Using X-ray diffraction, transmission electron microscopy, Brunauer-Emmett-Teller surface area measurement, ultraviolet-visible diffuse reflection spectra, and photoluminescence spectroscopy, the effect of mechanical milling on the photocatalytic activity of g-C 3 N 4 photocatalyst was investigated. The rhodamine B, as a photodegrading goal, was used to evaluate the photocatalytic activity of g-C 3 N 4 . The experimental results indicate that the milling treatment is an effective method to improve the photocatalytic activity of g-C 3 N 4 . The enhanced photocatalytic activity was attributed to the improvement in catalyst's surface area and dye adsorption on catalyst surface. Moreover, checking the luminescence properties of g-C 3 N 4 , it is found that the photocatalytic active sites on g-C 3 N 4 are likely the same as luminescence sites.