Mixed-conducting oxide SrFeCo 0.5 O y powders have been synthesized by auto-combustion of citrate-nitrate gel. The resulting powder is pure, homogeneous and possesses a reasonably fine particle size. Attempts have been made to understand the combustion process with the help of Differential Thermal Analysis (DTA) of the sample. The XRD, SEM and TEM studies on these powders confirmed that the method produces powder had greater composition uniformity, lower residual carbonate levels and smaller particle sizes.