In this study, Ni/NiO nanocomposites were prepared using simple, environment-friendly and lowcost solid-state thermal decomposition method from nickel (II) Schiff base complex at 400 and 500oC for 3 hours. The Ni/NiO nanocomposites were characterized with Fourier transformed infrared spectroscopy (FT-IR), X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and X-Ray fluorescence (XRF). Results of XRD and XRF confirmed that the nanocomposite products contain a mixture of nickel and nickel oxide. The Ni or NiO content varied with the temperature used for the synthesis. Upon increasing the temperature from 400 to 500oC, the amount of NiO was found to be increased due to a complete oxidation of Ni to NiO. The TEM images demonstrated that the composites were spherical with a distribution size of about 10-30 nm. In addition, the products displayed reasonable electrochemical performance.