Fabrication of Li2TiO3 pebbles by a freeze drying process

Li2TiO3 pebbles were successfully fabricated by using a freeze drying process. The Li2TiO3 slurry was prepared using a commercial powder of particle size 0.5–1.5 μm and the pebble pre-form was prepared by dropping the slurry into liquid nitrogen through a syringe needle. The droplets were rapidly frozen, changing their morphology to spherical pebbles. The frozen pebbles were dried at −10 °C in vacuum. To make crack-free pebbles, some glycerin was employed in the slurry, and long drying time and a low vacuum condition were applied in the freeze drying process. In the process, the solid content in the slurry influenced the spheroidicity of the pebble green body. The dried pebbles were sintered at 1200 °C in an air atmosphere. The sintered pebbles showed almost 40% shrinkage. The sintered pebbles revealed a porous microstructure with a uniform pore distribution and the sintered pebbles were crushed under an average load of 50 N in a compressive strength test. In the present study, a freeze drying process for fabrication of spherical Li2TiO3 pebbles is introduced. The processing parameters, such as solid content in the slurry and the conditions of freeze drying and sintering, are also examined.