Nanostructured metal-nitrides have attracted tremendous interest as a new generation of catalysts for electroreduction of CO₂, but these structures have limited activity and stability in the reduction condition. Herein, we report a method of fabricating FeN/Fe₃N nanoparticles with FeN/Fe₃N interface exposed on the NP surface for efficient electrochemical CO₂ reduction reaction (CO₂RR). The FeN/Fe₃N interface is populated with Fe−N₄ and Fe−N₂ coordination sites respectively that show the desired catalysis synergy to enhance the reduction of CO₂ to CO. The CO Faraday efficiency reaches 98% at −0.4 V vs. reversible hydrogen electrode, and the FE stays stable from −0.4 to −0.9 V during the 100 h electrolysis time period. This FeN/Fe₃N synergy arises from electron transfer from Fe₃N to FeN and the preferred CO₂ adsorption and reduction to *COOH on FeN. Our study demonstrates a reliable interface control strategy to improve catalytic efficiency of the Fe–N structure for CO₂RR.

Utilization of semiconductor photocatalyst materials to degrade pollutants for addressing environmental pollution problems has become a research focus in recent years. In this work, a 2D/2D S-scheme crystalline carbon nitride (CCN)/BiOIO₃ (BOI) van der Waals heterojunction was successfully constructed for effectively enhancing the degradation efficiency of antibiotic contaminant. The as-synthesized optimal CCN/BOI-3 sample exhibited the highest efficiency of 80% for the photo-degradation of tetracycline (TC, 20 mg/L) after 120 min visible light irradiation, which was significantly higher than that of pure CCN and BOI. The significant improvement in photocatalytic performance is mainly attributed to two aspects: (i) the 2D/2D van der Waals heterojunction can accelerate interface carriers’ separation and transfer and afford sufficient active sites; (ii) the S-scheme heterojunction elevated the redox capacity of CCN/BOI, thus providing a driving force for the degradation reaction. The degradation pathways of TC for the CCN/BOI composite were investigated in detail by liquid chromatography-mass spectrometry (LC-MS) analysis. This work provides a design idea for the development of efficient photocatalysts based on the 2D/2D S-scheme van der Waals heterojunctions.