The effects of the parameters of the sol-gel catalyst preparation such as hydrolysis ratio, acid/alkoxide ratio, and calcination temperature on surface area, porous structure, crystal structure and surface properties of nickel-titanium (Ni-Ti) composite xerogel catalyst were studied. The optimum hydrolysis ratio and acid/alkoxide ratio were determined under which conditions and 453 K calcination temperature, a Ni-Ti xerogel catalyst with a surface area of 426 m(2)/g was made. Increasing the calcination temperature would lead to dramatic decrease in surface area and collapse in porous structures. To compensate this deleterious effect, aluminum-containing compound was added into the precursor mixture in sol-gel preparation and the resultant Ni-Ti-Al composite xerogel catalyst had a significantly higher surface area even after undergoing a calcination temperature as high as 973 K. This xerogel catalyst showed comparably high activity for carbon dioxide reforming of methane where high temperature calcination is inevitable. (c) 2006 Elsevier B.V. All rights reserved.