a flame retardant when combined with a halogen-containing resin and a halogenated flame retardant, and colloid antimony pentoxide nanoparticles have been widely used as an optical materials because of their high refractive index and high abrasive resistance. Recently some authors reported that hydrous antimony oxides exhibit high proton conductivity, and these compounds are likely to be extremely useful in humiditysensing materials.13,14 Various antimony oxides can be obtained by heating antimonic acid in air.15 The growth and characterization of antimony oxide nanoparticles synthesized by microemulsion have been reported using the polyvinyl alcohol (PVA) surfactant.16 In this paper, an approach using simple chemical reactions, such as microemulsion, was employed to synthesize antimony oxide nanorods and for the first time using the surfactant sodium bis-2-ethylhexyllsulfosuccinate a)

e-mail: zhang [email protected] Present address: Max-Planck Institute for Material Research, Heisenbergstr. 3, 70569 Stuttgart, Germany.

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http://journals.cambridge.org

J. Mater. Res., Vol. 17, No. 7, Jul 2002 Downloaded: 13 Mar 2015

(AOT). Large-angle tilt diffraction experiments and high-resolution transmission electron microscopy (TEM) were carried out on the nanorods to characterize the microstructure since the various antimony oxides may be formed during the synthesis. II. EXPERIMENTAL PROCEDURES

The preparation procedures of antimony oxide nanorods are described here in detail. Two hundred twentyeight milligrams SbCl3 was dissolved into 10 ml aqueous solution at a hydrochloric acid concentration of 6 mol/l. T