Sonochemical fabrication and characterization of stibnite nanorods

Regular stibnite (Sb(2)S(3)) nanorods with diameters of 20-40 nm and lengths of 220-350 nm have been successfully synthesized by a sonochemical method under ambient air from an ethanolic solution containing antimony trichloride and thioacetamide. The as-prepared Sb(2)S(3) nanorods are characterized by employing techniques including X-ray powder diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, energy-dispersive X-ray analysis, transmission electron microscopy, selected area electron diffraction, high-resolution transmission electron microscopy, and optical diffuse reflection spectroscopy. Microstructural analysis reveals that the Sb(2)S(3) nanorods crystallize in an orthorhombic structure and predominantly grow along the (001) crystalline plane. High-intensity ultrasound irradiation plays an important role in the formation of these Sb(2)S(3) nanorods. The experimental results show that the sonochemical formation of stibnite nanorods can be divided into four steps in sequence: (1) ultrasound-induced decomposition of the precursor, which leads to the formation of amorphous Sb(2)S(3) nanospheres; (2) ultrasound-induced crystallization of these amorphous nanospheres and generation of nanocrystalline irregular short rods; (3) a crystal growth process, giving rise to the formation of regular needle-shaped nanowhiskers; (4) surface corrosion and fragmentation of the nanowhiskers by ultrasound irradiation, resulting in the formation of regular nanorods. The optical properties of the Sb(2)S(3) amorphous nanospheres, irregular short nanorods, needle-shaped nanowhiskers, and regular nanorods are investigated by diffuse reflection spectroscopic measurements, and the band gaps are measured to be 2.45, 1.99, 1.85, and 1.94 eV, respectively.