With an increasing demand for industrial dyes in our daily lives, water conditions have become worse. Recently, the removal of such environmentally hazardous pollutants from wastewaters through photocatalytic degradation has been drawing increased attention. Three mesoporous nanophases of BiFeVOx.y as (Bi2FeIIIV1−yO5.5−y) visible light photocatalysts were synthesized in this study using ethylene glycol-citrate sol-gel synthesis combined with microwave- assisted calcination. X-ray diffraction (XRD), differential thermal analysis (DTA), FTIR spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy coupled with energy dispersive X-ray spectrometry (SEM-EDS), nitrogen adsorption-desorption isotherms, and UV-Vis diffuse reflectance spectrophotometry (UV-Vis/DRS) were used to characterize the BiFeVOx.y photocatalysts. The visible light-induced photocatalytic activities of the BiFeVOx.y phases were evaluated by the degradation of methylene blue (MB) dye in aqueous solution at pH ~10.0. The results of this study show that the combination of doping strategy with the utilization of advanced synthesis methods plays an important role in improving the structure and surface properties of BiFeVOx.y phases, and thereby enhancing their adsorption and photocatalytic efficiencies. The synthesized mesoporous tetragonal γ-BiFeVOx.y nanophase has been proven to be a potential visible-light photocatalyst for the degradation of organic dyes.