Li3VO3 was synthesized at 300-350 degrees C by reaction of Li2CO3 and NH4VO3 which were blended in an aqueous solution. The product was termed LT LiV3O3 and its preparation reaction was studied by thermographic analyses-depolarization thermocurrent. LT LiV3O3 showed a high discharge capacity of 300 mAh/g active material, and maintained a capacity of 275 mAh/g after 15 cycles. Its electrochemical behavior as a cathode material for rechargeable lithium batteries was studied by galvanostatic charge-discharge and cyclic voltammetry. The structure and morphology of LT LiV3O3 were characterized by infrared, X-ray diffraction, scanning electron microscopy, and their relationships with good electrochemical performance were studied.