The hierarchical photocatalysts of Ag/AgCl@plate–WO3 have been synthesized by anchoring Ag/AgCl nanocrystals on the surfaces of single-crystalline WO3 nanoplates that were obtained via an intercalation and topochemical approach. The heterogeneous precipitation process of the PVP–Ag+–WO3 suspensions with a Cl− solution added drop-wise was developed to synthesize AgCl@WO3 composites, which were then photoreduced to form Ag/AgCl@WO3 nanostructures in situ. WO3 nanocrystals with various shapes (i.e., nanoplates, nanorods, and nanoparticles) were used as the substrates to synthesize Ag/AgCl@WO3 photocatalysts, and the effects of the WO3 contents and photoreduction times on their visible-light-driven photocatalytic performance were investigated. The techniques of TEM, SEM, XPS, EDS, XRD, N2 adsorption–desorption and UV-vis DR spectra were used to characterize the compositions, phases and microstructures of the samples. The RhB aqueous solutions were used as the model system to estimate the photocatalytic performance of the as-obtained Ag/AgCl@WO3 nanostructures under visible light (λ ≥ 420 nm) and sunlight. The results indicated that the hierarchical Ag/AgCl@plate–WO3 photocatalyst has a higher photodegradation rate than Ag/AgCl, AgCl, AgCl@WO3 and TiO2 (P25). The contents and morphologies of the WO3 substrates in the Ag/AgCl@plate–WO3 photocatalysts have important effects on their photocatalytic performance. The related mechanisms for the enhancement in visible-light-driven photodegradation of RhB molecules were analyzed.
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