In the present research, 1,2-di[N-2-phenylthio-5-azophenylsalicylidene]ethane (H2L1, 1,3-di[N-2-phenylthio-5-azophenylsali-cylidene]propane(H2L2) and 1,4-di[N-2-phenylthio-5-azophenylsalicylidene]butane (H2L3) were synthesized. ML1,ML2 and ML3 complexes were prepared through the reaction of H2L1,H2L2 and H2L3 with Ni(II) and Co(II) acetate salts. The prepared ligands and their complexes were characterized with FT-IR, 1H-NMR, elemental analysis, conductivity and magnetic measurements, ESI-mass, UV-Vis spectroscopy and cyclic voltammetry. The complexes had monomeric structure according to the mass spectral data. All of the complexes had a six-coordinated octahedral geometry. The electrochemical behavior of the ligands, Ni(II) and Co(II) complexes was investigated by CV in DMF under argon atmosphere. The results show that the coordination of Ni(II) causes the ligands to be deactivated. The voltammogram of Co(II) complexes shows that the reduction of CoL1 is harder than CoL3 and CoL2 is inactive. Their antibacterial activity was investigated and the complexes exhibited better antibacterial activity than the free ligands against selective bacteria. Keywords: Schiff base complexes, 5-azophenylsalicylaldehyde, electrochemical study, antibacterial properties.