Abstract: Cu, Co, Mn and Ni decorated Fe₂O₃/Al₂O₃ oxygen carriers were prepared by freeze-drying method in this work. Temperature programmed reduction (H₂-TPR) and Temperature programmed oxidation (TPO) experiments were conducted in an automatic chemisorption instrument, and the reactivity of transition metal decorated Fe₂O₃/Al₂O₃ oxygen carriers with H₂ and O₂ was evaluated. The results showed that the reactivity for oxygen carrier with H₂ was improved after decorated with Cu, Co and Ni. But when decorated with Mn, the reactivity and oxygen transport capacity of oxygen carrier decreased. The Cu-decorated Fe₂O₃/Al₂O₃ oxygen carrier demonstrated the best reactivity with H₂ and favorable stability. Therefore, it could be a potential oxygen carrier for using in the chemical looping combustion.