Synthesis of lithium titanate (Li₄Ti₅O₁₂) by addition of excess lithium carbonate (Li₂CO₃) in titanium dioxide (TiO₂) xerogel

Lithium titanate, Li₄Ti₅O₁₂ (LTO) is a promising candidate as lithium ion battery anode material. In this investigation, LTO was synthesized by a solid state method using TiO₂ xerogel prepared by the sol-gel method and lithium carbonate (Li₂CO₃). Three variations of Li₂CO₃ content addition in mol% or Li₂CO₃ molar excess were fabricated, i.e., 0, 50 and 100%, labelled as sample LTO-1, LTO-2 and LTO-3, respectively. The characterizations were made using XRD, FESEM, and BET testing. These were performed to observe the effect of lithium excess addition on structure, morphology, and surface area of the resulting samples. Results showed that the crystallite size and surface area of each sample was 50.80 nm, 17.86 m²/gr for LTO-1; 53.14 nm, 22.53 m2/gr for LTO-2; and 38.09 nm, 16.80 m²/gr for LTO-3. Furthermore, lithium excess caused the formation of impure compound Li₂TiO₃, while a very small amount of rutile TiO₂ was found in LTO-1. A near-pure crystalline Li₄Ti₅O₁₂ compound was successfully synthesized using the present method with stoichiometric composition with 0% excess, indicating very little Li⁺ loss during the sintering process.