Electrodeposition of Sm-Co alloy in DMF solution was studied by cyclic voltammetry and potentiostatic deposition at room temperature. The results show that small amount of water in a solution of Sm(NO 3) 3+CoCl 2+DMF blocked the electrodeposition of Sm-Co due to the formation of nonconductive Sm(OH) 3 film on the cathode surface. Citric acid could buffer the pH change and inhibit the precipitation of Sm(OH) 3 on the cathode surface which makes the co-deposition of Sm and Co easy. Potentiostatic deposition was carried out on copper electrode in Sm(NO 3) 3+CoCl 2+Citric acid+DMF solution and Sm-Co alloy films were obtained where the content of Sm could be as high as 57 56%.