The paper presents an improved method of depositing nanocrystalline thin films of Fe‐doped TiO2 to be used as a reusable cyclic photocatalyst for degrading the organic pollutants. The technique of electron cyclotron resonance plasma‐enhanced chemical vapor deposition was employed with titanium tetra‐isopropoxide (C12H28O4Ti) and ferrocene (C10H10Fe) as precursors of Ti and Fe, respectively. Optical emission spectroscopy was used to identify the reactive species, to determine the electron temperature and the ion density during deposition. The films were characterized using optical absorption and photoluminescence spectra, whereas the morphological analysis was carried out with scanning electron microscopy. Strong adhesion of the deposited films with the substrate ruled out any possibility of TiO2 particles being leached out. It was confirmed by observing the degradation rate of the same film repeatedly. Cyclic use of the film for the catalytic reactions thus makes the process much user friendly for the water treatment. Copyright © 2014 John Wiley & Sons, Ltd.