Undoped nickel oxide (NiO) thin films were deposited on 500 ∘ C heated glass substrates using spray pyrolysis method at (0.015-0.1 M) range of precursor. The latter was obtained by decomposition of nickel nitrate hexahydrate in double distilled water. Effect of precursor concentration on structural, optical, and electrical properties of NiO thin films was investigated. X-ray diffraction (XRD) shows the formation of NiO under cubic structure with single diffraction peak along (111) plane at 2 = 37.24 ∘ . When precursor concentration reaches 0.1 M, an increment in NiO crystallite size over 37.04 nm was obtained indicating the product nano structure. SEM images reveal that beyond 0.04 M as precursor concentration the substrate becomes completely covered with NiO and thin films exhibit formation of nano agglomerations at the top of the sample surface. Ni-O bonds vibrations modes in the product of films were confirmed by FT-IR analysis. Transparency of the films ranged from 57 to 88% and band gap energy of the films decreases from 3.68 to 3.60 eV with increasing precursor concentration. Electrical properties of the elaborated NiO thin films were correlated to the precursor concentration.