Photoassisted Electrocatalytic Oxidation of Glycerol to Formic Acid over Heterostructure Cu₂S/Ni₃S₂.

heterostructure promotes charge transfer, the CTAB-regulated morphology increases the electrochemically active surface area (ECSA), and illumination improves interfacial reaction kinetics while suppressing the competing oxygen evolution reaction (OER). Operando spectroscopy further suggests that NiOOH is the active oxidizing species and that glycerol is converted to formic acid through sequential oxidation and C-C bond cleavage steps. This work provides an effective strategy for coupling heterostructure engineering and photoassisted electrocatalysis to enhance selective glycerol upgrading.