The formation mechanism of Li                         4                         Ti                         5                         O                         12−y                          solid solutions prepared by carbothermal reduction and the effect of Ti                         3+                          on electrochemical performance

Guijun Yang; Soo Jin Park

doi:10.1038/s41598-019-41206-0

The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance

Guijun Yang
, Soo Jin Park

Inha University

Research output: Contribution to journal › Article › peer-review

Abstract

Samples of Li ₄ Ti ₅ O _12−y solid solutions are synthesized by one-step solid-state carbothermal reduction reaction using Li ₂ CO ₃ , anatase, and carbon black under a nitrogen atmosphere. The underlying formation mechanism that leads to Li ₄ Ti ₅ O _12−y solid solutions is proposed. The formation mechanism of the Li ₄ Ti ₅ O _12−y solid solution is investigated by in situ variable temperature X-Ray diffraction (VT-XRD) and thermogravimetric analysis/differential scanning calorimetry (TGA-DSC). First, some Ti ⁴⁺ centers are converted to Ti ³⁺ (TiO ₂ -TiO _2−x ) because of the presence of carbon black. Secondly, Li ₂ CO ₃ reacts with TiO _2−x (anatase) to form Li ₂ TiO ₃ . Thirdly, Li ₂ TiO ₃ reacts with TiO _2−x to form the Li ₄ Ti ₅ O _12−y solid solution, while anatase starts to transform into rutile at the same time. Rutile reacts with Li ₂ TiO ₃ to form Li ₄ Ti ₅ O _12−y at higher temperatures. The presence of Ti ³⁺ not only improves the electrical conductivity but also improves the ionic conductivity. As a result, the as-prepared material exhibits good rate capability and cycling stability with 99.3% capacity retention after 200 cycles.

Original language	English
Article number	4774
Journal	Scientific Reports
Volume	9
Issue number	1
DOIs	https://doi.org/10.1038/s41598-019-41206-0
Publication status	Published - 1 Dec 2019
Externally published	Yes

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Yang, G., & Park, S. J. (2019). The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance Scientific Reports, 9(1), Article 4774. https://doi.org/10.1038/s41598-019-41206-0

Yang, Guijun ; Park, Soo Jin. / The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance In: Scientific Reports. 2019 ; Vol. 9, No. 1.

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title = " The formation mechanism of Li 4 Ti 5 O 12−y solid solutions prepared by carbothermal reduction and the effect of Ti 3+ on electrochemical performance ",

abstract = " Samples of Li 4 Ti 5 O 12−y solid solutions are synthesized by one-step solid-state carbothermal reduction reaction using Li 2 CO 3 , anatase, and carbon black under a nitrogen atmosphere. The underlying formation mechanism that leads to Li 4 Ti 5 O 12−y solid solutions is proposed. The formation mechanism of the Li 4 Ti 5 O 12−y solid solution is investigated by in situ variable temperature X-Ray diffraction (VT-XRD) and thermogravimetric analysis/differential scanning calorimetry (TGA-DSC). First, some Ti 4+ centers are converted to Ti 3+ (TiO 2 -TiO 2−x ) because of the presence of carbon black. Secondly, Li 2 CO 3 reacts with TiO 2−x (anatase) to form Li 2 TiO 3 . Thirdly, Li 2 TiO 3 reacts with TiO 2−x to form the Li 4 Ti 5 O 12−y solid solution, while anatase starts to transform into rutile at the same time. Rutile reacts with Li 2 TiO 3 to form Li 4 Ti 5 O 12−y at higher temperatures. The presence of Ti 3+ not only improves the electrical conductivity but also improves the ionic conductivity. As a result, the as-prepared material exhibits good rate capability and cycling stability with 99.3\% capacity retention after 200 cycles.",

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Yang, G & Park, SJ 2019, ' The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance ', Scientific Reports, vol. 9, no. 1, 4774. https://doi.org/10.1038/s41598-019-41206-0

The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance . / Yang, Guijun; Park, Soo Jin.
In: Scientific Reports, Vol. 9, No. 1, 4774, 01.12.2019.

Research output: Contribution to journal › Article › peer-review

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N2 - Samples of Li 4 Ti 5 O 12−y solid solutions are synthesized by one-step solid-state carbothermal reduction reaction using Li 2 CO 3 , anatase, and carbon black under a nitrogen atmosphere. The underlying formation mechanism that leads to Li 4 Ti 5 O 12−y solid solutions is proposed. The formation mechanism of the Li 4 Ti 5 O 12−y solid solution is investigated by in situ variable temperature X-Ray diffraction (VT-XRD) and thermogravimetric analysis/differential scanning calorimetry (TGA-DSC). First, some Ti 4+ centers are converted to Ti 3+ (TiO 2 -TiO 2−x ) because of the presence of carbon black. Secondly, Li 2 CO 3 reacts with TiO 2−x (anatase) to form Li 2 TiO 3 . Thirdly, Li 2 TiO 3 reacts with TiO 2−x to form the Li 4 Ti 5 O 12−y solid solution, while anatase starts to transform into rutile at the same time. Rutile reacts with Li 2 TiO 3 to form Li 4 Ti 5 O 12−y at higher temperatures. The presence of Ti 3+ not only improves the electrical conductivity but also improves the ionic conductivity. As a result, the as-prepared material exhibits good rate capability and cycling stability with 99.3% capacity retention after 200 cycles.

AB - Samples of Li 4 Ti 5 O 12−y solid solutions are synthesized by one-step solid-state carbothermal reduction reaction using Li 2 CO 3 , anatase, and carbon black under a nitrogen atmosphere. The underlying formation mechanism that leads to Li 4 Ti 5 O 12−y solid solutions is proposed. The formation mechanism of the Li 4 Ti 5 O 12−y solid solution is investigated by in situ variable temperature X-Ray diffraction (VT-XRD) and thermogravimetric analysis/differential scanning calorimetry (TGA-DSC). First, some Ti 4+ centers are converted to Ti 3+ (TiO 2 -TiO 2−x ) because of the presence of carbon black. Secondly, Li 2 CO 3 reacts with TiO 2−x (anatase) to form Li 2 TiO 3 . Thirdly, Li 2 TiO 3 reacts with TiO 2−x to form the Li 4 Ti 5 O 12−y solid solution, while anatase starts to transform into rutile at the same time. Rutile reacts with Li 2 TiO 3 to form Li 4 Ti 5 O 12−y at higher temperatures. The presence of Ti 3+ not only improves the electrical conductivity but also improves the ionic conductivity. As a result, the as-prepared material exhibits good rate capability and cycling stability with 99.3% capacity retention after 200 cycles.

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Yang G, Park SJ. The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance Scientific Reports. 2019 Dec 1;9(1):4774. doi: 10.1038/s41598-019-41206-0

The formation mechanism of Li ₄ Ti ₅ O _12−y solid solutions prepared by carbothermal reduction and the effect of Ti ³⁺ on electrochemical performance

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