Synthesis of Li2tTiO3 Powders by a Hydrothermal Process

"The Eh-pH diagram of lithium-titanium-water system at 25°C, 100 °C and 200 °C was constructed. It shows that there exist thermodynamic stability areas of Li2TiO3. This indicates a thermodynamic possibility for the formation of Li2TiO3 in aqueous solution. A hydrothermal process has been applied for the preparation of Li2TiO3 using TiCl4 and LiOH•H2O as raw materials. The prepared samples were examined with X-ray diffraction, scanning electron microscopy and thermo-gravimetric analysis and differential scanning calorimetry. The results show that temperature and washing condition have significant effects on the phase composition of the product. Phase-pure Li2TiO3 powders were obtained at 200°C with Li:Ti molar ratio of 2.0.INTRODUCTIONLithium-containing ceramics enriched in 6Li, such as Li2O, LiAlO2, Li4SiO4, Li2ZrO3 and Li2TiO3, are considered as tritium breeding materials (Saito et al., 1998; Roux et al., 1998; Johnson et al., 1998; Hoshino et al., 2002). In view of its admirable properties: low-activation, good thermal stability and thermal conductivity, excellent tritium release performance and reasonable lithium atom density (Kopasz et al., 1994; Roux et al., 1996; Saito et al., 1998; Wu et al., 2008), Li2TiO3 is recognized as one of the most promising candidates of tritium breeding materials. Meanwhile, Li2TiO3, as the precursor of H2TiO3-type lithium absorbent, receives more attention as the development of extracting lithium from salt lakes (Zhong, 2004; Zhang, 2010).Several synthetic techniques have been applied to prepare Li2TiO3 powders, such as solid-state methods (Lulewicz and Roux, 2002; Ramaraghavulu et al., 2011; Mandal et al., 2012), sol-gel processes (Deptula et al., 2002; Lee, 2008) and solution combustion routes (Cruz et al., 2006; Jung et al., 2006; Sinha et al., 2010). A solid-state method may produce a series of problems, including impurity contamination and difficulty in morphology control of the obtained powders, although the process involved is simple. The solgel process is prolonged and usually demands for multi-step reactions, while solution combustion route requires plenty of energy and easily causes product contamination by the fuel used. Owing to its environmentally benign and highly suitable characteristics in fabricating materials, hydrothermal technology has been widely used and became a powerful tool in the field of material synthesis (Yoshimura and Byrappa, 2008). For example, ZnO in the form of bulk single crystals, fine particles and thin films, which is an attractive photoelectric material, was successfully synthesized by hydrothermal process (Sekiguchi et al., 2000; Ohshima et al., 2004). A hydrothermal technique was also used to the preparation of carbon nanotube, which possesses outstanding mechanical, structural and electric properties (Bernholc et al., 1997), and is superior to the commonly used method (Gogotsi and Libera, 2000). There, it provides an option for preparing Li2TiO3. Laumann et al. (Laumann et al., 2010) synthesized cubic a-Li2TiO3 by hydrothermal reaction at 180 °C for 18 h, using TiO2 powder, comprising of anatase and rutile, and lithium hydroxide in de-ionized water. However, the prepared a-Li2TiO3 is extremely unstable with a maximum lithium loss of 75% when treated in bathing experiment."