In Situ X‐Ray Diffraction of Lithium Intercalation in Nanostructured and Thin Film Anatase TiO2

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Abstract
Electrochemical lithium intercalation in thin films of porous nanostructured and dense electron‐beam evaporated (anatase) is investigated with in situ X‐ray diffraction (XRD). A complete and reversible phase transformation from tetragonal anatase to orthorhombic anatase is observed. The maximum amount of lithium that can be dissolved in anatase before the phase transformation occurs is estimated to be 0.05 Li/Ti. For nanostructured samples, the XRD spectra before and after insertion were fitted with some of the lattice parameters of the two phases as fit variables. For the phase, values of 3.85, 4.06, and 8.95 Å are found for the a, b, and c, axes, respectively, in good agreement with data reported for chemically lithiated anatase powder. Implications of the phase transition for the analysis of optical and electrochemical measurements on films are briefly discussed. © 1999 The Electrochemical Society. All rights reserved.

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