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.
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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 |
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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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