Abstract Phosphate-based mesoporous TiO 2 materials were prepared by surfactant-directed method using an alkylphosphate surfactant, which produced a mesoporous titania with high surface area (∼200 m 2/g) and a phosphate monolayer interface. Calcination of the as-synthesized greenbody in an ozone atmosphere generated materials with higher surface area, and higher purity, than did calcination in air. These interfacial phosphate groups are convenient functionality for chemically modifying the surface via ion-exchange processes. High doping ratios of P/Ti (0.47–0.69) and Cd/P (0.37–0.40) were observed. Materials were characterized by XRD, FE-SEM, TEM, and XPS.