La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) perovskite nanostructures were synthesised using a 42kHz ultrasound assisted synthesis technique for the fabrication of electrodes in the intermediate and/or low temperature solid oxide fuel and electrolysis cells (SOFCs/SOECs). The obtained nanomaterials were dried at 110°C followed by calcination in a normal atmosphere at various temperatures from 400 to 1000°C for 2h. Powder characteristics such as crystal structure, thermal decomposition, particle size and morphology were analysed. The transmission electron microscopy (TEM) study revealed the uniform equi-axial shape and growth of the obtained nanostructures with respect to the calcination temperature till 800°C. The structural and chemical analyses confirmed the existence of LSCF and CoFe2O4 phases.