Modifications of microstructure and pore morphology in lithium-orthosilicate pebbles, due to the addition of excess lithium.

Lithium orthosilicate (Li 4 SiO 4 ) was synthesized; without and with excess lithium (Li) in quantity of its stoichiometric requirement, with 5, 10, 15 and 20% excess lithium, and pebbles were fabricated by Solid State Reaction Process (SSRP), similar to that of lithium titanate. The green pebbles were sintered at 900 °C for 6 h. XRD analysis of the synthesized powders, confirmed the formation of single phase Li 4 SiO 4 when stoichiometric ratio of lithium carbonate and silica were used and the presence of multiple phases when excess lithium was used. Morphological modifications of mesoscopic structure in Li 4 SiO 4 pebbles with different quantities of excess lithium were investigated using Ultra-Small Angle Neutron Scattering (USANS) and Scanning Electron Microscopy (SEM). USANS measurements reveal the presence of sub-micrometric pores. It also indicates density fluctuations, even at nanometer length scale. Slight variation in pore size distribution with the amount of excess lithium was observed. Average size of the pores shows a decreasing trend initially with increase in Li amount but shows an opposite trend at around 15% of excess Li. [ABSTRACT FROM AUTHOR]