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Volume 110
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Morphological convergence in solid-state synthesis: Unveiling the critical role of TiO2 precursor size for high-performance H2TiO3 lithium ion-sieves
Ye Wang, Yuxin Xie, Xiaojing Guo *, Xi Yan, Yan Chen, Ping Hu, Peng Cheng, Wanzhong Lang *
The Education Ministry Key Laboratory of Resource Chemistry, Shanghai Key Laboratory of Rare Earth Functional Materials, Department of Chemistry and Chemical Engineering, Shanghai Normal University, Shanghai, 200234, China
10.1016/j.partic.2025.12.023
Volume 110, March 2026, Pages 1-13
Received 20 October 2025, Revised 23 December 2025, Accepted 30 December 2025, Available online 8 January 2026, Version of Record 17 January 2026.
E-mail: guoxj@shnu.edu.cn; wzlang@shnu.edu.cn
Highlights

• Morphological convergence to 28–32 nm LTO occurs for sub-40 nm TiO2 precursors.

• A critical precursor size of 40 nm is identified for optimal H2TiO3 performance.

• The 40-HTO adsorbent delivers a high Li+ capacity of 58.02 mg g−1.

• 40-HTO's adsorption rate constant is 2.3-fold higher than that of 150 nm-derived sample.

• 40-HTO shows superb stability (<0.15 % Ti loss) and selectivity in brine.


Abstract

The solid-state synthesis of H2TiO3 (HTO) lithium ion-sieves is highly sensitive to the particle size of the TiO2 precursor, which governs both structural properties and ultimate adsorption performance. This study reveals a striking morphological convergence during the synthesis of Li2TiO3 (LTO) intermediates: despite employing TiO2 precursors spanning 15–40 nm, the resulting LTO particles consistently exhibited a narrow size range of 28–32 nm, indicating a distinctive size-regulation mechanism in the solid-state reaction. In contrast, precursors ≥60 nm led to fragmented structures with reduced crystallinity. Leveraging this finding, we identified 40 nm as a critical precursor size for crafting optimal HTO adsorbents. The 40 nm-derived HTO (40-HTO) delivered a superior equilibrium Li+ adsorption capacity of 58.02 mg g−1, a pseudo-second-order rate constant 2.3-fold higher than that of its 150 nm-derived counterpart, and exceptional cyclic stability (<0.15 % Ti dissolution over 10 cycles). Importantly, in a simulated concentrated brine with a high Mg2+/Li+ mass ratio of 20, 40-HTO maintained a high Li+ uptake of 36.5 mg g−1 and exhibited exceptional selectivity, with a separation factor as high as 780. This work underscores precursor size engineering, targeting a critical size threshold, as a vital strategy for developing high-efficiency lithium ion-sieves.

Graphical abstract
Keywords
Lithium; Adsorption; H2TiO3; Particle size
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