Abstract

POZADAS, Luz J. et al. Nueva ruta de síntesis atrano/hidro-solvotermal para el control del tamaño de nanopartícula de Li₄Ti₅O₁₂ a través del uso de TOHAC's. Rev. Bol. Quim [online]. 2023, vol.40, n.1, pp.8-20. ISSN 0250-5460.  https://doi.org/10.34098/2078-3949.40.1.2.

New atrane/ hydro-solvothermal synthesis route for the control of the size of Li4Ti5O12 nanoparticle through the use of TOHAC's. In the present work, a new wet chemical synthesis route called "Atrane/Hydro-Solvothermal" is proposed, which allows obtaining Li4Ti5O12 (LTO) nanoparticles with predefined sizes. This is achieved by controlling the growth rate of the hydrolysis and condensation processes of metal atrane clusters formed in aqueous and solvothermal solutions. LTO nanoparticles were synthesized from atrane precursors (lithiatrane, titanatrane). These form complexes of oligomeric species called "Titanium-Oxo-Hydroxo-atrane clusters" (TOHAC's) nanoparticles. The TOHAC's with predefined sizes are obtained by controlling the hydrolysis and condensation time. The average diameter size of the formed TOHAC's was characterized by the dynamic light scattering technique (DLS), obtaining average sizes of 2.4, 7.17, 20.13, 40 nm for the samples (B:0), (B:48), (B:144), and (B:288), respectively. The TOHAC’s are used as building blocks, followed by a Hydro-Solvothermal treatment, and a thermal treatment at 500°C. The XRD diffractograms of the products have shown the presence of Li4Ti5O12 (LTO) as the major phase with a spinel structure, and the monoclinic β-Li2TiO3 as the minor phase. The SEM images show particles with an average size of 12.82 ±5 nm (LTO: B:0), 10.03 ±3 nm (LTO: B:48), 20.03 ±7.6 nm (LTO: B:144), and 40.0 ±5 nm (LTO: B:288). The particle sizes were correlated with the TOHAC's (building blocks) used.

Keywords : Lithium titanate; Titanium-oxo-hydroxo atrane clusters; TOHAC´s; Atrane ,Litanatrane; Tithiatrane; Building blocks.

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