LiVPO4F was synthesized by a novel sol-gel method under Ar atmosphere using V2O5·nH2O, LiF, NH4H2PO4 and citric acid as starting materials, and its physicochemical properties were investigated using X-ray diffraction (XRD), SEM and electrochemical methods.XRD patterns showed that LiVPO4F prepared displayed with a triclinic structure with a space group of p(i).SEM results indicated that the particle size of LiVPO4F was about about 0.5 μm together with homogenous distribution.