Chemical looping combustion potentially offers inherent CO2 capture during power generation. Implementation of the process, however, is hindered by the lack of suitable materials to function as oxygen carriers. In this context, spinel-supported nickel oxides were investigated, using modified TGA to study the redox characteristics of NiO/NiAl2O4 and (NiO)(1-y)(MgO)(y)/Ni(1-x)MgxAl2O4, prepared by solution combustion synthesis using varying precursor ratios. The long-term performance of the promising stable oxide (NiO)(0.79)(MgO)(0.21)/Ni0.62Mg0.38Al2O4 was tested by cycling the oxidant/reductant gases 100 times at 1000 degrees C, where it exhibited excellent reactivity and stability. Finally, attrition resistance of the oxygen carriers was determined via a modified ASTM test, which indicated mechanical strength superior to that of commercially available iron oxide.