In order to utilize the full potentials of the existing energetic materials, nitrocellulose/Al (NC/Al) nano-composite materials were prepared through sol-gel and supercritical carbon dioxide drying methods. The structures of nano-composite materials were characterized by FTIR, BET, SEM and DSC methods. Experimental results show that the nano-composite materials belong to mesoporous material and the nano-aluminum powders is well-distributed in the gel matrix. The specific surface area of the material decreases with the Al powders content increasing. When Al:NC (mass ratio) equals to 5:10, the decomposition heat per unit mass of NC component increases to 2408.07 J·g^-1 from 1689.21 J·g^-1.