M 1 II-M 2 II-M 11 II type linear complexes (where M 1 = Ni 2+, Cu 2+ and M 2 = Cu 2+, Zn 2+, Co 2+ and Cd 2+ were prepared and dissolved in dimethyl sulfoxide. They were then electrodeposited on mild steel surfaces by the use of rotating disc electrodes. The deposition potentials were determined from cyclic voltammetric i-E scans. The metal films deposited on mild steel surfaces were characterized with atomic absorption spectrometer (AAS), X-ray fluorescence (XRF) and ion chromatography (IC) methods. Although the stoichiometric quantity of M 2 metal cation was half of the M 1 metal cation in the complex, the amount of M 2 metal deposited upon the surface was markedly greater. The amount of M 2 ion deposited on the surface was found to increase with the hardness of the ion. The X-ray diffraction (XRD) patterns showed that the excessively deposited metal on the surface was in metallic form as wellas alloy. The size ofthe deposited film particles was investigated by the use of atomic force microscope (AFM) technique and the particles were observed to be bigger than nanoparticle size. © FSCT and OCCA 2009.