Three series of binary oxide systems B(2)O(3)/Al(2)O(3) were prepared and the effect of alumina on dispersion of boron (B(2)O(3)) component was investigated. The aim of the study was to achieve a maximum dispersion of B(2)O(3) in the Al(2)O(3) a gel matrix that would lead to increased sorption capacity on boron oxide. Many attempts were made to establish the preparation conditions that would lead to a maximum dispersion of B(2)O(3) in the Al(2)O(3) gel matrix needed to increase the hydrogen sorption capacity on boron oxide. The systems were characterized by X-ray diffraction, SEM, TEM and low temperature nitrogen adsorption. Hydrogen adsorption was tested in the volumetric system. Results of the study showed that the amount of hydrogen adsorbed on B(2)O(3) depended not only on the surface area of the system but also on the separation of B(2)O(3) domains in Al(2)O(3) gel network. Irrespective of the method of synthesis of the binary oxide system, the dispersion of B(2)O(3) phase reflected in the amount of hydrogen adsorbed was the highest for the systems of the lowest B/Al molar ratios studied, i.e. for B/Al = 0.25. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.