N-F codoped TiO 2 /straw charcoal composites (NF-TiO 2 /SC) were synthesized using a simple, bioframe-assisted sol-gel method and confirmed by XRD, SEM, EDX, TEM, N 2 adsorption-desorption, Raman, FT-IR, XPS, UV-vis DRS measurements. It has been found that the as-synthesized catalysts formed 3D-hierarchical structure with carbon framework after calcination.The physicochemical properties such as BET surface area, porosity, crystallite size and pore size distribution could be effectively controlled by adjusting the calcination temperature. Higher surface area, smaller crystallite size and higher absorption in the visible light region were obtained for NF-TiO 2 /SC calcined at 450 ºC. Under visible light irradiation, NF-TiO 2 /SC450 exhibited much higher adsorptive ability and photocatalytic activity and there existed a significant synergistic effect between adsorption and photocatalytic degradation. Furthermore, the as-synthesized catalysts have a good mineralized ability and can be used repeatedly, revealing great potential for practical applications in environmental cleanup.