<p>Controlled modulation of the structural, optical, and magnetic properties of TiO₂ through doping and adjustments in the synthesis route is crucial for optimizing its performance in technological applications. In this study, the effect of two distinct sol–gel routes on the synthesis of pure and Co²⁺- and Fe³⁺-doped TiO₂ nanoparticles was comparatively investigated, evaluating how variations in synthesis parameters directly influence defect formation, bandgap narrowing, and magnetic behavior. X-ray diffraction confirmed that the anatase phase was predominant in all synthesized TiO₂ samples. Raman spectroscopy indicated that the synthesis route, dopant type, and increasing dopant concentration reduced the intensity of the characteristic mode at 144 cm⁻¹. Diffuse reflectance spectroscopy revealed that method 1 yielded the lowest bandgap values. Increasing dopant concentration led to higher Urbach energy, with TiO₂ doped with 5% Co via method 2 exhibiting the highest value (U_E = 2073 meV), suggesting enhanced defect generation. XPS analysis confirmed the elemental composition and oxidation states of the dopants. Scanning electron microscopy revealed that doping favored the formation of agglomerates, whereas pure samples exhibited spherical nanoparticle morphology, which was corroborated by BET results. Room-temperature magnetic measurements evidenced diamagnetic behavior for pure TiO₂ and paramagnetic behavior for doped samples, with a slight ferromagnetic contribution indicated by the hysteresis loops. The coercive field (Hc) values ranged from 5 to 80 Oe, higher in Co-doped samples. The reduction in bandgap and the observed magnetic properties were attributed to the presence of dopants in the TiO₂ lattice and the employed synthesis route.</p><p></p>