In this dissertation, pristine ordered, metal- (Fe, Co, and Ni), and nonmetal- (N) doped ordered mesoporous titania were synthesized via co-precipitation using the EISA method combined with the LCT pathway. In addition, for un-doped mesoporous TiO2, various parameters were systematically varied including solvent evaporation temperature, surfactant extraction conditions, molar surfactant/titanium ratio, and titanium source. Moreover, the photocatalytic activity of the synthesized materials was evaluated in the photodegradation of phenol under various irradiation sources.