The paper reports a microwave irradiation method to rapidly synthesize Li 3 V 2 (PO 4 ) 3 /C materials as cathode for lithium ion batteries by the self-assembly microwave reaction oven with carbon seal reactor, using LiH 2 PO 4 , V 2 O 5 and sucrose as raw materials. Sucrose was used to be reducer and carbon source. Thermogravimetric (TG) analysis, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) were used to characterize its structure and morphology. Electrochemical properties of the Li 3 V 2 (PO 4 ) 3 /C materials were studied by cyclic voltammetry (CV) and charge–discharge cycling performance. The results showed that the diffraction peaks of the sample correspond to a single-phase, and can be indexed as monoclinic structure with a space group of P2 1 /n. An electrochemical test showed that Li 3 V 2 (PO 4 ) 3 /C demonstrated an excellent electrochemical capacity of 138mAhg −1 at 0.2C rate and 124.1mAhg −1 at 5C rate with stable cycle ability.