<p>In the current research, calcium ferrite (CaFe₂O₄) powders are synthesized via the sol-gel auto combustion approach in which the fuel is DEA (diethanolamine). The study seeks to discover the influence of calcination temperature upon both calcined and as-synthesized CaFe₂O₄ powders, taking into consideration the morphology and structure along with the optical, chemical, and magnetic properties. Various methods were used to perform the analyses, among which were X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), UV-visible diffuse reflectance spectroscopy (UV-DRS), and vibrating sample magnetometry (VSM). From the findings of XRD and FT-IR, powders of the non-calcined samples presented signs of multiple calcium ferrite phases, including structures comprising dicalcium diiron pentaoxide (Ca₂Fe₂O₅), calcium triiron pentaoxide (CaFe₃O₅), and calcium iron oxide (CaFe₂O₄). Once the temperature reached 500&#xa0;°C, the prominent structure was CaFe₂O₄, which exhibited a single phase as there were no impurities. UV-DRS analysis revealed that optimal calcination conditions produced better sample reflection levels in comparison to the visible and infrared spectra which were seen for the as-synthesized sample. For wavelength in the visible and infrared region, the reflectance of the samples calcined under ideal condition increases to 22% and 80%, whereas in contrast, the uncalcined sample reached just 8% and 11%. The bandgap energy (<i>E</i>_<i>g</i>) for calcined samples measured 1.88&#xa0;eV to 2.13&#xa0;eV, while for the as-synthesized sample the value was 1.79&#xa0;eV. According to VSM measurements, the superparamagnetic behavior can arise in those samples with the optimum calcination temperature, although the as-synthesized sample exhibits ferrimagnetic properties. In addition, magnetization of CaFe₂O₄ spinel powders was decreased by higher calcination temperatures, and there was a notable decline in coercivity.</p>