The composition, crystal structure and habit of Cu-Au and Cu-Al particles prepared by evaporation of mother alloys in argon gas were investigated by X-ray diffraction and electron microscopy. With the progress of evaporation, the Al concentration of the Cu-Al particle changed so as to fall at about 35 at%, while the Au concentration of the Cu-Au particles always increased up to 100 at%, irrespective of the composition of the starting materials. Both the Cu-Au particles over the whole range of Au concentration and the Cu-Al particles containing up to about 35 at% Al showed the same well-defined crystal habits as pure metal particles, corresponding to their crystal structures.