| Summary: | Copper and its oxides are the main catalyst materials able to promote the formation of hydrocarbons from the electrocatalytic CO<sub>2</sub> conversion. Herein, we describe a novel preparation method for carbon-doped copper oxide catalysts based on an oxidative thermal treatment of copper-containing deep eutectic solvents (DES). XRD and EDX analysis of the samples show that thermal treatment at 500 °C in air for a prolonged time (60 min) provides exclusively carbon-doped copper(II) oxide catalysts, whereas shorter calcination time leads to a mixture of less oxidized forms of copper (Cu<sub>2</sub>O and Cu<sup>0</sup>), CuO, and a higher carbon content from the DES. Chronoamperometry of the electrode containing the prepared materials in 0.5 M KHCO<sub>3</sub> electrolyte show the reduction of CuO to less oxidized copper species. The materials prepared by the use of different DES, copper precursors and calcination times were used as electrocatalysts for the electrochemical CO<sub>2</sub> reduction. Chemical analysis of the products reveals an enhanced selectivity toward C2 and C3 products for the catalyst prepared from the DES galactose-urea with copper nanoparticles and calcination for 60 min in air. The electrocatalytic activity of the prepared materials were compared to commercial CuO and showed a higher product concentration at −1.7 V vs. Ag/AgCl, with formation rates of 7.4, 6.0, and 10.4 µmol h<sup>−1</sup> cm<sup>−2</sup> for ethanol, n-propanol, and ethylene, respectively.
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