Combining Underpotential Deposition and Soft‐Template to Construct Ordered Mesoporous PdSb Nanocubes for Selective Ethylene Glycol Oxidation

ABSTRACT Rational design of bimetallic nanocrystals with ordered mesoporous architectures and precise compositional control is critical for high‐performance electrocatalysis, yet it remains a significant challenge. Herein, we report the synthesis of PdSb ordered mesoporous cubes (PdSb OMCs) via a seed‐mediated growth strategy, driven by the synergistic interplay between Sb underpotential deposition (UPD) and hexadecyltrimethylammonium bromide (CTAB) soft‐template. Mechanistic studies reveal that the Sb ions and CTAB play decisive roles in directing the ordered self‐assembly of surfactant micelles on the Pd surface, enabling the controlled growth of a uniform mesoporous alloy shell. Consequently, the resulting PdSb OMCs exhibit reliable and steady electrocatalytic performance for the ethylene glycol oxidation reaction, directing the conversion of ethylene glycol to glycolic acid with a selectivity of ∼95%. Experimental investigations suggest that this enhancement stems from the unique ordered mesoporous architecture, which facilitates mass transport, and the electron‐rich Pd surface modulated by Sb, which suppresses C─C bond cleavage. This work provides a promising approach for UPD‐assisted soft‐template synthesis and offers insights into designing electrocatalysts for value‐added chemical production.