We used CaCl 2 and NH 4 F from Merck Company for synthesis CaF 2 NPs. We synthesized CaF 2 Nanoparticales (NPs) using Co-precipitation and hydrothermal method successfully. The synthesized NPs were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), UV-Vis spectroscopy and Photoluminescence (PL) techniques. The XRD results indicated the formation of CaF 2 NPs with Cubic phase and the crystallite size is estimated using Scherrer’s formula to be in the range 20–27nm for the powders prepared by co-precipitation and 20–31nm for hydrothermal methods, respectively. TEM images revealed the grains have almost spherical shape. Optical absorption spectrum shows a strong absorption edge at about 300nm.