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The 15D/R achieve near 99.6% selectivity at the gas–solid interface for UV–Vis light-driven CO 2 reduction to CO, with a rate of 42.41 μmol·g−1. The high conductivity of RGO and the strong interaction with DUT-67 enhanced the electron coupling effect, which was conducive to the separation of carriers. The rapid formation of HCOO− and the rapid desorption of CO are responsible for the high CO yield and selectivity. [Display omitted] • The DUT-67/RGO aerogel are first prepared for CO 2 reduction in a gas–solid system. • 15D/R achieve near 99.6% selectivity for UV–Vis light-driven CO 2 reduction to CO. • Separation efficiency of carriers is the main reason for the improvement of CO yield. Herein, DUT-67/RGO aerogel photocatalysts with three-dimensional (3D) macroscopic morphology were first prepared by a facile hydrothermal and freeze-drying process. It was observed that DUT-67 endowed aerogels with strong adsorption/activation capacity for CO 2 molecules. Besides, RGO not only dispersed DUT-67 as a macroscopic carrier, but also improved the utilization rate of light energy. The high conductivity of RGO and the strong interaction with DUT-67 enhanced the electron coupling effect, which was conducive to the separation of carriers. 15D/R achieved near 99.6% selectivity at the gas–solid interface for UV–Vis light-driven CO 2 reduction to CO, with a rate of 42.41 μmol·g−1. The adsorption behavior of products at the interface and formation process of intermediates were monitored based on CO-TPD and in situ Fourier transform infrared spectra. The extremely high selectivity for CO came from the weak adsorption of CO on the surface of 15D/R and formation of CH 4 required more complex intermediates. [ABSTRACT FROM AUTHOR]