The Cu 8 4 Co 1 6 alloy melt processed by differential thermal analysis, electromagnetic levitation and drop tube experiences a liquid phase separation when it is undercooled into the metastable miscibility gap. The phase separation and coagulation processes are mainly controlled by the degree of undercooling, cooling rate and convection level in the containerless states. Disperse structures have been formed in droplets solidified during free fall in the drop tube.