Abstract <p>This work explores the influence of synthesis time and annealing temperature on the physiological and morphological properties of titanium dioxide (TiO₂) nanoparticles. TiO₂ nanoparticles were synthesized through a sol–gel method and subjected to varying synthesis durations and annealing temperatures to evaluate their impact on nanoparticle characteristics. Detailed analysis was performed using X-ray diffraction (XRD) to assess crystallinity, and field emission scanning electron microscopy (FESEM) was employed to evaluate particle morphology. Results demonstrated that extended synthesis times led to enhanced crystallite growth, while higher annealing temperatures significantly influenced the transformation of crystallite phase from anatase to rutile, thus altering the nanoparticle morphology. Furthermore, the physical properties were highly dependent on the annealing conditions, with a direct correlation to the degree of crystallization and particle size distribution. Cyclic Voltammetry was carried out in dark and illuminated conditions to study the photoelectrical properties of the materials. This work emphasises the critical role of fabrication and thermal treatment parameters in tailoring the properties of TiO₂ nanoparticles for specific applications in catalysis, photovoltaics, and biomedical fields.</p>