An ion exchange method has been developed to separate no-carrier-added 6 4 Cu from irradiated Ni target. The target is first dissolved in nitric acid and the solution is evaporated to dryness and the residue is dissolved in an ethanol-HCl solution. Cu, Co and Ni in ethanol-HCl solution are then absorbed on an anion exchange column. Co and Ni are removed from the column by eluting with 72% ethanol-0.3mol/l HCl. Finally, the 6 4 Cu is eluted with water. For separating Ni from Co isotopes and recovering the 6 4 Ni target, the eluate of 72% ethanol-0.3mol/l HCl is evaporated to dryness, the residue is dissolved in a concentrated HCl solution, and loaded to an another column, Ni is eluted by 9mol/l HCl, while Co remains on the column. The procedure developed has been successfully applied for the production of no-carrier-added 6 4 Cu from enriched 6 4 Ni generated by the reaction 6 4 Ni(p,n) 6 4 Cu using a cyclotron. The decontamination of Co in Cu fraction is higher than 99% and recoveries of 6 4 Cu and 6 4 Ni are higher than 95%.