Indium doped cadmium sulfide thin films were prepared by spray pyrolsis on glass substrates at different temperatures ranging from 300degreesC to 450degreesC in 25degreesC steps, using aqueous solution of copper chloride and thiourea salts. We used In(COOH)(3) as the dopant. Structural characterization was carried Out by X-ray diffractometry and scanning electron microscopy and high resolution electron microscopy were used together with atomic force microscopy (AFM) to follow the evolution of structural and morphological parameters of the films with substrate temperature (T,,). At least two preferential growth, (1 12) for samples with T. between 325degreesC and 400degreesC and (002) for T, between 400degreesC and 450degreesC, respectively were detected. For the films obtained at higher substrate temperatures, HREM micrographs revealed the presence of a large number of structural defects together with nanostructured configurations. AFM revealed surface modifications of CdS:In grains at higher substrate temperature. The substrate temperature is directly related with the shift detected in the band gap values derived from optical of parameters. (C) 2004 Elsevier B.V. All rights reserved.