The successive ionic layer adsorption and reaction (SILAR) method is relatively new, simple and less expensive. This method is employed to deposit nanocrystalline Bi2Se3, Sb2Se3 and Bi2Se3-Sb2Se3 thin films onto amorphous glass substrates at low temperature (300 K). The preparative parameters such as concentration of precursor solutions. rinsing time, immersion cycles and immersion time are optimized to get nanocrystalline films. These films are characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM). atomic force microscopy (AFM), high resolution transmission electron microscopy (HRTEM), energy dispersive X-ray analysis (EDAX), optical absorption and electrical measurement techniques.