Recently, several methods has been used for the synthesis of bimetal oxide nanocomposite, however, very few studies are available on the solvent free mechanochemical synthesis of nanomaterials. In this study, mortar and pestle assisted fabrication of copper oxide-zirconium dioxide nanocomposite (CuO-ZrO2 NC) was carried out and was calcined at 300, 600 and 900
°C. The variation in crystallographic parameters was examined through X-ray diffraction (XRD) and the crystallite size was found to be gradually increased with increasing calcination temperature. The morphological changes with increasing calcination temperature were traced during scanning electron microscopy (SEM) analysis. The percentage elemental composition was verified through energy dispersive X-ray (EDX) spectroscopy whereas the functional group analysis was done through Fourier transform infrared (FTIR) spectroscopy, where the intensity of peaks assigned to hydroxyl moiety decreased with increasing calcination temperature. The CuO-ZrO2NCs were used as a photocatalysts for the degradation of the Fluorescein in the presence of solar light and highest photodegradation (77.27 %) was noticed for the CuO-ZrO2 NC calcined at 900 °C.