The precipitation processes in a Cu–2.8 at% Ni–1.4 at% Si alloy were studied using differential scanning calorimetry (DSC), transmission electron microscopy (TEM) and microhardeness measurements. The analysis of the calorimetric curves from room temperature to 900 K shows the presence of one exothermic reaction attributed to the formation of δ-Ni2Si particles in the copper matrix that was confirmed by Transmission Electron Microscopy (TEM) and EDS microanalysis. The activation energies calculated for the precipitation of δ-Ni2Si was lower than the ones corresponding to diffusion of nickel and silicon in copper. A correlation between of microhardness of the alloy and the formation of δ-Ni2Si particles has been found.