Nickel oxide/cobalt phthalocyanine (NiO-CoPc) nanocomposite is synthesized by solvent evaporation method. The synthesized nanocomposite is characterized for thermal, structural, and optical properties. Thermogravimetric and differential thermal analysis results proved the thermal stability of the sample. XRD patterns revealed an average crystallite size of 16 and 17.5 nm, respectively, for the pure and nanocomposite samples. The formation of NiO/CoPc nanocomposite is confirmed by the FTIR results. The characteristic B and Q bands of metal phthalocyanines are visible in the absorption spectrum. A decrease in band gap and an enhanced absorption in the visible region are observed for the nanocomposite. The PL emission spectrum of the nanocomposite exhibits fluorescence quenching which makes them suitable for solar cells and photocatalysis. This work constitutes the first report on the synthesis and characterization of the NiO/CoPc nanocomposite.