Amorphous Alumina Coatings: Processing, Structure and Remarkable Barrier Properties

Samélor, Diane; Lazar, A. P.; Aufray, Maëlenn; Tendero, Claire; Lacroix, Loïc; Béguin, Jean-Denis; Caussat, Brigitte; Vergnes, Hugues; Alexis, Joël; Poquillon, Dominique; Pébère, Nadine; Gleizes, Alain; Vahlas, Constantin

doi:10.1166/jnn.2011.5068

Cited by 19 publications

(15 citation statements)

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“…[ 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.…”

Section: Doi: 101002/admi201600014mentioning

confidence: 99%

“…[ 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.…”

Section: Doi: 101002/admi201600014mentioning

confidence: 99%

“…[ 6 ] In particular, amorphous alumina coatings present interesting physicochemical characteristics whose nature, extent, and combination depend on the processing conditions. [ 7,8 ] With the aim to process dense, adherent, and durable alumina coatings on metal or polymer substrates various between 500 and 550 °C at a nominal base pressure of 0.6 Torr were stoichiometric, amorphous, and presented a nodular surface morphology.…”

Section: Introductionmentioning

confidence: 99%

“…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.…”

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confidence: 99%

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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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Section: Doi: 101002/admi201600014mentioning

confidence: 99%

Section: Doi: 101002/admi201600014mentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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

Etchepare

Baggetto

Vergnes

et al. 2016

Adv Materials Inter

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“…Films composed of a-Al 2 O 3 are selected for this purpose due to their excellent barrier and anti-corrosion properties [19][20][21][22] and high optical transmission [23]. They compete with silica based coatings which also present excellent barrier properties, although limited durability [24].…”

Section: Introductionmentioning

confidence: 99%

Modeling a MOCVD process to apply alumina films on the inner surface of bottles

Etchepare¹,

Vergnes²,

Samélor³

et al. 2015

Surface and Coatings Technology

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a b s t r a c tDeposition inside a cavity with a narrow neck, i.e. a hollow body, is a challenge, in particular for the supply and the evacuation of the reactive phase and of the effluents through the same entrance. High gradients (pressure, velocity, species concentrations) and important convective mechanisms related to the impacting jet of the gaseous phase on the bottom inner wall of the cavity are created in that region. Given the increasing number of experimental parameters, modeling helps efficient process optimization with better understanding of physical and chemical phenomena occurring inside the hollow body. This study presents a numerical modeling using the CFD code Fluent to simulate a direct liquid injection metalorganic chemical vapor deposition of amorphous alumina coatings from aluminum tri-isopropoxide (ATI) on the inner walls of a glass bottle. The model is used to predict local profiles of gas velocity, temperature and species concentrations into the reactor as well as local growth rate based on an apparent heterogeneous kinetic law of ATI decomposition. Comparison with experimental thickness profiles allows validating the model and leads to a better insight in the phenomena which impact film thickness inhomogeneity along the inner surface. The model contributes to the improvement of the reactor configuration by increasing the distance between nozzle and bottle and the outlet section of the nozzle.

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Process‐structure‐properties relationship in direct liquid injection chemical vapor deposition of amorphous alumina from aluminum tri‐isopropoxide

Etchepare

Baggetto

Vergnes

et al. 2015

Phys. Status Solidi C

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We propose a method to apply amorphous alumina films on the inner surface of glass containers aiming to improve their hydrothermal barrier property. We have carried out alumina deposition on Si substrates as a function of deposition temperature to determine the physico‐chemical properties of the thin film materials, and on glass containers to evaluate the influence of post‐deposition hydrothermal ageing on the films properties. Film preparation has been achieved by metal‐organic chemical vapor deposition (MOCVD), using tri‐isopropoxide aluminum (ATI) dissolved in anhydrous cyclohexane as precursor, in a temperature range between 360 °C and 600 °C. A direct liquid injection technology is used to feed the reactor in a controlled and reproducible way. The amorphous alumina films have been characterized by several techniques such as XRD, EPMA, XPS, SEM, AFM and scratch‐test method. Films are amorphous and hydroxylated at 360 and 420 °C and close to stoichiometric at 490 and 560 °C. Hydrothermal ageing simulated by a standard sterilization cycle modifies the adhesion and surface morphology of the alumina film on glass containers to a rough, porous and non‐adhesive layer. (© 2015 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)

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Amorphous Alumina Coatings: Processing, Structure and Remarkable Barrier Properties

Cited by 19 publications

References 0 publications

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

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

Modeling a MOCVD process to apply alumina films on the inner surface of bottles

Process‐structure‐properties relationship in direct liquid injection chemical vapor deposition of amorphous alumina from aluminum tri‐isopropoxide

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