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Palladium catalysts have attracted widespread attention as advanced electrocatalysts for the formic acid oxidation (FAO) due to their excellent electrocatalytic activity and relatively high abundance. At present, electrodeposition methods have been widely developed to prepare small-sized and highly-dispersed Pd electrocatalysts. However, the customary use of surfactants would introduce heterogeneous impurities, which requires complicated removal processes. In this work, we reported a two-step electrochemical method that employed square-wave potential treatment (SWPT) to modify electrodeposited Pd particles without the use of capping agents. Under the SWPT with a mixed frequency, Pd particles show significantly reduced size and more dispersed distribution, exhibiting a high mass activity of 1.43 A mg−1 toward FAO, which is 4.6 times higher than the counterpart of commercial Pd/C. The increase in electrocatalytic activity of FAO is attributed to the highly developed surface of palladium particles uniformly distributed over the support surface.

Palladium Particles Modified by Mixed-Frequency Square-Wave Potential Treatment to Enhance Electrocatalytic Performance for Formic Acid Oxidation