The vanadates of LiNi1-xMxVO4(M=Fe,Co,Ni) containing VO4 tetrahedrons were synthesized by soft chemical method through a new mild liquid route. The samples sintered at 450℃ for 3h and at 650℃ for 3h are named for LT LiNiVO4 and for MT LiNi1-xMxVO4 respectively. All of the products were measured by X ray diffraction, IR and Raman spectra respectively. In comparison with IR spectra of V2O5 and NiO, the LT LiNiVO4 has a strong and broad IR absorption band of VO4 tetrahedrons located at 600～850cm-1 with three small splitting peaks corresponding to the asymmetry stretching vibrations of V O bonds. The results of IR and Raman spectra for MT LiNi1-xMxVO4 show that the cations of Ni2+, Co2+, Fe2+ have the influences on the frequency shifts of the V O vibrations.
