We report a facile approach to synthesize Fe-Sb-based hybrid oxides nanocomposites consisting of Sb, Sb2O3, and Fe3O4 for use as new anode materials for lithium-ion batteries. The composites are synthesized via galvanic replacement between Fe3+ and Sb at high temperature in triethylene glycol medium. The phase, morphology, and composition changes of the composites involved in the various stages of the replacement reaction are characterized using X-ray diffractometry, high-resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy. The as-prepared composites have different compositions with very small particle sizes ( < < 10 nm). The FexSbyOz-18 h composite, for instance, exhibits high capacity, better cyclic stability, and rate performance than other composites, with a highly stable specific capacity of 434 mAh g(-1) at 500 cycles. The excellent electrochemical performance can be ascribed to the high interfacial contact area between the nano composite and electrolyte, stable structure of the composites owing to a mixture of inactive phases generated by the conversion reaction between Li+ and oxide metal whose structure serves as an electron conductor, inhibits agglomeration of Sb particles, and acts as an effective buffer against volume change of Sb during cycling and high Li+ diffusion ability.