Abstract: Perovskite-type metal oxides SrCo_0.8Fe_0.2O_3-δ(SCF182) powder was synthesized by combined EDTA-citrate complexing process. The effects of the pH value of precursor solution on the crystal structure and morphology of synthesized SCF182 powder were investigated by X-ray diffraction and environmental scanning electron microscopy. Fixed-bed experiments were conducted to study the oxygen adsorption/desorption performance of SCF182. The results show that the pH values do not affect the forming of main crystal phase of SCF182 but affect the grain size and microstructure. The net-like porous structure is formed in the system when the pH value of the precursor is 8.The fixed-bed experimental results indicate that the pH value of precursor solution has effects on the oxygen adsorption reaction rate of SCF182. Furthermore, the maximum oxygen desorption amount of SCF182, 42.2 mg/g, can be obtained when the pH value is 8.