A CeO-NiO nanocomposites have been synthesized by a Sol-Gel method based on polymeric network of polyvinyl alcohol (PVA). In this method mixture solvent of 50:50 ethanol- water was used to dissolve cerium nitrate, nickel nitrate and PVA. The mixture was heated to 800C to form homogeneous gel solution. The obtained gel was slowly heated to evaporate the solvent to form a hard homogeneous gel. The hard gel was calcinated at a temperature of 6000C for 4 hours and 8 hours and converted into nanocomposites. The prepared nanocomposites have been characterized using X-Ray Diffraction, SEM, FTIR, UV-VIS. The size of a nanocomposites haeated at 6000C for 4 hours and 8 hours using scherrer formula comes out to be17 nm and 18.3nm. TEM images of nano composite confirms that the nanoparticles formed are in nanosize. At 4h spectra, absorption first decreases in ultraviolet region and there is absorption peak at 240 nm wavelength . Then absorption peak increase a little in UV region and there is second absorption peak at about 310 nm. It increases further little in UV region and then decreases in the visible region up to 800 nm At 8 h spectra, absorption first decreases fast and there is peak at 220 nm and then it rises exponentially up to 400 nm in ultraviolet region. Absorption curve then remain constant up to 580 nm and then decreases fast in the visible region. Infrared spectroscopy is used to determine presence of certain functional group. The nanocompsite result was confirmed with tem analysis. FTIR spectra shows new peaks at 3838 cm-1 ,3740 cm-1 ,1624 cm-1 , and 412 cm-1 when calcinated for 8 h.