Basic molten salt process-A new route for synthesis of nanocrystalline Li4Ti5O12-TiO2 anode material for Li-ion batteries using eutectic mixture of LiNO3-LiOH-Li2O2

Authors

Md Mokhlesur Rahman, University of WollongongFollow
Jiazhao Wang, University of WollongongFollow
Mohd Faiz Hassan, University of WollongongFollow
Shulei Chou, University of WollongongFollow
David Wexler, University of WollongongFollow
Hua-Kun Liu, University of WollongongFollow

RIS ID

31834

Publication Details

Rahman, M. M., Wang, J., Hassan, M. Faiz., Chou, S., Wexler, D. Liu, H. K. (2010). Basic molten salt process-A new route for synthesis of nanocrystalline Li₄Ti₅O₁₂–TiO₂ anode material for Li-ion batteries using eutectic mixture of LiNO₃–LiOH–Li₂O₂. Journal of Power Sources, 195 (13), 4297-4303.

Abstract

A nanocrystalline Li₄Ti₅O₁₂–TiO₂ duplex phase has been synthesized by a simple basic molten salt process (BMSP) using an eutectic mixture of LiNO₃–LiOH–Li₂O₂ at 400–500 °C. The microstructure and morphology of the Li₄Ti₅O₁₂–TiO₂ product are characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The sample prepared by heat-treating at 300 °C for 3 h (S-1) reveals dense agglomerates of ultra-fine nanocrystalline Li₄Ti₅O₁₂; with heat treatment at 400 °C for 3 h (S-2), there is a duplex crystallite size (fine < 10 nm, and coarse > 20 nm) of Li₄Ti₅O₁₂–TiO₂; at 500 °C for 3 h (S-3), a much coarser and less-dense distribution of lithium titanate (crystallite size ∼15–30 nm) is observed. According to the results of electrochemical testing, the S-2 sample shows initial discharge capacities of 193 mAh g⁻¹ at 0.2 C, 168 mAh g⁻¹ at 0.5 C, 146 mAh g⁻¹ at 1 C, 135 mAh g⁻¹ at 2 C, and 117 mAh g⁻¹ at 5 C. After 100 cycles, the discharge capacity is 138 mAh g⁻¹ at 1 C with a capacity retention of 95%. The S-2 sample yields the best electrochemical performance in terms of charge–discharge capacity and rate capability compared with other samples. Its superior electrochemical performance can be mainly attributed to the duplex crystallite structure, composed of fine (<10 >nm) and coarse (>20) nm nanoparticles, where lithium ions can be stored within the grain boundary interfaces between the spinel Li₄Ti₅O₁₂ and the anatase TiO₂.