Carbon‐Anchored Molybdenum Oxide Nanoclusters as Efficient Catalysts for the Electrosynthesis of Ammonia and Urea

The electrochemical NO₃ ⁻ reduction and its coupling with CO₂ can provide novel and clean routes to synthesize NH₃ and urea, respectively. However, their practical application is still impeded by the lack of efficient catalysts with desirable Faradaic efficiency (FE) and yield rate. Herein, we report the synthesis of molybdenum oxide nanoclusters anchored on carbon black (MoOx /C) as electrocatalyst. It affords an outstanding FE of 98.14 % and NH₃ yield rate of 91.63 mg h⁻¹ mgcat. ⁻¹ in NO₃ ⁻ reduction. Besides, the highest FE of 27.7 % with a maximum urea yield rate of 1431.5 μg h⁻¹ mgcat. ⁻¹ toward urea is also achieved. The formation of electron-rich MoOx nanoclusters with highly unsaturated metal sites in the MoOx /C heterostructure is beneficial for enhanced catalytic performance. Studies on the mechanism reveal that the stabilization of *NO and *CO₂ NOOH intermediates are critical for the NH₃ and urea synthesis, respectively.