Abstract: The electrocatalytic oxidation of biomass-derived furfural (FF) feedstocks into 2-furoic 

acid (FA) holds immense industrial potential in optics, cosmetics, polymers, and food. Herein, we 

fabricated CoO/nickel foam (NF) and Cu2O/NF electrodes via in situ pulsed laser irradiation in 

liquids (PLIL) for the bifunctional electrocatalysis of water and FF oxidation evolution reactions 

(OERs and FORs, respectively). Simultaneous oxidation of NF surface to NiO and deposition of 

CoO and/or Cu2O on NF during PLIL offers distinct advantages for enhancing both the OER and 

FOR. CoO/NF electrocatalyst provides a consistently low overpotential of ~359 mV (OER) at 10 

mA/cm2, achieving the maximum FA yield (~16.37 mM) with 61.5% selectivity, 79.5% carbon 

balance, and a remarkable Faradaic efficiency of ~90.1% during 2 h of FOR at 1.43 V (vs. 

reversible  hydrogen  electrode). Mechanistic  pathway  via  in situ  electrochemical–Raman 

spectroscopy on CoO/NF reveals the involvement of phase transition intermediates (NiOOH and 

CoOOH) as surface-active centers during electrochemical oxidation. The carbonyl carbon in FF 

is attacked by hydroxyl groups to form unstable hydrates that subsequently undergo further 

oxidation to yield FA products. This method holds promise for large-scale applications, enabling 

simultaneous production of renewable building materials and fuel.