| Summary: | Fe-Ce/layered double hydroxides (LDHs) were synthesized via a facile route by exploiting the “structural memory” of the LDH when the calcined MgAlLDH and ZnAlLDH were reconstructed in the aqueous solutions of FeSO<sub>4</sub>/Ce(SO<sub>4</sub>)<sub>2</sub>. XRD analysis shows the formation of heterostructured catalysts that entangle the structural characteristics of the LDHs with those of Fe<sub>2</sub>O<sub>3</sub> and CeO<sub>2</sub>. Furthermore, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, TG/DTG, SEM/EDX and TEM results reveal a complex morphology defined by the large nano/microplates of the reconstructed LDHs that are tightly covered with nanoparticles of Fe<sub>2</sub>O<sub>3</sub> and CeO<sub>2</sub>. Calcination at 850 °C promoted the formation of highly crystallized mixed oxides of Fe<sub>2</sub>O<sub>3</sub>/CeO<sub>2</sub>/ZnO and spinels. The photo-electrochemical behavior of Fe-Ce/LDHs and their derived oxides was studied in a three-electrode photo-electrochemical cell, using linear sweep voltammetry (LSV), Mott–Schottky (M-S) analysis and photo-electrochemical impedance spectroscopy (PEIS) measurements, in dark or under illumination. When tested as novel catalysts for the degradation of phenol from aqueous solutions, the light-driven catalytic heterojunctions of Fe-Ce/LDH and their derived oxides reveal their capabilities to efficiently remove phenol from water, under both UV and solar irradiation.
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