Fe2O3/SnO2 nanocomposites were successfully synthesized by microwave heating and spray drying process. Spherical secondary particles (less than 5 mu m) of the Fe2O3/SnO2 nanocomposites consisted of primary particles (about 5 nm), and the atomic ratio of Sn: Fe was Sn: Fe = 63: 37. The Fe2O3/SnO2 nanocomposites preheated at 300 degrees C worked as a rechargeable electrode material. The initial lithium insertion capacity of 1344mAh g(-1) (cutoff voltage: 10 mV) was achieved, and the rechargeable capacity at the 2nd cycle was 927mAh g(-1).