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Photoactive (IOI) inorganic/organic interface assemblies were prepared using an occlusion electrodeposition method. Poly-2,2′:5′,2′′-Terthiophene (PTTh) were the organic thin films that occluded each of CdS, TiO 2 , and Zn-doped WO 3 nanoparticles. The energy band gap structures were investigated using spectroscopic and electrochemical techniques. The obtained assemblies were investigated in aqueous solutions under both dark and illuminated conditions. The results were compared with the behavior of PTTh thin film. Oxygen played an important role in minimizing electron/hole recombination as was evident by observed very low photocurrent when oxygen was removed by nitrogen purge. Results show that PTTh/CdS gave the greatest photocurrent, followed by PTTh/Zn-WO 3 and PTTh/TiO 2 .