Advanced Fe-doped carbon xerogels as bifunctional electro-catalysts for targeted hydroxyl radical production and superior electro-Fenton pollutant removal in water Ramírez Valencia, Lilian Daniela Bailón García, Esther Carrasco Marín, Francisco Álvarez Merino, Miguel Ángel Pérez Cadenas, Agustín Francisco Bifunctional Hydrothermal iron carbide Encapsulation Electro-Fenton Hydroxyl radicals The authors acknowledge the support by Grants PID2021-127803OB-I00 and CNS2023-144680 funded by MICIU/AEI/https://doi.org/10.13039/501100011033 and by “ERDF A way of making Europe” and “European Union NextGenerationEU/PRTR”, respectively. This article is part of the reference aid DGF_PLSQ_2023_00183 granted by Consejería de Universidad, Investigación e Innovación of the Regional Government of Andalusia, funded by the Andalusia 2021-2027 FEDER Operational Programme. Esther Bailón-García is grateful for her grant RYC2020-029301-I funded by MCIN/AEI/https://doi.org/10.13039/501100011033 and, by “ESF Investing in your future”. Lilian D Ramírez-Valencia acknowledge “MINCIENCIAS” for supporting their PhD studies. Funding for open access charge: Universidad de Granada / CBUA. Bifunctional catalysts for H2O2 production via oxygen reduction reaction (ORR) and OH• generation via Fenton reaction are fundamental for the development and optimization of Electro-Fenton technology. In this context, Fe- doped carbon xerogels have been synthesized by sol-gel polymerization under hydrothermal conditions, which allowed the efficient encapsulation of iron nanoparticles (Fe3C-type crystalline species) within the carbon matrix. This strategy enabled control over the selectivity of the materials towards a three-electron pathway, favoring the direct production of hydroxyl radicals (OH•). Moreover, a good balance between graphitization degree and micro-mesoporous structure resulted in high electrochemical performance in ORR, reaching a kinetic current density as high as 11.56 mA/cm2 at −0.45 V and 32.66 mA/cm2 at −0.80 V. This remarkable performance was reflected in Electro-Fenton experiments, achieving 94% degradation of tetracycline after 8 h, demonstrating the bifunctional effectiveness of the synthesized catalysts. 2025-07-10T07:29:11Z 2025-07-10T07:29:11Z 2025-07-02 journal article L.D. Ramírez-Valencia et al. Chemical Engineering Journal 519 (2025) 165565. https://doi.org/10.1016/j.cej.2025.165565 https://hdl.handle.net/10481/105160 10.1016/j.cej.2025.165565 eng info:eu-repo/grantAgreement/EC/NextGenerationEU/CNS2023-144680 http://creativecommons.org/licenses/by-nc-nd/4.0/ open access Attribution-NonCommercial-NoDerivatives 4.0 Internacional Elsevier