<p>Ca-doped LaFeO₃ perovskite oxide powders have been synthesized via sol-gel processing method. The work investigates the effect of synthesis parameters such as introduction of citric acid and/or ethylene glycol and processing parameters including calcination temperature and time on the properties of Ca-doped LFO perovskite materials. Different chemical additives and calcination conditions were employed to optimize the synthesis process. Characterization techniques including thermal analysis (DTA/TGA), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and Fourier-transform infrared spectroscopy (FT-IR) were used to evaluate the structural and morphological properties of the synthesized samples in view of their possible application as the cathode materials for solid oxide fuel cells (SOFCs) devices. The results indicate that the sample processed with both citric acid (CA) and ethylene glycol (EG) and calcined at 1200 °C for 1 h (CA, EG (1200 °C, 1 h)) achieved optimal structural characteristics, demonstrating purity, appropriate nano-crystallinity, and a porous structure with well-connected particles that suggest its viability as a cathode material. Furthermore, the influence of calcination temperature was examined by varying it from 700 °C to 1200 °C and the findings revealed that the material calcined at 1200 °C exhibited a porous single-phase structure and a favorable particle size distribution. Also, to survey the effect of calcination temperature, while extended calcination time generally enhanced crystallinity; the sample calcined at 1000 °C for 1 h displayed better properties compared to that calcined for 3 h, which experienced over-sintering and excessive particle growth. This research underscores the importance of synthetic parameters in tailoring the properties of Ca-doped LFO perovskites, thereby providing valuable insights for optimizing materials suitable for cathode applications.</p><p></p>