Abstract. Nickel oxide doped Fe 2 O 3 thin films have been prepared by spray pyrolysis technique on glass substrate. The initial solution was including a 0.1 M/L for both NiCl 2 and FeCl 3 diluted with re-distilled water and a few drops of HCl. The effect of annealing temperature on some optical properties was studied, using UV-Visible spectrophotometer to determine transmittance and absorbance spectra at a thickness of 400 nm. The reflectance increased with increasing annealing temperature, the same behavior observed for absorption coefficient α,extinction coefficient k and refractive index n, while the transmittance decreases slightly with increasing annealing temperature and the optical energy gap was decreased from 2.86 eV before annealing to 2.70 eV at 500 ºC annealing temperature .