Advanced Oxidation Process is modern chemical method for the treatment of water containing non- biodegradable /toxic substances and to get decontaminated drinking water. Zinc acetate precursor is used to deposit zinc oxide thin films by Spray pyrolysis technique. Preperative parameters such as, substrate temperature, solution concentration and quantity of spraying solution were optimized to get good quality zinc oxide thin films. The prepared films were characterized by PEC, XRD, SEM, EDAX and UV-vis spectroscopy characterization techniques. Silver and gold deposited zinc oxide films were prepared to enhance photocatalytic inactivation of bacteria. The optimized stratified layer of TiO2 was given on zinc oxide thin films to improve its performance in photocatalytic process. The films prepared at optimized conditions of temperatures, concentrations are used in specially designed photoelectrochemical detoxification reactor. The prepared ZnO, Ag: ZnO, Au: ZnO and ZnO/TiO2 films are used to degrade Methylene blue (MB), textile effluent and inactivation bacteria such as E.coli, Bacillus, Salmonella, Staphylococcus etc.