In this paper, a formaldehyde-free copper electroless plating process was optimized using statistical analysis (Design of Experiment) in order to maximize the adhesion and the electrical conductivity when deposited on carbon-epoxy substrates. The coatings' morphologies, the electrical resistance, and the adhesion vary significantly as function of electroless plating parameters, but among the selected processing parameters, (pH of the electroless solution, temperature, concentration of reducing agent (glyoxylic acid), and concentration of complexing agent (EDTA)) only the temperature and the concentration of the reducing agent resulted to be influencing factors for the deposition process. A multi-objective optimization approach allowed to set the electroless process parameters in order to obtain optimized coatings presenting improved adhesion (scratch test’s critical load CL3 > 30 N) and electrical conductivity (Rs = 1.91 × 10–2 Ω/sq).