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

¹ Institute of Solid State Chemistry and Mechanochemistry, SBRAS, Novosibirsk 630128, Russia
² Novosibirsk State Technical University, Novosibrsk, 630071, Russia
³ Budker Institute of Nuclear Physics SBRAS, Novosibirsk 630090, Russia

^* Corresponding author. Tel.: +7 383 2332410 *1535; fax: +7383 3322847. E-mail address: koza0707@yandex.ru

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.