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对铝和镓氨基烯醇酸酯配合物的结构、反应活性及气溶胶辅助化学气相沉积的研究。

Investigations into the structure, reactivity, and AACVD of aluminium and gallium amidoenoate complexes.

作者信息

Mears Kristian L, Bhide Malavika A, Knapp Caroline E, Carmalt Claire J

机构信息

Department of Chemistry, University College London, 20 Gordon Street, London, WC1H 0AJ, UK.

出版信息

Dalton Trans. 2021 Dec 20;51(1):156-167. doi: 10.1039/d1dt03365d.

Abstract

Amidoenoate (AME = {ethyl-3-(R-amido)but-2-enoate}) complexes of aluminium and gallium, of the type: [AlCl(AME)] R = iPr (1-Al); [AlCl(AME)] R = iPr (2-Al), Dip (3-Al); [GaCl(AME)] R = iPr (1-Ga) and [GaCl(AME)] R = iPr (2-Ga), Dip (3-Ga), have been synthesised (iPr = isopropyl, Dip = 2,6-diisopropylphenyl). The coordination chemistry of these complexes has been studied in relation to precursor suitability. Investigations into the reactivity of the aluminium and gallium amidoenoate complexes involved reactions with hydride sources including alkali metal hydride salts, alkylsilanes, and magnesium hydride species and magnesium(I) dimers. The isolation of alkyl metal amidoenoate precursors including an aluminium hydride amidoenoate, [AlH(AME)] (4-Al) and dimethyl gallium amidoenoates [GaMe(AME)] (4-Ga), [GaMe(AME)] (5-Ga) concluded the synthetic studies. A selection of the isolated complexes were used as precursors for aerosol assisted chemical vapour deposition (AACVD) at 500 °C. Thin films of either amorphous AlO or GaO were deposited and subsequently annealed at 1000 °C to improve the materials' crystallinity. The films were characterised by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), UV-visible (UV-vis) spectroscopy and energy dispersive X-ray analysis (EDXA).

摘要

铝和镓的氨基烯酸酯(AME = {乙基 - 3 - (R - 氨基)丁 - 2 - 烯酸酯})配合物,类型如下:[AlCl(AME)],R = 异丙基(1 - Al);[AlCl(AME)],R = 异丙基(2 - Al),二异丙基苯基(3 - Al);[GaCl(AME)],R = 异丙基(1 - Ga)和[GaCl(AME)],R = 异丙基(2 - Ga),二异丙基苯基(3 - Ga),已被合成(异丙基 = 异丙基,二异丙基苯基 = 2,6 - 二异丙基苯基)。已针对前体适用性研究了这些配合物的配位化学。对铝和镓氨基烯酸酯配合物的反应性研究涉及与氢化物源的反应,包括碱金属氢化物盐、烷基硅烷、氢化镁物种和镁(I)二聚体。分离出包括氢化铝氨基烯酸酯[AlH(AME)](4 - Al)和二甲基镓氨基烯酸酯[GaMe(AME)](4 - Ga)、[GaMe(AME)](5 - Ga)在内的烷基金属氨基烯酸酯前体,从而完成了合成研究。选择一些分离出的配合物作为500℃下气溶胶辅助化学气相沉积(AACVD)的前体。沉积了非晶态AlO或GaO薄膜,随后在1000℃下退火以提高材料的结晶度。通过X射线衍射(XRD)、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、紫外可见(UV - vis)光谱和能量色散X射线分析(EDXA)对薄膜进行了表征。

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