A series of Bi 2 S 3 /(BiO) 2 CO 3 composite photocatalysts with different loadings of amorphous Bi 2 S 3 were successfully synthesized through an ultrasonic-assisted ionexchange reaction between thioacetamide (CH 3 CSNH 2 ) and (BiO) 2 CO 3 , and characterized by XRD, XPS, BET, EELS, EDX, SEM, TEM/HRTEM, UV-Vis, and photoluminescence (PL) techniques. The results of TEM/HRTEM, EELS, and EDX indicate that the composite catalyst Bi 2 S 3 / (BiO) 2 CO 3 has been successfully synthesized with the deposited Bi 2 S 3 present in amorphous state on the surface of (BiO) 2 CO 3 . The activities of the catalysts for RhB degradation under visible light show that the catalyst prepared under ultrasonic is more active than the one synthesized without ultrasonic. The optimized sample Bi 2 S 3 / (BiO) 2 CO 3 (U5.0) exhibits a much higher activity, about 4.8 times to that of pure (BiO) 2 CO 3 . Based upon the band structures of Bi 2 S 3 /(BiO) 2 CO 3 , it is deduced that the migration of the visible light-induced electrons from the conduction band of Bi 2 S 3 to that of (BiO) 2 CO 3 should have facilitated the separation of photogenerated carriers, as confirmed by the suppressed photoluminescence spectra. Using different scavengers, the ÁO 2 -and holes are clearly identified as the main oxidative species for RhB photodegradation. In light of these observations, a potential photocatalytic mechanism of RhB degradation over Bi 2 S 3 / (BiO) 2 CO 3 is proposed.