This dataset comprises experimental data generated during a master's research project focused on the synthesis and characterization of Au–CuO/C heterodimer catalysts and CuO/C materials. The data include structural, morphological, and spectroscopic analyses obtained from techniques such as TEM, XPS, UV-Vis spectroscopy, and electrochemical measurements. The dataset supports the evaluation of material properties and their relationship with catalytic performance, covering different compositions and experimental conditions.