Structural effect and oxygen storage capacity (OSC) on alumina-supported cerium oxide catalysts have been studied. The behavior and activity of active oxygen species originated from OSC also have been characterized. In those catalysts, the catalyst prepared by an alkoxide method using needle boehmite sol derived from aluminum tri-isopropoxide (AIP) and cerium nitrate dissolved in ethylene glycol gave a finely-divided nonstoichiometric cerium oxide dispersed on alumina (Ce0
2-x/Al
2O
3) after the H
2reduction at 900°C. The presence of a finely-divided nonstoichiometric cerium oxide containing Ce
3+and Ce
4+ ions was anticipated by XRD, EXAFS and fluorescent measurements. The higher OSC was achieved on Ce0
2-x/Al
2O
3 catalyst, compared with CeO
2/Al
203 and CeAlO
3/Al
2O
3 where cerium oxides were stoichiometric structures. It was concluded by
18O tracer studies that the higher activity of Ce0
2-x /Al
2O
3 catalyst for methane oxidation was mainly associated with the activation sites of oxygen species, where the sites consisted of oxygen vacancies formed by finely-divided nonstoichiometric structures, from the surface to the bulk and vice versa. The addition of palladium to CeO
2/Al
2O
3 catalyst enhanced drastically the OSC and improved the catalytic activity on NO decomposition by the acceleration of oxygen spillover, indicating the generation of synergetic effect between Pd and CeO
2-x. The good relation between OSC and NO decomposition activity on Pd/CeO
2-x, /Al
2O
3 catalyst might promise the preparation of new catalyst by the control of OSC.
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