Molybdenum dichalcogenides are semiconductors with layered type structure, which can act as efficient electrodes in the realization of photoelectrochemical solar cells. The main advantage of this molybdenum diselenide (MoSe2) semiconductor is the prevention of electrolyte corrosion because of the phototransitions involving non-bonding d-d orbital of the Mo atoms. Polycrystalline molybdenum diselenide thin films are prepared by pulsed electrodeposition on conducting glass and titanium substrates in galvanostatic mode from an ammoniacal solution of H2MoO4 and SeO2. The growth kinetics of the film was studied and the deposition parameters such as electrolyte bath concentration, bath temperature, time of deposition, deposition current, pH of the electrolyte and duty cycle of the current are optimized. X-ray diffraction analysis of the as deposited and annealed films showed the presence of highly textured MoSe2 films with polycrystalline nature. EDAX spectrum of the surface composition confirms the nearly stoichiometric MoSe2 nature of the film. Surface morphology studies by scanning electron microscope (SEM) shows that the films are pinhole free and of device quality nature. The optical absorption spectra show an indirect band gap value of 1.16 eV. Conductivity measurements were carried out at different temperatures and electrical constants such as activation energy, trapped energy state and barrier height were calculated. (C) 2004 Elsevier Ltd. All rights reserved.