A series of x NiAl_2O_4/γ-Al_2O_3 composites with various Ni contents have been prepared via one-step partial hydrolysis of metal nitrate salts in the absence of surfactants and used for carbon dioxide reforming of methane. The characterization results demonstrated that the Ni Al_2O_4/γ-Al_2O_3 materials possessed mesoporous structures of uniform pore sizes; and the Ni~(2+) ions were completely reacted with alumina to Ni Al_2O_4 spinel in the matrices using N2 sorption, XRD, TEM, and XPS. The Ni Al_2O_4/γ-Al_2O_3 materials exhibited excellent catalytic properties and superior long-term stability for carbon dioxide reforming of methane. The effects of Ni content on the intrinsic activities and the amounts of coke disposition of the x NiAl_2O_4/γ-Al_2O_3 catalysts were discussed in detail for the carbon dioxide reforming of methane. The results revealed that the Ni particle sizes did not affect the intrinsic activity of metallic Ni, but smaller Ni particles could reduce the rate of coke deposition. A series of x NiAl_2O_4 / γ-Al_2O_3 composites with various Ni contents have been prepared via one-step partial hydrolysis of metal nitrate salts in the absence of surfactants and used for carbon dioxide reforming of methane. The characterization results demonstrated that the Ni Al_2O_4 / γ-Al 2 O 3 materials possessed mesoporous structures of uniform pore sizes; and the Ni 2+ ions were completely reacted with alumina to Ni Al 2 O 4 spinel in the matrices using N2 sorption, XRD, TEM and XPS. The Ni Al 2 O 4 / γ- The effects of Ni content on the intrinsic activities and the amounts of coke disposition of the x NiAl_2O_4 / γ-Al_2O_3 catalysts were discussed in detail for the carbon dioxide reforming of methane. The results revealed that the Ni particle sizes did not affect the intrinsic activity of metallic Ni, but smaller Ni particles could reduce the rate of c oke deposition.