Publication date: 15th December 2025
Electrochemical oxidation of biomass-derived furfural (FF) into value-added furoic acid (FA) offers a sustainable and efficient strategy to replace the kinetically sluggish oxygen evolution reaction (OER) at the anode. Herein, we report the in-situ fabrication of nickel-iron layered double hydroxide (NiFe-LDH) catalysts directly grown on carbon cloth, systematically optimizing their electrocatalytic performance. Additional optimization of the Ni:Fe ratio further enhanced the electrocatalytic activity and selectivity for the furfural oxidation reaction (FOR), significantly surpassing those of fluoride-assisted NiFe-LDH and similarly synthesized NiCo-LDH. The optimized NF-0F catalyst achieved exceptional electrocatalytic activity towards FOR, exhibiting a notably low onset potential of 1.39 V vs. RHE. In contrast, the competing OER had a higher onset potential of 1.52 V vs. RHE, highlighting FF oxidation as a substantially more energy-efficient anodic pathway. Detailed mechanistic investigations using in situ Raman spectroscopy revealed an electrochemical-chemical (EC) coupling mechanism through the structural dynamic transformation of catalysts. Electrochemical impedance spectroscopy coupled with Distribution of Relaxation Time (EIS-DRT) analysis provided quantitative insights into distinct reaction kinetics, clearly demonstrating significantly faster electron transfer and catalytic turnover for FOR compared to OER. This study presents scalable and fluoride-free electrocatalysts, offering a comprehensive mechanistic understanding of biomass-derived substrate oxidation. Such insights pave the way toward integrated and sustainable electrochemical systems that combine biomass valorization and efficient hydrogen production.
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