The role of molybdenum in promoting the electrochemical glycerol oxidation performance of iron–molybdenum layered double hydroxides†

The glycerol oxidation reaction (GOR) emerges as a promising alternative to the sluggish and energy-intensive oxygen evolution reaction, offering dual benefits of reducing the energy input required for hydrogen production via electrochemical water splitting and generating value-added organic chemicals. However, the practical implementation of the GOR is constrained by the limited availability of active, selective, and stable electrocatalysts. Here, we report the synthesis of iron–molybdenum layered double hydroxides (FeMo-LDHs) via a facile electrochemical deposition method and systematically investigate the impact of Mo incorporation on the catalytic performance. Morphological characterization reveals that FeMo-LDH adopts an ultrathin nanosheet structure, while electronic analysis and theoretical calculations indicate that Mo donates electrons, thereby increasing the electron density around Fe sites. Electrochemical evaluations show that the FeMo-LDH exhibits faster reaction kinetics, lower charge transfer resistance, and higher electrochemical active surface area compared to Fe(OH)₃, thereby contributing to a decrement of 40 mV in overpotential at 100 mA cm⁻². Additionally, FeMo-LDH shows a faradaic efficiency of >80% for formate production and a durability of 50 hours. Therefore, this work introduces an efficient, stable, and easily fabricated FeMo-LDH catalyst, emphasizing the crucial role of Mo incorporation in enhancing the electrochemical GOR performance of FeMo-LDHs.