The synthesis of binary MoS2, MoSe2 and mixed [Mo(S1-xSex)(2)] thin films onto a glass substrates using arrested precipitation technique ( APT) is presented in this investigation. Growth kinetics and mechanism of film formation were studied for these films and are explained in brief. The stoichiometry of the film is confirmed by analyzing films using Extractive spectrophotometric ( ESP), atomic absorption spectroscopic (AAS) and electron difftraction X-ray microanalysis (EDAX) techniques. The semiconductor solution containing Mo(VI) and Se(IV) is extracted with N-n-octylaniline in xylene and determined by ESP, AAS and EDAX techniques. Further these films are characterized for its semiconducting behavior to test the suitability of molybdenum chalcogenides as a photoelectrode to convert radiant energy into electricity. It is found that stoichiometry of the film formed by our recently developed arrested precipitation technique ( APT) has strong influence on photoconduction in molybdenum chalcogenide photoelectrodes. (C) 2004 Kluwer Academic Publishers.