Regular stibnite (Sb2S3) 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 Sb2S3 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 Sb2S3 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 Sb2S3 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 Sb2S3 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
Sb2S3 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.