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Abstract Currently, the production of urea by photochemical routes holds significant potential. However, photocatalytic urea synthesis is significantly limited by the co‐sorption and activation of CO 2 , H 2 O, and N 2 as well as C─N coupling process. Herein, Ru 1 (single atom)/CeO 2 ‐V O (containing oxygen vacancies) is synthesized by a room‐temperature photochemical strategy. Benefiting from the synergistic effect of Ce 3+ ‐V O and single atoms, Ru 1 /CeO 2 ‐V O nanosheets delivered the highest urea yield rate of 13.73 µmol g −1 h −1 . Ultrafast transient absorption spectroscopy demonstrated that the localized asymmetric structure formed by oxygen vacancies and Ru single atoms on CeO 2 can generate a stronger locally polarized electric field, thereby extending the photogenerated carrier lifetime. Experimental and theoretical calculations showed that Ru site promoted N 2 adsorption and optimized water dissociation, which ensured the formation of N‐containing intermediates and the supply of protons to synthesize urea. The Ce‐ V O site activated CO 2 to generate *CO, and the formed *CO migrated from the site to the adjacent Ru‐V O site. Further, the synergistic action of the dual sites promotes *CO couples with *NNH to form *NCONH, eventually converting to urea. Accordingly, this work sheds insight into the design of dual sites for effective photocatalytic C─N bond coupling to synthesize urea.
Ren et al. (Tue,) studied this question.