Nanocrystalline thin films of Sb2S3 and Sb2Se3 are obtained at low temperature by simple chemical deposition method. The preparative parameters are optimized to get nanocrystalline films. The films are characterized for structural, surface morphological and compositional analyses by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), high-resolution transmission electron micrograph (HRTEM), energy-dispersive X-ray analyses (EDAX) and Rutherford back-scattering (RBS). XRD study confirms orthorhombic structure of Sb2S3 and Sb2Se3. Nanocrystallinity is evidenced from SEM, AFM and HRTEM studies with some random distribution of nanocrystallites. Stoichiometry of films are studied from EDAX and RBS analyses which showed some inclusion of oxygen in the films which is unavoidable for chemically deposited chalcogenides films. (C) 2002 Elsevier Science B.V. All rights reserved.