B/Fe2O3 samples were prepared by mixing nano sized boron powder with iron oxide xerogels that had been synthesized using a sol-gel method that included various types of proton scavengers such as 1,2-epoxybutane, tetrahydrofuran, 1,4-dioxane and ammonium hydroxide. The effects of the proton scavengers and drying conditions on the textural properties of the iron oxide samples and on the heat output and thermal behavior of the nano-composites were examined. The iron oxide samples were subjected to direct drying (DD) or sequential solvent exchange (SSE). The heat output values of the B/Fe2O3 nano-composites varied from 240 to 1200 J/g depending on the drying condition and the proton scavenger used. It was found that the thermal behaviour and the textural properties of B/Fe2O3 nano-composites (such as porosity, surface area and crystallinity) could be tailored by both the drying conditions and the proton scavenger used.