A new approach has been used to prepare nanostructured lead oxide-carbon (PbO-C) composites via the spray pyrolysis technique. In this study, the electrochemical performance of the PbO-carbon nanocomposites as anode materials for lithium-ion rechargeable batteries was investigated. The prepared powders consist of fine nanocrystalline PbO homogeneously distributed within an amorphous carbon matrix with highly developed surface area. The estimated average crystal sizes of these nanocomposites from X-ray diffraction (XRD) patterns are in the range of 26-102 nm. The combination of spray technology and carbon addition increased the specific surface area (above 6 m(2) g(-1)) and the conductivity of PbO, improved the specific capacity, and maintained cycle life with a reversible capacity above 100 mAh g(-1) beyond 50 cycles. The increase in capacity retention for PbO-carbon compared to that of pure PbO was due to the presence of a conductive and highly developed carbon matrix that can absorb large volume changes during the alloying/dealloying of lead with lithium over the 1.50 to 0.01 V potential range, which yields LixPb alloys (0 < x < 4.5).