Electro-Fenton’s process is a well-known electrochemical advanced oxidation processes (EAOPs) fordegradation and mineralization of refractory pollutants. The nature of cathode material used in thisprocess is essential parameters that determine the efficiency of the process because the cathode controlsthe generation and regeneration of Fenton’s reagents (i.e. H2O2 and Fe2+)1. In this study we prepared forthe first time, a layered double hydroxide (LDH) coated carbon-felt that acts as a suitable cathode interms of Fenton’s reagents production for electro-Fenton degradation of organic pollutants. Cobalt-iron(Co-Fe) LDH was deposited on a raw carbon-felt via in-situ solvo-thermal process at different treatmenttemperature (70 – 120 oC) and concentrations of Co2+/Fe3+. The X-ray diffraction pattern of both powderLDH and coated carbon-felt showed a well crystalline structure with 00l characteristic peaks of LDH andhuge peak associated with carbon (Fig. 1a). The as-prepared cathode showed superior mineralizationefficiency (93% TOC removal) when compared to raw carbon-felt cathode (66%) with addition of 0.2mM Fe2+ for treatment of acid orange II in Electro-Fenton process (Fig b). The better mineralizationobtained with as-prepared cathode is attributed to two phenomena: (i) co-catalyst effect of the Co releasedfrom the LDH (ii) controlled/gradual release of both catalyst that eliminate waste reactions. The preparedcathode is a suitable and promising cathode material for application in electro-Fenton process forwastewater treatment.