The microstructure of Cu75Cr25 alloys was investigated by using vacuum non-consumable arc melting, electromagnetic levitation and splat quenching. The microstructure and solidification behavior of the Cr-rich were investigated by scanning electron microscopy (SEM). The results showed that inhomogeneous Cr-rich dendrite distributes on Cu-rich matrix for arc melted alloys. The microstructure consisting of a fine dispersion of Cr-rich dendrite in a Cu-rich matrix for electromagnetic levitated alloys. However, the morphology and size of the Cr-rich phase vary greatly with the cooling rate for splat quenched alloys. The Cr-rich phase show both dendrites and spheroids, this means liquid phase separation occurred during rapid solidification.