CaAl2O4:(Eu,Nd)/rutile phase TiO2-x N y composites were synthesized via a two-step method, i.e. a solvothermal reaction followed by a mechanochemical treatment. The photocatalytic deNO x activity of the composites was evaluated under UV light (λ > 290 nm) irradiation and after turning off the UV light. It was confirmed that rutile phase TiO2-x N y nanoparticles could be uniformly dispersed on the surface of CaAl 2O4:(Eu,Nd) after planetary ball milling treatment. The composites prepared by this two-step method had high photocatalytic activity and good prolonged catalysis time even after turning off the light.