This work used the Sol-Gel method to prepare NiO nanoparticles that were both undoped and doped by Copper and Tin. According to the XRD data, every sample is polycrystalline.Scherrer's equation was used to calculate the crystallite size of the samples, and it was found that the crystallite size (7.2841, 4.97262, 4.97262, 10.07331, 5.63056 and 5.39887 nm) for undoped (NiO), and doped (d1, d2, d3, d4 and d5) respectively, were d is the doping ratio.According to an FTIR spectrum of NiO NPs, showed absorption peaks at the two regions (1566 and 1332 cm -1 ) Due to the bonds (H-O-H, C-H) respectively, FESEM image for undoped and doped of NiO nanoparticle, shows that the structure with a spherical shape. The spectrum also showed absorption peaks in the region (400-500 cm -1 ) which is due to the stretching vibration of the (Ni-O) band. The percentage filled by grafting atoms (Cu + Sn). Optical measurements show that the transmittance increases as wavelength increases. The photoluminescence measurement shows that the sample before doping has a peak value of (489.3 nm), and the double-grafted grains record peak values at (367.2, 368.1, 681.1, 582.2, 772.7, 438.6 nm) for pure NiO, d1, d2, d3, d4 and d5) respectively, and the value of the energy gap was (3.377, 3.369, 1.821, 2.129, 1.704 and 2.827 eV) for (pure NiO, d1, d2, d3, d4 and d5) respectively.