Co3O4　composite　metal　oxide　catalyst　is　prepared　via　the　solvent　assisted　hydrothermal　method　using　cobalt　acetate　as　cobalt　source.　Its　physicochemical　properties　are　characterized　by　XRD,　SEM,　BET　and　H2-TPR,　XPS,　N2O-TPSR　and　O2-N2O-TPSR.　The　activity　of　the　catalyst　in　catalytic　decomposition　of　N2O　is　evaluated　in　a　fixed-bed　micro-reactor　and　the　effects　of　crystallization　temperature　on　its　activity　in　catalytic　decomposition　of　N2O　are　investigated.　Evaluation　results　show　that　Co3O4　catalysts　prepared　via　solvent　assisted　hydrothermal　method　have　a　spinel　structure　and　the　crystallization　temperature　does　affect　catalysts＇　morphology,　redox　performance　and　activity　in　catalytic　decomposition　of　N2O.　The　result　by　N2O-TPSR　and　O2-N2O-TPSR　shows　that　the　oxygen　adsorbed　on　the　catalyst　surface　plays　an　important　role　in　the　catalytic　decomposition　of　N2O.　The　redox　performance　of　Co3O4　catalyst　prepared　at　a　crystallization　temperature　of　160℃　is　good,　over　which　the　catalytic　decomposition　of　N2O　can　be　performed　under　a　low　temperature.　The　T10　and　T95　are　266℃　and　410℃,　respectively　under　the　conditions　that　reaction　gas　consists　(volume　fraction)　0.68%　of　N2O,　0.88%　of　O2　and　Ar　as　equilibrium　gas　with　a　flow　rate　of　80　mL•min-1.　©　2019,　China　National　Chemical　Information　Center.　All　right　reserved.