Perovskite-type oxides are promising oxygen carriers in producing oxygen-enriched CO 2 gas stream for oxyfuel combustion. In this study, a new series of SrCo 1-x Fe x O 3-δ (x = 0.2, 0.4, 0.6, 0.8) was prepared and used to produce O 2 /CO 2 mixture gas. The phase, crystal structure, and morphological properties of SrCo 1-x Fe x O 3-δ were investigated through X-ray diffraction, specific surface area measurements, and environmental scanning electron microscopy. The oxygen desorption performance of SrCo 1-x Fe x O 3-δ was studied in a fixed-bed reactor system. Results showed that the different x values of SrCo 1-x Fe x O 3-δ have no obvious effects on crystalline structure. However, the oxygen desorption performance of SrCo 1-x Fe x O 3-δ is improved by Co doping. Moreover, SrCo 0.8 Fe 0.2 O 3-δ synthesized via a new EDTA method has a larger BET surface area (40.396 m 2 /g), smaller particle size (48.3 nm), and better oxygen production performance compared with that synthesized through a liquid citrate method.