Synchrotron X-ray diffraction in situ study of Li4Ti5O12 synthesis from rutile and anatase

Abstract

The comparative study of solid state synthesis of Li4Ti5O12 from rutile and anatase as initial reagents was carried out using the method of in situ synchrotron radiation dynamic diffractometry. Initial samples were obtained by mechanical treatment of Li2CO3 and TiO2 (anatase or rutile modifications). It was found that on the first stage an intermediate β-Li2TiO3 phase forms in the reaction system. On further heating the process of formation of the Li4Ti5O12 phase from β-Li2TiO3 and TiO2 is limited by lithium cation diffusion through the β-Li2TiO3 phase. Reaction strongly accelerates at temperatures above 800 oC. Using nano-sized anatase precursor, well-crystallized LTO with smaller grain size may be obtained at lower temperatures.