Effects were shown for the composition and post-synthesis heat treatment in an oxygen atmosphere on the electrochemical properties of nanocomposites derived from polypyrrole (PPy) and a V 2 O 5 xerogel with host-guest structure. PPy 0.05 V 2 O 5 was found to have the highest specific discharge capacity of about 290 mA·h/g and high stability upon prolonged charge-discharge cycling among the PPy x V 2 O 5 nanocomposites prepared (where x = 0.1, 0.05, 0.025). Post-synthesis heat treatment in an oxygen atmosphere leads to oxidation of the reduced portion of the inorganic nanocomposite component and nanostructurization of the composite with formation of nanofibers that facilitate a considerable increase in the specific capacity and stability upon cycling.Among various chemical current sources, lithium ion batteries (LIB) hold special interest due to their good functional characteristics [1,2]. An important component of LIB is the cathode material, whose electrochemical properties largely determine the operational characteristics of the LIB [3-6]. The most well-studied cathode materials are transition metal compounds such as LiCoO 2 , LiMn 2 O 4 , and LiFePO 4 [3-6], but the specific discharge capacity of these materials, as a rule, does not exceed~150 mA·h/g, which is only about one half of the specific capacities of carbon anodes [4] used in commercial LIB. This finding led to an intensive search for more efficient alternative electrode materials, which would increase the energy capacity of LIB.Among such materials, hybrid nanocomposites (HNC) derived from organic and inorganic components have attracted the greatest attention. These nanocomposites can be used to construct both chemical current sources and other advanced-generation devices such as optoelectronic elements and sensors [7][8][9]. Interest in HNC has arisen since these materials have functional characteristics unachievable for massive or microstructurized analogs. Since LIB are used in an enormous number of devices, the development of efficient nanostructurized electrode materials for them is currently an important area of research [9][10][11][12][13][14][15][16][17][18][19][20].HNC derived from transition metal compounds in the nanosized state and conducting polymers (CP), which may have one of two structural types, are promising cathode materials for LIB. The first structural type is based on the insertion of 0040-5760/15/5103-0163