Supported nickel has been used in a wide range of applications for industrial reactions, such as steam reforming, hydrogenation and methanation. In this work, nickel aluminate was prepared by the sol-gel process using alumatrane as the alkoxide precursor, directly synthesized from the reaction of inexpensive and available compounds, aluminum hydroxide and TIS (triisopropanolamine) via the oxide one pot synthesis (OOPS) process. Various conditions of the sol-gel process, such as pH, calcination temperature, hydrolysis ratio and ratio of nickel to aluminum, were studied. All samples were characterized using FTIR, TGA, XRD, TPR, DR-UV and BET. The BET surface area was in the range of 340-450 m 2 /g at the calcination temperature of 500 • C with a mesoporous pore size distribution. Catalyst activity testing in CO oxidation reaction depended on Ni : Al ratio and calcination temperature. Higher activity was obtained from higher Ni content and lower calcination temperature. In addition, catalysts prepared using alumatrane precursor had higher percentage conversion than those prepared using aluminum hydroxide precursor.