The La0.56Sr0.4Co0.2Fe0.8O3-δ (LSCF) perovskite cathode, substituted by Sr and Fe at the A and B sites, respectively, is a good candidate for intermediate temperature solid oxide fuel cell (IT-SOFC) applications. The powders were prepared by sol-gel method using various metal nitrates as starting materials. The adipic acid was used as a chelating agent and ethylene glycol as a dispersant. The gel precursor was heated at 700 °C for 4 h to obtain LSCF cathode powders. X-ray diffraction pattern showed the single phase of the perovskite structure. The microstructure of LSCF materials was observed by scanning electron microscopy which was loosely aggregated and could be ground easily into fine powders. The average particle size of the powders was found to be around 80-200 nm. TGA/DTA techniques exhibited the weight loss after high temperature process. It was found that no weight loss after 550 °C suggests the completion of combustion process.