Abstarct: Electrodeposition is one of the simple and applicable methods in the field of mextallic thin film growth. By using this method, thin films of Ni and Ni-Co-Cu alloy from their citrate-sulphate solution were prepared. In order to investigate the potentiodynamical behavior of electrolyte, the related CV curves were studied. Then from this study, the suitable voltages of deposition were selected. The films were deposited on Cu substrate with preferred (200) orientation and Si (111) substrate and the effects of changing electrolyte temperature on films were investigated. The results of X-ray diffraction spectra revealed all films have fcc structure on both substrates. It observed that for Ni-Co-Cu film on the Cu substrate, by increasing deposition voltage to -1.1 V and decreasing copper concentration to 0.003 mol.dm-3 in electrolyte, films structure changes from homogeneous to cobalt cluster formation on Cu substrate. This phenomenon was not happened for Si substrate. The results of X-ray diffraction spectra of the Ni-Co-Cu films on Si substrate which were prepared in electrolyte temperature of 〖45〗^° c , 〖55〗^° c and 〖65〗^° c showed that increasing electrolyte temperature causes increase in grain size and decrease in copper percentage in alloy. By increasing temperature from 〖45〗^° c to 〖65〗^° c copper percentage decreased in alloy. Surface morphology of the films was studied by atomic force microscope (AFM). Some break trails in the nickel film grown on the Si substrate were observed, while the film grown on Cu substrate was relatively smooth. The surface of Ni-Co-Cu film on Si substrate which was deposited by electrolyte at 〖65〗^° c , was more smoother and had bigger grain size. CHA curves of Ni-Co-Cu showed, without stirring in -0.85 V, only copper deposited. CHA curves with stirring exhibited semi-state current density after increasing current in peaks. The results of magnetic studies with alternating gradient force magnetometer (AGFM) revealed maximum magnetization occur for Ni-Co-Cu films on Si substrate, with 〖65〗^° c electrolyte. Keywords: Electrodeposition, X-ray diffraction (XRD), cyclic voltammogram (CV), Ni-Co-Cu alloy, AGFM, Ni thin film, chronoamperometry (CHA). Electrodeposition is one of the simple and applicable methods in the field of mextallic thin film growth. By using this method, thin films of Ni and Ni-Co-Cu alloy from their citrate-sulphate solution were prepared. In order to investigate the potentiodynamical behavior of electrolyte, the related CV curves were studied. Then from this study, the suitable voltages of deposition were selected. The films were deposited on Cu substrate with preferred (200) orientation and Si (111) substrate and the effects of changing electrolyte temperature on films were investigated. The results of X-ray diffraction spectra revealed all films have fcc structure on both substrates. It observed that for Ni-Co-Cu film on the Cu substrate, by increasing deposition voltage to -1.1 V and decreasing copper concentration to 0.003 mol.dm-3 in electrolyte, films structure changes from homogeneous to cobalt cluster formation on Cu substrate. This phenomenon was not happened for Si substrate. The results of X-ray diffraction spectra of the Ni-Co-Cu films on Si substrate which were prepared in electrolyte temperature of 〖45〗^° c , 〖55〗^° c and 〖65〗^° c showed that increasing electrolyte temperature causes increase in grain size and decrease in copper percentage in alloy. By increasing temperature from 〖45〗^° c to 〖65〗^° c copper percentage decreased in alloy. Surface morphology of the films was studied by atomic force microscope (AFM). Some break trails in the nickel film grown on the Si substrate were observed, while the film grown on Cu substrate was relatively smooth. The surface of Ni-Co-Cu film on Si substrate which was deposited by electrolyte at 〖65〗^° c , was more smoother and had bigger grain size. CHA curves of Ni-Co-Cu showed, without stirring in -0.85 V, only copper deposited. CHA curves with stirring exhibited semi-state current density after increasing current in peaks. The results of magnetic studies with alternating gradient force magnetometer (AGFM) revealed maximum magnetization occur for Ni-Co-Cu films on Si substrate, with 〖65〗^° c electrolyte.