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A visible‐light photocatalyst containing Ag2Se and reduced graphene oxide (RGO) was synthesized by a facile sonochemical‐assisted hydrothermal method. X‐ray diffraction, scanning electron mi‐croscopy with energy‐dispersive X‐ray analysis, and ultraviolet‐visible diffuse reflectance spectros‐copy results indicated that the RGO‐Ag2Se nanocomposite contained small crystalline Ag2Se nano‐particles dispersed over graphene nanosheets and absorbed visible light. The high crystallinity of the nanoparticles increased photocatalytic activity by facilitating charge transport. N2 adsorp‐tion‐desorption measurements revealed that the RGO‐Ag2Se nanocomposite contained numerous pores with an average diameter of 9 nm, which should allow reactant molecules to readily access the Ag2Se nanoparticles. The RGO‐Ag2Se nanocomposite exhibited higher photocatalytic activity than bulk Ag2Se nanoparticles to degrade organic pollutant rhodamine B and industrial dye Texbrite BA‐L under visible‐light irradiation (λ>420 nm). The generation of reactive oxygen spe‐cies in RGO‐Ag2Se was evaluated through its ability to oxidize 1,5‐diphenylcarbazide to 1,5‐diphenylcarbazone. The small size of the Ag2Se nanoparticles in RGO‐Ag2Se was related to the use of ultrasonication during their formation, revealing that this approach is attractive to form po‐rous RGO‐Ag2Se materials with high photocatalytic activity under visible light.

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