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The catalytic properties of oxidized Ni3Sn2 powders were investigated for producing hydrogen from decomposing methanol in the temperatures ranging from 240 to 480 ºC. The oxidized Ni3Sn2 had much higher catalytic activity than that of Ni3Sn2 in the temperature range of 320~400 ºC. The results of an isothermal test performed at 320 ºC revealed that the oxidized Ni3Sn2 was spontaneously activated within 4 h of the reaction and slowly deactivated in the followed reaction time. The oxidized Ni3Sn2 suppressed side reactions such as methanation and water-gas shift reaction and showed a high efficiency for H2 production from methanol decomposition. Surface analysis revealed that the activity of oxidized Ni3Sn2 was attributed to the formation of Ni/SnO2 catalyst, which was supposed to serve as active sites for methanol decomposition.