Abstract <p>Pure and Fe-doped Al₂O₃ nanoparticles (NPs) with 1, 2, 3, and 4% Fe were successfully produced using the sol-gel route and the precursors C₉H₂₁AlO₃ and FeSO₄. According to the XRD data, Fe³⁺ ions were substituted in the alumina structure to form a hexagonal Fe-Al₂O₃ nanocomposite with an alpha phase. Scanning Electron Microscopy (SEM) observations showed that the homogeneity and porosity increased with Fe concentration. Energy Dispersive X-ray spectroscopy (EDX) examination revealed that the crystalline phase of the sample changed to α-alumina when the Al quantity decreased from 56.86 wt% to 53.98 wt%. The vibrational frequencies observed at 756 cm⁻¹ and 507 cm⁻¹ correspond to the tetrahedral and octahedral groups of the Al₂O₃ structure, respectively. Photoluminescence (PL) measurements showed that the PL intensity observed at 3.4 eV decreased with increasing iron atom concentration, indicating that Fe-doped alumina (4%) exhibited the highest photocatalytic efficiency. Vibrating-Sample Magnetometry (VSM) confirmed the ferromagnetic behavior of the formed iron-doped alumina NPs with low magnetization of saturation (Ms = 0.245 emu/g), magnetic susceptibility (χ = 35.736 × 10⁻⁷emu g⁻¹Oe⁻¹), and magnetocrystalline anisotropy constant (<i>K</i>_<i>1</i> = 2.678 × 10²erg/cm³).</p> Graphical Abstract <p></p>