ZnO nanoparticles embedded in hollow carbon fiber membrane for electrochemical H2O2 production by two-electron water oxidation reaction

Electrochemical two-electron water oxidation reaction (2e-WOR) provides a promising alternative route for hydrogen peroxide (H₂O₂) production, where the design of earth abundant and environmentally friendly electrocatalysts with both high selectivity and production rate is crucial. Here we report the synthesis of ZnO nanoparticles embedded in hollow carbon fiber membrane as efficient 2e-WOR electrocatalyst by a metal-organic framework engaged electrospinning-pyrolysis method. The resultant ZnO@carbon composite fiber exhibits a foam-like hierarchical structure composed of interconnected hollow carbon nanocubes encapsulated with oxygen vacancy rich ZnO nanocrystals. Owing to the improved selectivity of ZnO, excellent conductivity of carbon fiber, promoted active site exposure and mass transfer of hollow structure, the free-standing membrane electrode shows superior 2e-WOR performances with high selectivity (83.8% at 2.8 V vs. RHE), H₂O₂ generation rate (19.7 μmol cm⁻² min⁻¹) and robust stability.