This experimental thesis was carried out in the United States at the University of California, Irvine (UCI), under the supervision of Prof. Stefania Specchia and Prof. Plamen Atanassov, together with his research group. The work focused on the synthesis, characterization, and evaluation of the electrocatalytic activity of different copper-based catalysts for the electrochemical reduction of carbon dioxide (CO₂RR). In particular, three new catalysts were synthesized — two copper-based and one containing silver nanoparticles — using a synthesis method previously employed by the group for platinum- and cobalt-based catalysts, adapted here to the chemical compounds of interest. After synthesis, the research shifted to their characterization, using X-ray diffraction (XRD) and transmission electron microscopy (TEM) to verify the crystalline phases, as well as the morphology and particle size of the obtained catalysts.