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Volume 115
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Lithium content effects on the phase evolution, microstructure and morphology of hydrothermally synthesized Li4Ti5O12-TiO2 nanocomposites
Hamed Aghamohammadi a *, Atousa Khazaeli b, Reza Eslami-Farsani b
a Department of Advanced Materials and New Technologies, Iranian Research Organization for Science and Technology (IROST), Tehran, Iran <> b Faculty of Materials Science and Engineering, K. N. Toosi University of Technology, Tehran, Iran
10.1016/j.partic.2026.05.003
Volume 115, August 2026, Pages 47-54
Received 12 April 2026, Revised 6 May 2026, Accepted 8 May 2026, Available online 12 May 2026, Version of Record 22 May 2026.
E-mail: aghamohammadi@irost.ir; hamed.aghamohammadi@outlook.com
Highlights

• Effects of different LiOH·H2O:TBT ratios on the hydrothermal synthesis of LTO-TiO2 investigated.

• Phase, microstructure, and morphology of the samples were studied.

• Phase evolution occurred by increasing the Li precursors ratios.

• LTO crystallite size reduced from 40nm to 20–21 nm with increasing Li content.

• Higher Li ratios favor LTO-TiO2 rutile nanocomposites with refined morphology.


Abstract

Li4Ti5O12-TiO2 nanocomposites represent highly promising materials for energy storage applications owing to their attractive electrochemical properties. However, precisely optimizing their morphology and compositions is essential. In this study, the effects of lithium content on the synthesis of the Li4Ti5O12-TiO2 nanocomposites prepared by the hydrothermal method were investigated. The samples were prepared using different molar ratios of LiOH·H2O: tertbutyl titanate (TBT) (4:5, 6:5, 8:5, 10:5, and 12:5) using a hydrothermal process at 180 °C for 12 h, followed by a calcination step. The microstructure, phase analysis, and morphology of the samples were investigated using X-ray diffraction (XRD), Raman spectroscopy, and field-emission scanning electron microscopy (FESEM) analyses. XRD results showed a phase evolution from an anatase-rich TiO2 (at a ratio of 4:5) to a Li4Ti5O12-dominated nanocomposite (at a ratio of 12:5) with a minor TiO2 rutile phase. Also, the crystallite size of the Li4Ti5O12 phase first increased to a maximum value of 47.3 nm and then decreased to 20–21 nm at higher ratios. FESEM images revealed a growth in particle size of the samples from 138 to 196 nm, by increasing the ratio from 4:5 to 6:5, and then a reduction of particle size to about 55 nm by using higher ratios. The results showed that for achieving Li4Ti5O12-TiO2 rutile nanocomposites with nanoscale particles, higher LiOH·H2O:TBT ratios are preferred.

Graphical abstract
Keywords
Li4Ti5O12-TiO2 nanocomposite; Hydrothermal synthesis; Lithium precursor ratio; Microstructure; Morphology
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