Two series of mixed oxides, CoAlM and MgAlM (M= Cr, Mn, Fe, Co, Ni, Cu) , were prepared by calcining their corresponding hydrotalcite-like compounds (HTLc) . The ratio of Mg: Al: M (or Co: Al: M) was 3:1:1. The catalytic activity of all samples for the reaction of NO + CO was investigated. The results showed that the activity of CoAlM was much higher than that of MgAlM. The structure and the property of redox were characterized by XRD and H2-TPR. The results indicated that only MgO phase was observed after calcining MgAlM hydrotalcites, and the transition metals became more stable. The spinel-like phase appeared in all of CoAlM samples after the calcination, and the transition metals were changed to be more active, and easily reduced . The activities of three series of mixed oxides CoAlCu obtained from different preparation methods, different ratio of Co:Al:Cu and at different calcination temperatures, were studied in detail for proposing the mechanism of reaction. The ability of adsorption of NO and CO The series of mixed oxides, CoAlM and MgAlM (M = Cr, Mn, Fe, Co, Ni, Cu), were prepared by calcining their corresponding hydrotalcite- like compounds (HTLc). The ratio of Mg: Al: M : Al: M) was 3: 1: 1. The catalytic activity of all samples for the reaction of NO + CO was investigated. The results showed that the activity of CoAlM was much higher than that of MgAlM. The structure and the property of The results indicated that only the MgO phase was observed after calcining MgAlM hydrotalcites, and the transition metals became more stable. The spinel-like phase appeared in all of CoAlM samples after the calcination, and the transition The activities of three series of mixed oxides CoAlCu obtained from different preparation methods, different ratio of Co: Al: Cu and at different calcination temperatures, were studied in detail for proposing the mechanism of reaction. The ability of adsor ption of NO and CO