In the present work, we report the development of phase pure and highly crystalline stibnite Sb2S3 nanostructures by a surfactant-mediated hydrothermal method. Polyvinylpyrrolidone (PVP) as the surfactant has a striking effect on the assembly of nanorods into dumbbell shaped nanorod-bundles. While nanorods with high aspect ratio were formed in absence of the surfactant, dumbbell shaped nanorod bundles were obtained using the surfactant. The structural, morphological, and optical properties were examined by X-ray diffraction (XRD), Raman scattering, scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy (XPS), and UV–visible spectrophotometer. Both XRD and Raman spectroscopy confirmed the formation of orthorhombic phase pure stibnite (Sb2S3). The ratio of Sb to S is found to be close to 2:3, corresponding to Sb2S3. The optical band gap varied in the range of 1.65–1.68 eV depending on the concentration of the surfactant.
