Summary: | A ZnO-Fe-MXene nanocomposite was fabricated and examined with diverse spectroscopic techniques. The hexagonal structure of ZnO, MXene, and ZnO-Fe-MXene nanocomposites were validated through XRD. FTIR showed the characteristic vibrational frequencies of ZnO and MXene. The micrographs of the SEM showed nanoparticles with a flower-like structure. The electrocatalytic reduction efficiency of ZnO-Fe-MXene nanocomposite was analyzed through cyclic voltammetry and electrochemical impedance spectroscopy methods. The ZnO-Fe-MXene electrode was confirmed to have a high current density of 18.75 mA/cm<sup>2</sup> under a CO<sub>2</sub> atmosphere. Nyquist plots also illustrated a decrease in the impedance of the ZnO-Fe-MXene layer, indicating fast charge transfer between the Zn and MXene layers. Additionally, this electrochemical study highlights new features of ZnO-Fe-MXene for CO<sub>2</sub> reduction.
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