Chemical looping combustion technology has drawn much attention due to advantages such as no NOx formation and simple CO2 separation. The thermally stable oxygen carrier in the redox cycle at 1,000-1,400 K is necessary for the chemical lopping combustion. The thermally stable hexaaluminate can be a good candidate for the support material of the oxygen carrier. In this work, NiO/hexaaluminate has been developed in order to apply for chemical looping combustion. From the X-ray diffraction patterns, it was found that most of Ni existed in the form of NiO and NiAl2O4 in the obtained sample. The NiO supported on NiAl2O4 showed good characteristics in the reduction and oxidation reaction. The present work suggested that NiO/hexaaluminate is a promising material as oxygen carrier for the chemical looping combustion.