Synthesis of Lithium Titanate (Li₄Ti₅O₁₂) through hydrothermal process by using Lithium Hydroxide (LiOH) and Titanium Dioxide (TiO₂) xerogel

Lithium Titanate (Li₄Ti₅O₁₂) or (LTO) has a potential as an anode material for a high performance lithium ion battery. In this work, LTO was synthesized by a hydrothermal method using Titanium Dioxide (TiO₂) xerogel prepared by a sol-gel method and Lithium Hydroxide (LiOH). The sol-gel process was used to synthesize TiO₂ xerogel from a titanium tetra-n-butoxide/Ti(OC₄H₉)₄ precursor. An anatase polymorph was obtained by calcining the TiO₂ xerogel at a low temperature, i.e.: 300°C and then the hydrothermal reaction was undertaken with 5M LiOH aqueous solution in a hydrothermal process at 135°C for 15 hours to form Li₄Ti₅O₁₂. The sintering process was conducted at a temperature range varying from 550°C, 650°C, and 750°C, respectively to determine the optimum characteristics of Li₄Ti₅O₁₂. The characterization was based on Scanning Thermal Analysis (STA), X-ray Powder Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Fourier Transform Infrared spectroscopy (FTIR), and Brunauer-Emmett-Teller (BET) testing results. The highest intensity of XRD peaks and FTIR spectra of the LTO were found at the highest sintering temperature (750°C). As a trade-off, however, the obtained LTO/Li₄Ti₅O₁₂ possesses the smallest BET surface area (< 0.001 m²/g) with the highest crystallite size (56.45 nm).