Alumina-silica mixed oxide nano-catalyst materials with compositions 83.6wt.% Al2O3-16.4wt.% SiO2 (3Al(2)O(3)center dot lSiO(2)), 71.82wt.% Al2O3-28.18wt.% SiO2 (3Al(2)O(2)center dot 2SiO(2)), 62.84wt.% Al2O3-37.16wt.% SiO2 (3Al(2)O(3)center dot 3SiO(2)) and 56.03wt.% AI,O-3-43.97wt.% SiO2 (3Al(2)O(3)center dot 4SiO(2)) have been prepared by a hybrid sol-gel technique using boehmite as the precursor for alumina and tetraethoxysilane as that for silica. The bonding characteristics and coordination features around Al and Si in the mixed oxide catalysts have been studied using FTIR and Al-27 MAS NMR after calcination at 400 degrees C which is the temperature region where cross-condensation is seen to take place. A high BET specific surface area of 287 m(2)g(-1) is obtained for 3Al(2)O(3)center dot lSiO(2) mixed oxide composition. The porosity features are further established by BET adsorption isotherms and pore size distribution analysis. The temperature-programmed desorption studies showed more surface active sites for the silica-rich composition, suggesting enhanced catalytic potential. The TEM features of the mixed oxides showed a homogeneous distribution of alumina and silica phases with particle sizes in the nano-range. The low silica-containing mixed oxide showed a needle-like morphology with a high aspect ratio of 1:50 and similar to 10nm particle size while the silica-rich composition had particle size in a wide range (similar to 20-75 nm). (c) 2005 Elsevier B.V. All rights reserved.