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Ni-ZrO2 catalytic materials were prepared by the selective oxidation of Ni-ZrH2 composite and amorphous Ni-Zr alloypowders synthesized by means of ball milling of NiZr2 alloys under pressurized H2 and Ar atmospheres, respectively. Structural characterization was performed using X-ray diffraction and transmission electron microscopy. Ni-ZrH2 compositeand amorphous Ni-Zr alloy powders were oxidized at 550 oC and 800 oC, respectively. The size of Ni particles in Ni-ZrO2-hranged from 5 to 20 nm while that of Ni-ZrO2-a were not separated obviously as fine particles. The mean sizes of the Niparticles in Ni-ZrO2-h and Ni-ZrO2-a obtained by XRD were about 16.9 nm and 28.4 nm, respectively. The methanolconversion ratio of Ni-ZrO2-h was higher than that of the Ni-ZrO2-a catalysts at all temperatures. Furthermore, it was foundthat Ni-ZrO2-h has a highly endurable structure. It is believed that the enhanced catalytic properties of Ni-ZrO2-h are due toits high surface area and separately dispersed Ni nanoparticles.