The effects of addition of polyethylene wax on the synthesis of Cu-Ni alloy (Monel) with 50wt%Ni processed in a high energy ball mill were investigated by X-ray diffraction. The Monel powder was characterized by laser particle size measurement and scanning electron microscopy. The results showed that the addition of wax at the beginning of milling causes a delay in alloy formation, and the particle shape obtained was essentially flaky. However, a strong effect was observed on the shape and particle size distribution when wax was added to the Monel powder with a flaky shape previously processed without wax. The particle shape changed from flake to more irregular and the median particle size decreased from 55 mu m to 7.5 mu m after 4 hours of milling.