The lithium vanadate LixV2O5 (x= 1.0, 1.2 and 1.4) has been prepared by solid state reaction method. The Li-7 MAS-NMR, Laser Raman and Fourier Transform Infrared (FTIR) spectroscopic analysis reveals the delta-LiV2O5 and gamma-LiVO5 phase formation. The Li-7 MAS-NMR spectrum shows the chemical shift around -1 and -10 ppm, which confirms the presence of gamma and delta phases of lithium vanadate. The formation of delta phase and gamma phase of LiV2O5 has been detected by the presence of Raman peaks at 971 and 982 cm(-1). The phase transformation from delta to gamma phases of LiV2O5 With lithium incorporation has been identified. The reduction in the oxidation state of vanadium (V5+ to V4+) has been identified, due to lithium incorporation. This reduction affects the vanadium oxygen bonding nature and leads to the phase transformations. (C) 2004 Elsevier B.V. All rights reserved.