Scalable Ru‐Doped Pt/NiFe‐LDH Catalyst via Pulse Electrolysis Enables Stable Glycerol Oxidation to Glyceric Acid at High Current Density

ABSTRACT Selective electrooxidation of glycerol (GLY) to glyceric acid (GLA) offers a promising route for GLY valorization but remains hindered by limited activity and stability. Herein, we report a scalable self‐corrosion strategy for large‐area fabrication of a Ru‐doped Pt/NiFe‐LDH catalyst on Ni foam (PtRu/NiFe‐LDH) with an area of up to 36 cm 2 . The incorporation of Ru modulates the electronic structure, enhances the adsorption of both OH − and GLY, and lowers the free energy barrier for OH* formation, thereby significantly boosting catalytic activity to achieve a recorded current density of 439.5 mA cm − 2 . Furthermore, pulse electrolysis effectively suppresses the formation of PtO x , ensuring long‐term stability. When integrated into a GLY oxidation‐assisted hydrogen evolution system, this bifunctional catalyst reduces the cell voltage by 1.01 V relative to conventional water splitting, while delivering 78.5% selectivity towards GLA and stable operation for over 120 h. This work establishes a viable pathway toward the industrialization of selective electrochemical oxidation of GLY to GLA by integrating advanced catalyst design with optimized electrolyzer configuration.