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In this paper,C-N co-doped TiO2 microspheres were synthesized by microwave-assisted approach.The average diameter of TiO2 microspheres is about 0.5 μm.The TiO2 microspheres are consisted of C-N co-doped anatase and carbon layer.The carbon on the surface of TiO2 makes TiO2 microspheres absorb visible light and organic pollutants.Furthermore,C and N were successfully doped into the TiO2 lattice,which caused the distortion of the lattice and decreased it gap to 3.02 eV.The influences of the amount of NH4F and ethanol on the morphology of C-N codoped TiO2 microspheres were investigated in detail.Moreover,the C-N codoped TiO2 microspheres synthesized with 0.26 g of NH4F showed highest photocatalytic property.The microwave-assisted synthesis process of C-N co-doped TiO2 microspheres is simple,short time-consuming and has practical significance.