Physico-chemical and structural investigation of aluminium isopropoxide

Turova, Nataliya; Kozunov, V.A.; Yanovskii, A. I.; Bokii, N. G.; Struchkov, Yu. T.; Tarnopol'skii, B. L.

doi:10.1016/0022-1902(79)80384-x

Cited by 122 publications

(53 citation statements)

References 23 publications

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“…This is known to cause de-oligomerization of the tetrameric units [2,10,11]. According to literature, the solution consists mainly of dimeric and trimeric species after fast cooling to room temperature, but some tetrameric [Al(O i Pr) 3 ] 4 is still present or reformed.…”

Section: Methodsmentioning

confidence: 99%

“…All signals were assigned by COSY, HSQC and HMBC NMR spectroscopy, showing the coexistence of more than one species in solution, but with one clearly dominating form. The methine signals of the iso-propoxo are clearly assigned to bridging and terminal groups, but in the CH 3 2 , and an X-ray crystal structure analysis was carried out. Although the quality of the data set was affected by formation of thin platelets and partial decomposition of the crystal during the measurement, the dimeric nature of the compound with one octahedrally and one tetrahedrally coordinated aluminum atom was confirmed (Fig.…”

Section: Methodsmentioning

confidence: 99%

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Modification of aluminum alkoxides with β-ketoesters: new insights into formation, structure and stability

Lichtenberger

Puchberger

Baumann

et al. 2009

J Sol-Gel Sci Technol

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Pr) 2 (b-ketoesterate)] 2 derivatives are asymmetrically substituted dimers with one octahedrally and one tetrahedrally substituted aluminum atom, bridged by two isopropoxo groups, whereas the Al(b-ketoesterate) 3 derivatives are monomers with octahedrally coordinated aluminum. Transesterification as a possible side reaction was only observed at elevated temperatures for Al(tert-butyl acetoacetate) 3 in the presence of liberated iso-propanol.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Modification of aluminum alkoxides with β-ketoesters: new insights into formation, structure and stability

Lichtenberger

Puchberger

Baumann

et al. 2009

J Sol-Gel Sci Technol

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“…[37] In these studies, none of the invoked mechanisms takes into account the oligonuclear structure of ATI mainly consisting of tetranuclear molecules. [38][39][40][41] In the present study we address the question of the dependence of the composition of films processed by ATI-MOCVD upon experimental parameters, mainly the deposition temperature. This paper is limited to films prepared without an additional oxygen source in the gas phase.…”

Section: Introductionmentioning

confidence: 99%

CVD‐Fabricated Aluminum Oxide Coatings from Aluminum tri‐iso‐propoxide: Correlation Between Processing Conditions and Composition

Gleizes

Vahlas

Sovar

et al. 2007

Chemical Vapor Deposition

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This paper presents results on aluminum oxide thin films processed using metal-organic (MO) CVD from aluminum tri-isopropoxide (ATI) without any additional oxygen source, in the temperature range 623-973 K. The films do not diffract X-rays, except when grown at 973 K or annealed at 1073 K. Their composition was investigated using several techniques; electron probe micro analysis (EPMA), energy dispersive X-ray spectroscopy (EDX), elastic recoil detection analysis (ERDA), and Rutherford back-scattering spectroscopy (RBS). It corresponds to the formula AlO(OH) for those grown at 623 K. The composition of films prepared above 688 K corresponds to the formula Al 2 O 3 . Between 623 K and 688 K, partly hydroxylated films are obtained. This is confirmed by Fourier transform infrared (FTIR) transmission spectroscopy (no OH absorption band in the 3500 cm -1 region for films prepared above 688 K), and by thermogravimetric analysis (TGA, DTG) (no significant mass loss for films prepared above 688 K). Observations using the transmission electron microscopy (TEM) showed that films prepared at 623 K are amorphous, while those prepared at 973 K are nanocrystalline. In both cases, c-Al 2 O 3 crystals are formed and progressively grow on exposure to the TEM electron beam. Knowing the correlation between processing conditions and the composition of such films should help optimize the process with regards to any aimed property of use.

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“…[ 11 ] The ATI molecule is well described in the literature. [ 17 ] It is sensitive to water vapor and thus it is subjected to ageing upon exposure to ambient atmosphere, which results in its partial or total hydrolysis in nonvolatile compounds, Al(O i Pr) 3− n (OH) n ( n = 1, 2) and Al(OH) 3 , respectively. [ 12,17 ] The precursor is usually melted, maintained in supercooled state, and vaporized with a bubbler.…”

Section: Doi: 101002/admi201600014mentioning

confidence: 99%

“…[ 12,17 ] The precursor is usually melted, maintained in supercooled state, and vaporized with a bubbler.…”

mentioning

confidence: 99%

Amorphous Alumina Barrier Coatings on Glass: MOCVD Process and Hydrothermal Aging

Etchepare

Baggetto

Vergnes

et al. 2016

Adv Materials Inter

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OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible. This is an author-deposited version published in : http://oatao.univ-toulouse.fr/ Eprints ID : 15772 [ 9 ] radio frequency magnetron sputtering, [ 2 ] atomic layer deposition, [ 10 ] sol-gel, [ 5 ] and metalorganic chemical vapor deposition (MOCVD). [ 7,[11][12][13] CVD is one of the most attractive techniques for the time effi cient deposition of such coatings on complexin-shape geometries with conformal coverage, i.e., uniform thickness along the surface. Composition, stoichiometry, crystallinity, and microstructure of the material can be adjusted by fi ne tuning of the MOCVD experimental parameters such as reactor design, precursor selection, reactive atmosphere, deposition temperature, and pressure. The MOCVD of alumina from vaporized aluminum tri-isopropoxide (ATI) is very well documented. [ 7,8,[11][12][13][14][15][16] ATI yields amorphous and stoichiometric alumina coatings with a smooth and dense microstructure at 5 Torr in the temperature range 420 to 650 °C. [ 7,8,14,15 ] Higher process temperatures lead to the deposition of nanocrystallized γ -Al 2 O 3 [ 15 ] or to the homogeneous decomposition of ATI, which generates a different microstructure. [ 11 ] The ATI molecule is well described in the literature.[ 17 ] It is sensitive to water vapor and thus it is subjected to ageing upon exposure to ambient atmosphere, which results in its partial or total hydrolysis in nonvolatile compounds, Al(O i Pr) 3− n (OH) n ( n = 1, 2) and Al(OH) 3 , respectively. [ 12,17 ] The precursor is usually melted, maintained in supercooled state, and vaporized with a bubbler.Despite the simplicity and the cost effectiveness of this solution, the use of ATI in the supercooled state has two drawbacks. First, maintaining ATI at the vaporization temperature for a long-period impacts the stability of the molecule and subsequently the coating quality. [ 12 ] Second, it is diffi cult to know exactly the mass fl ow rate of the generated reactive gas. Such poorly controlled transport conditions lead to nonreproducible processes, especially for the present case when low activation energy prevails in the entire temperature range of interest, de facto resulting in mass transport limited process. The direct liquid injection (DLI) technology overcomes these drawbacks with the controlled vaporization of the solution made of ATI dissolved in a carrier solvent. [ 18 ] The DLI of ATI is insuffi ciently documented in the literature. Song et al. [ 19 ] and Krumdieck et al. [ 13 ] implemented the technique in a pulsedpressure MOCVD process. The authors used a solution of ATI in n -octane and in dry toluene, respectively. Coatings obtained

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Physico-chemical and structural investigation of aluminium isopropoxide

Cited by 122 publications

References 23 publications

Modification of aluminum alkoxides with β-ketoesters: new insights into formation, structure and stability

Modification of aluminum alkoxides with β-ketoesters: new insights into formation, structure and stability

CVD‐Fabricated Aluminum Oxide Coatings from Aluminum tri‐iso‐propoxide: Correlation Between Processing Conditions and Composition

Amorphous Alumina Barrier Coatings on Glass: MOCVD Process and Hydrothermal Aging

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