This paper pursed one new cost effective strategy to improve the photocatalytic activity of the sol-gel developed Zn doped TiO2 by mechano-chemically milling in high energy planetary mill. The results showed that the photocatlytic activity was improved two times due to the increase of the surface area and the decrease in average crystallite size at the same time after using the high energy ball milling. Kubelka-Munk spectra of pristine and ball milled samples revealed a blue shift from 3.2 eV to 3.35 eV, which may be because of the presence of quantum size effects. SEM microstructural investigations revealed variations in the surface morphology with different Zn doping concentrations in the TiO2-Xwt.% Zn nanoparticulates. EDS spectra of these samples confirmed the stoichiometric concentration of Zn. Other characterization including X-ray diffraction (XRD), BET surface and the photocatalytic decomposition were also studied and the results were in agreement with each other.