This work aims to fabricate of polyethylene oxide (PEO)/nickel oxide (NiO)/indium oxide (In2O3) films for photo-degradation of dyes pollutants with low cost, low concentration of nanoparticles contents, excellent dispersion and good activity compared of other nanomaterials. The structural and optical characteristics of PEO/NiO-In2O3 films have been investigated. The structural characteristics of films included: optical microscopic, scanning electron microscope and Fourier transform infrared spectroscopy. The optical properties of PEO/NiO-In2O3 films recorded in wavelength range (200-800) nm. The optical properties results of PEO/NiO-In2O3 films indicated that the absorbance (A) of PEO rises about 62.5% while the transmittance (T) reduced about 70.7% at lambda = 300 nm, this behavior makes the PEO/NiO-In2O3 nanostructures are suitable for different photonics fields. The energy gap reduces about 55.3% when the In(2)O(3)NPs content reached (5.4 wt%), this behavior make it may be considered as a key for optical and electronic applications. The optical constants of PEO: absorption coefficient (alpha), refractive index (n), extinction coefficient (k), real (epsilon(1)) and imaginary (epsilon(2)) parts of dielectric constants and optical conductivity (sigma(op)) enhanced with doping of NiO NPs and NiO-In2O3 NPs, this performance make the PEO/NiO-In2O3 nanostructures can be considered as good optical materials for photo-degradation, electronics and optics applications. The PEO/NiO-In2O3 nanomaterials tested for photodegradation of dyes pollutants. The final results indicated that the PEO/NiO-In2O3 nanomaterials can be utilized for excellent photodegradation efficiency reached (88.3%) for the sample (5.4 wt% In2O3 NPs) with few cost and good dispersion compared of other nanomaterials.