The CoFeAlO4 oxygen-containing materials with spinel structure were synthesized by combustion synthesis. The chemical looping combustion reaction and cycling thermal stability of CoFeAlO4 oxygen carriers were investigated and characterized at different temperatures. The changes in the crystal structure and surface morphology of CoFeAlO4 oxygen carriers were analyzed. The results show that the increase of temperature is beneficial to improve the ability of CoFeAlO4 to convert reducible gas CO

resulting in the reduction rate faster

but redox at high temperature will cause CoFeAlO4 oxygen carrier phase separation

it is difficult to maintain a stable self-supported spinel structure. The analysis of the crystal structure of CoFeAlO4 oxygen carrier crystals before and after the reaction shows that the CoFe2O4 and CoAl2O4 detected after the redox cycle at high temperature is the main reason for the sintering of CoFeAlO4 oxygen carrier and the decrease of its cyclic thermal stability.