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ABO
3-δ perovskites are ideal for high-temperature thermochemical air separation for oxygen production because their oxygen nonstoichiometry δ can be varied in response to changes in temperature and oxygen partial pressure [
p
O
2
]. Herein, the outstanding oxygen-sorption performance of CaCo
x Zr
1-x O
3-δ perovskites and their potential application as oxygen-selective sorbents for air separation is reported. In situ thermal X-ray diffraction was used to study the materials' structural changes in response to temperature variations in air and inert atmosphere. Temperature-programmed reduction was employed to elucidate the relationship between perovskite composition and redox property. O
2 sorption performance was evaluated by isothermal analyses at various temperature and
p
O
2
along with long-term absorption-desorption cycle tests. The high oxygen-sorption capacity was mainly attributed to Co at B-site, whereas partial substitution of Co by Zr enhanced the structural crystallinity and thermal stability of the perovskite. A stable oxygen production of 2.87 wt % was observed at 900 °C during 5 min-sorption cycles for 100 cycles.
