A carbon doped (C-) photocatalyst, which shows good photocatalytic activity to Ultraviolet irradiation and visible irradiation, was successfully prepared by co-grinding of with ethanol or Activated Carbon(C), followed by heat treatment at in air for 60 min. Ethanol and C were used as a representative agent of liquid and solid for carbon doping. Their influence on improving photocatalytic ability and carbon doping degree was studied with degradation of methyl orange and XPS analysis. The product prepared by co-grinding of with Ethanol had Ti-C and C-O chemical bonds and showed higher photocatalytic activity than the product prepared by co-grinding of with C, where just C-O chemical bond existed. As a result, mechanochemical route is useful to prepare a carbon doped photocatalyst activating to visible irradiation, where the solid-liquid operation is more effective than solid-solid operation to obtain a carbon doped .