The electrocodeposition of alumina particles (primary particle size 13 nm) in a copper matrix was investigated. Three copper plating baths covering a wide pH range were used: an acidic copper sulphate, a neutral pyrophosphate, and an alkaline sorbitol based bath. The highest amount of incorporated particles (ca. 11 wt.% alumina) was found for the pyrophosphate bath. From zeta potential measurements in diluted solutions we concluded that the particles are charged negatively in this electrolyte. A tentative electrostatic model is proposed to explain qualitatively the relation between the surface charge of the particles and the amount of incorporated particles. Furthermore, the microstructure, microhardness and electric conductivity of the layers were characterized.