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NiO-Ni nanocomposite was synthesized by a conventional sol-gel process. Ni-NiO nanocomposite has been fabricated via the thermal decomposition of nickel salts by using glutaric acid as a spacer agent. A possible mechanism was showed which proposed an optimum temperature to remove nickel impurity from composite in calcinations of nickel glutarate. The produced nanoparticles through the thermal decomposition process were characterized by X-ray diffractometer (XRD) and scanning electron microscope (SEM). The chemical structure of the products was studied by Fourier transform infrared (FT-IR) spectroscopy. The mean crystallite size of the obtained nanosized was estimated to be in the range of 22 nm to 41 nm. The thermal behavior of compound was studied by thermal gravimetric (TG) and differential thermal analyses (DTA).