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Herein, CuO/Bi 2 MoO 6 hybrid nanosheets were prepared as a surface multifunctional photocatalyst for gas-phase toluene oxidation with high conversion (>99%). Aberration-corrected scanning transmission electron microscopy suggested that CuO species were highly dispersed on the nanosheets. X-ray absorption fine structure spectra indicated that the distorted and stretched Cu−O coordination structures in CuO/Bi 2 MoO 6 nanosheets would provide open active sites. In situ Fourier transform infrared and density functional theory results showed that toluene molecules could be chemisorbed and activated on the active sites of CuO/Bi 2 MoO 6 nanosheets by the C−H group forming CuO/ Bi 2 MoO 6 •••Ph-CH 3 surface complex compounds. These would induce electron−hole transfer and initiate photocatalytic reactions under visible light irradiation. The corresponding intermediates of benzaldehyde and benzoic acid would be detected by in situ diffuse reflectance infrared Fourier transform spectroscopy. Furthermore, the synergistic effect of CuO and Bi 2 MoO 6 nanosheets could monitor charge dynamics to facilitate their respective transmission from photoexcitation sites to active centers. This work provides new insights into the essence of visible-light-driven surface photocatalysis and is expected to promote the design of novel and more effective photocatalysts at the molecular level.

High-efficiency, low-temperature, durable catalysts are regarded as promising tools for oxidizing volatile organic compounds (VOCs). In this study, we design an alternative core/shell structure with inert porous SiO 2 nanoparticles decorated with Pt nanoparticles as the core and an ultrathin ZrO 2 layer as the shell (SiO 2 @Pt@ZrO 2 ), where the average thickness of the ZrO 2 shell is 6 nm. The close three-dimensional contact between the Pt nanoparticles and the ZrO 2 shell maximizes the metal− support interaction and enables strong electronic interactions. Consequently, the as-prepared samples show superior charge separation, thermal stability, and reactive oxygen generation capacity. Photothermal synergetic catalytic activity is demonstrated via the toluene oxidation reaction, and it is found that toluene can be completely oxidized within 1 h of light illumination at 150 °C, compared to 80% oxidation under the same conditions without light illumination. The results provide insight into the design of high-performance catalysts of refractory VOCs.