We synthesized both the V 2 O 5 xerogel and the composite V 2 O 5 xerogel/C starting from the solution of V 2 O 5 in hydrogen peroxide. After the characterization by XRD, thermal (TGA-DTA), SEM methods and by particle size analysis, the investigation of Li + and Mg 2+ intercalation/deintercalation reactions in an aqueous solutions of LiNO 3 and Mg(NO 3 ) 2 were performed by cyclic voltammetry. The composite material V 2 O 5 xerogel/C displayed relatively high intercalation capacity, amounting to 123 mA h g −1 and 107 mA h g −1 , in lithium and magnesium salt solutions, respectively.