Evidence of two-phase formation upon lithium insertion into the Li1.33Ti1.67O4 spinel

Li(1.33)Ti(1.6)7O(4) synthesized from Li2CO3 and TiO2 was electrochemically inserted with lithium at room temperature. The defect spinel Li1.33Ti1.67O 4 and the fully lithiated Li2.33Ti1.67O4 with ordered rock-salt-type struct ure show nearly identical X-ray diffractions. Due to similar lattice consta nts of both phases and the low scattering factor of the lithium ions, the i dentification of the insertion mechanism using X-ray powder diffraction is possible only by using high angle X-ray scans of several samples inserted w ith different amounts of Lithium. Precise analysis of the obtained data sup plies the evidence for the presence of two distinct phases which are mutual ly interconvertible upon lithium exchange. This result is in good agreement with electrochemical data postulating a two-phase mechanism from the const ant electrical potential found during cycling. (C) 1999 The Electrochemical Society. S0013-4651(98)06-031-1. All rights reserved.