<p> Ammonia synthesis is key to stable food production as it is present in most of the common fertilizers. However, its synthesis is very energy intensive and leads to significant CO₂ emissions. An alternative approach is to electrochemically generate ammonia from nitrates. In neutral-to-alkaline media, copper and its alloys have shown promising activity for this reaction, but it is difficult to assess which catalyst is the most promising given the variety of synthetic approaches and experimental conditions (pH, nitrate concentration, stirring, cell design, etc.) used in the literature. In this work, Cu_xM_100−x (M = Co, Fe or Ni) nanoparticles were prepared by the same technique, pulsed laser ablation in liquids, in the same conditions to allow for an easier comparison. Their activity and selectivity for the electroreduction of nitrates to ammonia was then assessed. Analysis of transmission electron microscope images revealed that Cu, Cu₅₀Co₅₀ and Cu₅₀Ni₅₀ had a size of ≈ 12&#xa0;nm whereas Cu₅₀Fe₅₀ nanoparticles were ≈ 21&#xa0;nm. All nanoparticles were copper-rich compared to their targets, as determined by emission spectroscopy. Of the four catalysts tested, Cu₅₀Ni₅₀ had the lowest onset potential for nitrate reduction. However, Cu₅₀Ni₅₀ (as Cu and Cu₅₀Fe₅₀) produces mostly nitrite at this potential (~ 90%). Cu₅₀Co₅₀ nanoparticles were found to display the best selectivity for ammonia production. In the optimal conditions of this study, a maximum FE of 86 ± 9 at − 1.1&#xa0;V was observed for Cu₅₀Co₅₀ NPs on carbon cloth with a partial current density for ammonia production of − 8 ± 2&#xa0;mA cm⁻².</p> Graphical Abstract <p></p>