In this research, the solid-state method was utilized to synthesize LaFeO3 powders, with La2O3 and Fe2O3 being employed as precursor perovskite materials. The prepared samples were calcined at different temperatures 800°C, 900°C, 1000°C, 1100°C, 1200°C and 1300°C for 4h to study phase stability. The thermal effect on structural and morphological properties was reported. The X-ray diffraction results confirmed the pure phase in its orthorhombic configuration at 1200°C and 1300°C, which was confirmed by Rietveld’s analysis. Scanning electron microscopy coupled with Energy-dispersive X-ray spectroscopy was employed to analyze the surface morphology and compositional characteristics. In addition, the samples were analyzed by Fourier Transform Infrared Spectroscopy. The thermal behavior of the product was investigated through the utilization of thermogravimetric analysis.