FeVO4photocatalysts were synthesized via a surfactant-assisted sol-gel method and characterized with X-ray diffraction (XRD), scanning electron microsoope (SEM)and specific surface area (BET). The photocatalytic activity was evaluated by photocatalytic degradation of methyl orange (MO) solution under visible light. The XRD patterns of no-surfactant-assisted, PEG-assisted, CTAB-assisted and SDS-assisted FeVO4, indicate that diffraction peaks can be well indexed as triclinc FeVO4. And the crystalline sizes of samples were evaluated as 113, 69, 66, 76 nm for FVO, FVO-PEG, FVO-CATB and FVO-SDS respectively.The addition of surfactant woul greatly affect the morphology of FeVO4photocatalysts, which can lead to different photocatalytic activities between them. In the experimental conditions used, the PEG-assisted FeVO4product had a much higher photocatalytic activity (the photodegradation rate was about 77% or so in 14h) than the other three products.