Developing efficient photocatalysts for synchronously producing H2 and high value‐added chemicals holds great promise to enhance solar energy conversion. Herein, a facile strategy of simultaneously engineering Pd cocatalyst and oxygen vacancies (VOs) on TiO2 to promote H2 production coupled with selective oxidation of benzylamine is demonstrated. The optimized PdSA+C/TiO2‐VO photocatalyst containing Pd single atoms (SAs), clusters (C), and VOs exhibits much superior performance to those of TiO2‐VO and PdSA/TiO2‐VO counterparts. The production rates of H2 and N‐benzylidenebenzylamine over PdSA+C/TiO2‐VO are 52.7 and 1.5 times those over TiO2‐VO, respectively. Both experimental and theoretical studies have elucidated the synergistic effect of Pd SAs, clusters, and VOs on TiO2 in boosting the photocatalytic reaction. The presence of Pd SAs facilitates the generation and stabilization of abundant VOs by the formation of PdOTi3+ atomic interface, while Pd clusters promote the photogenerated charge separation and afford the optimum active sites for H2 evolution. Surface VOs of TiO2 guarantee the efficient adsorption and dissociation/activation of reactant molecules. This study reveals the effect of active‐site engineering on the photocatalysis and is expected to shed substantial light on future structure design and modulation of semiconductor photocatalysts.

A novel amperometric biosensor for glucose detection was fabricated based on a mimetic multi-enzyme system by combing mimetic enzymes (metal–organic frameworks, MOFs) and glucose oxidase (GOx).

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