This study initiates the preparation of Sm1-xCaxFeO3 (0.1 <= x <= 0.5) compounds by sol-gel based Pechini method at low temperatures. The samples are analyzed by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA), and Differential Thermal Analysis (DTA) techniques for appropriate characterization of the distinct thermal events occurring during synthesis. The resulting XRD data reveal that a pure phase with perovskite structure is obtained for each composition. An exothermic peak appears in the DTA curve at 700 degrees C for x = 0.1 sample, suggesting a crystallization process; a similar behavior is found to occur for the other compositions as well. The microstructural characteristics of all the phases show particles of different morphology and size. (C) 2012 Elsevier B.V. All rights reserved.