Co
3O
4/BiVO
4 composite photocatalyst with a p-n heterojunction semiconductor structure has been synthesizedby the impregnation method. The physical and photophysical properties of the composite photocatalyst havebeen characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transimission electronmicroscopy (TEM), BET surface area, and UV-visible diffuse reflectance spectra. Co is present as p-typeCo
3O
4 and disperses on the surface of n-type BiVO
4 to constitute a heterojunction composite. The photocatalystexhibits enhanced photocatalytic activity for phenol degradation under visible light irradiation. The highestefficiency is observed when calcined at 300
C with 0.8 wt % cobalt content. On the basis of the calculatedenergy band positions and PL spectra, the mechanism of enhanced photocatalytic activity has been discussed.