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A novel 2D/2D BizMoO6/g-C3 N4 step-scheme (S-scheme) composite by loading Au as cocatalyst was suc-cessfully fabricated using a photoreduction and hydrothermal route.The obtained Bi2MoO6/g-C3N4/Au photocatalysts were characterized by X-ray diffraction (XRD),transmission electron microscope (TEM),X-ray photo-electron spectroscopy (XPS),UV-vis diffuse reflectance spectra (UV-vis),Fourier transform infrared spectroscopy (FTIR),photoluminescence (PL),photocurrent response(I-t),and electrochemical impedance spectroscopy (EIS).The HRTEM images revealed that an intimate interface in composites were formed.The optimum photocatalytic activity of Rhodamine B degradation over Bi2 MoO6/g-C3N4/Au was about 9.7 times and 13.1 times as high as those of Bi2MoO6 and g-C3N4,respectively.The notably improved photocatalytic activity of Bi2MoO6/g-C3N4/Au could be mainly ascribed to the abundant active sites and the enhanced separation efficiency of photogenerated carriers in Bi2MoO6/g-C3N4 S-scheme system.Notably,Au nanoparticles could act as a co-catalyst to further promote electron transfer and sep-aration from the conduction band of g-C3N4.Additionally,a possible step-scheme photocatalytic reaction mechanism of RhB degradation over Bi2MoO6/g-C3N4/Au was tentatively proposed.PL and transient pho-tocurrent analysis implied that Bi2MoO6/g-C3N4/Au photocatalysts possessed the lower recombination rate of photogenerated carriers compared with pure Bi2MoO6 and g-C3N4,respectively.The present work is expected to provide useful information in designing 2D/2D S-scheme heterojunction photocatalysts.