The dye-sensitized solar cells made of NiO@ZnO nanoparticles were synthesized by a novel Pechini route using different NiO molar concentration ratios. The thermal, structural morphological, optical and electrical properties of the prepared samples were investigated using thermal gravimetric analysis and differential scanning calorimetery (TGA/DSC), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), FT-IR and Raman spectroscopy, UV-diffuse reflectance (UV-DRS), photoluminescence (PL) and current-voltage (I-V) measurements. The success of doping process was confirmed by the XRD patterns, which revealed the existence of new peak at 43.2° corresponding to secondary phase NiO. UV spectra exhibited red shifts in NiO doped ZnO NCs and PL spectra showed strong emission band at 355 nm. The doping of ZnO with NiO was intended to enhance the surface defects of ZnO. The current-voltage measurements showed an improvement of the short circuit photocurrent (Jsc) and fill factor (FF) and a decrease in the open circuit voltage (VOC) for dye-sensitized solar cell (DSSC) based on NiO-ZnO NCs. A clear enhancement in efficiency of DSSC from 1.26±0.10 % for pure ZnO to 3.01±0.25 % for NiO-ZnO NCs at the optimum doping with 1.5 mol% of NiO to ZnO (ZN1.5) was observed. The obtained material can be a suitable candidate for photovoltaic applications.