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NiV2O6 thin films were grown on glass slides with varying thicknesses using nebulizer spray pyrolysis. The impact of thickness on the thin films’ optical, structural, morphological, and electrical characteristics was systematically investigated. X-ray diffraction and micro-Raman analysis confirmed the formation of the triclinic NiV2O6 system. Surface morphology and roughness variations in the as-deposited NiV2O6 films were studied using scanning electron microscopy (SEM) and a profilometer. Optical properties, including optical band gap (Eg), extinction coefficient (k), absorption coefficient (α), and refractive index (n), were determined through optical reflectance and transmittance measurements. The optical energy gap of the as-deposited NiV2O6 films decreased from 2.02 eV to 1.58 eV with increased layer thickness. Furthermore, the photo-detectivity of the films demonstrated an enhancement corresponding to the prolonged spray time. The sensitivity values obtained for visible irradiation were 328, 511, and 433 for samples S1, S2, and S3, respectively. The obtained results can be imputed to the specific porous microstructure.