NiO-CuO nanocomposites were synthesized via precipitation method by using a cationic precursor [(nickel acetate dihydrate, Ni(CH₃CHOO)₂.2H₂O), copper acetate dihydrate, (Cu(CH₃CHOO)₂.2H₂O)], an anionic precursor (alkali hydroxide, NaOH), complexing agent (2-hydroxy propane-1,2,3-tricarboxylic acid, C₆H₈O₇), and mono hydric alcohol (monohydoxymethane, CH₃OH)) as a solvent. The prepared (NiO-CuO) nanocomposites were characterized by physico-chemical studies such as X-ray diffraction (XRD), energy dispersive X-ray (EDX), scanning electron microscopy (SEM), optical absorption (UV) and photoluminescence (PL). The optical absorption spectra exhibit that the band gap energies of the NiO-CuO nanocomposite decrease with the increase in the calcination temperature, which can be attributed to the improvement in the crystallinity of the NiO-CuO. The PL intensity of the NiO-CuO nanocomposite peaks which decreased with the increase in the calcinations temperature was observed from the PL spectra; it was due to the lesser oxygen vacancy defects that occurred. The schematic formation of the NiO-CuO nanocomposite is also discussed.