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Structural and Dynamic Properties of Gallium Alkoxides

Mears, KL; Bloor, LG; Pugh, D; Aliev, AE; Knapp, CE; Carmalt, CJ; (2019) Structural and Dynamic Properties of Gallium Alkoxides. Inorganic Chemistry , 58 (15) pp. 10346-10356. 10.1021/acs.inorgchem.9b01496. Green open access

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Abstract

A comparison of chlorido-gallium functionalized alkoxides as precursors for aerosol-assisted chemical vapor deposition (AACVD) was carried out. Variable-temperature (VT)-NMR studies were used to probe the fluxional behavior of these alkoxides in solution, and hence their utility as precursors. The synthesis involved the initial isolation of the dimer [GaCl(NMe2)2]2 via a salt metathesis route from GaCl3 and 2 equiv of LiNMe2. This dimer was then reacted with 4 equiv of HOCH2CH2CH2NEt2, resulting in the formation of Ga[μ-(OCH2CH2CH2NEt2)2GaCl2]3 (1). Mass spectrometry and VT-NMR confirmed the oligomeric structure of 1. Tuning of the ligand properties, namely, the chain length and substituents on N, resulted in formation of the monomers [GaCl(OR)2] (R = CH2CH2NEt2, (2); CH2CH2CH2NMe2, (3)). VT-NMR studies, supported by density functional theory calculations, confirmed that the ligands in both 2 and 3 possess a hemilabile coordination to the gallium center, owing to either a shorter carbon backbone (2) or less steric hindrance (3). Both 2 and 3 were selected for use as precursors for AACVD: deposition at 450 °C gave thin films of amorphous Ga2O3, which were subsequently annealed at 1000 °C to afford crystalline Ga2O3 material. The films were fully characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, UV-visible spectroscopy, and energy dispersive X-ray analysis.

Type: Article
Title: Structural and Dynamic Properties of Gallium Alkoxides
Open access status: An open access version is available from UCL Discovery
DOI: 10.1021/acs.inorgchem.9b01496
Publisher version: https://doi.org/10.1021/acs.inorgchem.9b01496
Language: English
Additional information: Copyright © 2019 American Chemical Society. This is an open access article published under a Creative Commons (CC-BY) Attribution 4.0 International Public License, which permits unrestricted use, distribution and reproduction in any medium, provided the author and source are cited.
Keywords: Thin films, Ligands, Precursors, Gallium, Deposition
UCL classification: UCL
UCL > Provost and Vice Provost Offices > UCL BEAMS
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Maths and Physical Sciences
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Maths and Physical Sciences > Dept of Chemistry
URI: https://discovery.ucl.ac.uk/id/eprint/10078889
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