In the present paper, thin film CdSe compound semiconductors have been electroplated on transparent conducting oxide coated glass substrates from nonaqueous dimethyl formamide bath containing CdCl2, KI and Se under controlled temperature ranging from 100 to 140 degrees C. Thickness of the deposited films as obtained through focussed ion beam technique as well as their microstructural and photoelectrochemical properties have been found to depend on temperature. The film growth was therefore optimized at a bath temperature similar to 125 degrees C. The formation of crystallites in the range of 100-150 nm size has been ascertained through atomic force microscopy and scanning electron microscopy. Energy dispersive analysis of X-rays for the as deposited film confirmed the 1:1 composition of CdSe compound in the matrix exhibiting band-gap energy of 1.74 eV. Microstructural properties of the deposited films have been determined through X-ray diffraction studies, high-resolution transmission electron microscopy and electron diffraction pattern analysis. Electrochemical impedance spectroscopy and current-potential measurements have been performed to characterize the electrochemical behavior of the semiconductor-electrolyte interface. The photo-activity of the films have been recorded in polysulphide solution under illumination and solar conversion efficiency >= 1% was achieved. (c) 2006 Elsevier B.V. All rights reserved.