Synthesis of pure nano-sized Li4Ti5O12 powder via solid-state reaction using very fine grinding media

Abstract Li 4 Ti 5 O 12 was synthesized by a solid-state reaction using Li 2 CO 3 and anatase TiO 2 at 800 °C for 3 h for anode application in Li-ion batteries. In order to examine the effects of milling conditions on the properties of Li 4 Ti 5 O 12 , 3 different ZrO 2 media of sizes 0.45, 0.10 and 0.05 mm were subjected to 5 h of high energy milling, while 5 mm balls were subjected to 24 h of ball milling for comparison. High energy milling was found to be much more effective in decreasing both the reaction temperature and the final Li 4 Ti 5 O 12 particle size than ball milling through the efficient size reduction and mechanochemical activation of the starting materials. The use of 0.10 and 0.05 mm beads resulted in the synthesis of pure nanosized Li 4 Ti 5 O 12 , depressing the formation of unwanted rutile TiO 2 in the final products, whereby the finer milling media showed more desirable particle properties. Consequently, pure Li 4 Ti 5 O 12 of 145 nm size, which is comparable to the particle sizes from expensive wet chemical methods, could be synthesized by an economic solid-state reaction.