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3D plasmonic Bi metal@defective BiOCl hierarchical microspheres were constructed by a one-step solvothermal method. The effects of solvent thermal temperature on the microstructure and the photocatalytic performance were investigated. The photocatalyst prepared at 200 °C (Bi/BiOCl-200) showed most efficient visible photocatalytic activity for NOx removal. The enhanced activity can be ascribed to synergistic effects of oxygen vacancies and Bi metals. The oxygen vacancies in BiOCl induce the formation of an intermediate level to allow electrons transition from the valence band to intermediate level and then to the conduction band as revealed by density functional theory (DFT). The surface plasmon resonance (SPR) effect of elemental Bi enables the improvement of the visible light absorption efficiency and the promotion of the charge carrier separation as evidenced from the charge difference distribution …