Co3O4-C composite powder has been synthesized via spray pyrolysis of cobalt nitrate-sugar solution at 600 degrees C and assessed for application as anode materials in Li-ion batteries. Microstructural characterization by scanning electron microscopy, transmission electron microscopy, and energy-dispersive X-ray spectroscopy confirm an even distribution of carbon throughout particles, as well as the presence of a carbon-based surface sheath surrounding Co3O4-C particle agglomerates. Charge-discharge cycling of half-cells indicates a stable reversible discharge capacity above 800 mAh g(-1). Equivalent circuit modeling of Nyquist plots show the Co3O4-C electrode has significant kinetic advantages over non-composite transition metal oxide electrodes. (c) 2006 The Electrochemical Society.