Novel Z-scheme type MoO 3 -g-C 3 N 4 composites photocatalysts were prepared with a simple mixingcalcination method, and evaluated for their photodegradation activities of methyl orange (MO). The optimized MoO 3 -g-C 3 N 4 photocatalyst shows a good activity with a kinetic constant of 0.0177 min À1 , 10.4 times higher than that of g-C 3 N 4 . Controlling various factors (MoO 3 -g-C 3 N 4 amount, initial MO concentration, and pH value of MO solution) can lead to the enhancement of the photocatalytic activity of the composite. Only MoO 3 and g-C 3 N 4 are detected with X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) spectra. N 2 adsorption and UV-vis diffuse reflectance spectroscopy (DRS) results suggest that the addition of MoO 3 slightly affects the specific surface area and the photoabsorption performance. The transmission electron microscopy (TEM) image of MoO 3 -g-C 3 N 4 indicates a close contact between MoO 3 and g-C 3 N 4 , which is beneficial to interparticle electron transfer. The high photocatalytic activity of MoO 3 -g-C 3 N 4 is mainly attributed to the synergetic effect of MoO 3 and g-C 3 N 4 in electron-hole pair separation via the charge migration between the two semiconductors. The charge transfer follows direct Z-scheme mechanism, which is proven by the reactive species trapping experiment and the cOH-trapping photoluminescence spectra.