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Main Title: Investigating the trimethylaluminium/water ALD process on mesoporous silica by in situ gravimetric monitoring
Author(s): Strempel, Verena E.
Knemeyer, Kristian
Naumann d’Alnoncourt, Raoul
Rosowski, Frank
Type: Article
Language Code: en
Abstract: A low amount of AlOx was successfully deposited on an unordered, mesoporous SiO2 powder using 1–3 ALD (Atomic Layer Deposition) cycles of trimethylaluminium and water. The process was realized in a self-built ALD setup featuring a microbalanceand a fixed particle bed. The reactor temperature was varied between 75, 120, and 200 °C. The self-limiting nature of the deposition was verified by in situ gravimetric monitoring for all temperatures. The coated material was further analyzed by nitrogen sorption, inductively coupled plasma-optical emission spectroscopy, powder X-ray diffraction, high-resolution transmission electron microscopy, attenuated total reflection Fourier transformed infrared spectroscopy, and elemental analysis. The obtained mass gains correspond to average growth between 0.81–1.10 Å/cycle depending on substrate temperature. In addition, the different mass gains during the half-cycles in combination with the analyzed aluminum content after one, two, and three cycles indicate a change in the preferred surface reaction of the trimethylaluminium molecule from a predominately two-ligand exchange with hydroxyl groups to more single-ligand exchange with increasing cycle number. Nitrogen sorption isotherms demonstrate (1) homogeneously coated mesopores, (2) a decrease in surface area, and (3) a reduction of the pore size. The experiment is successfully repeated in a scale-up using a ten times higher substrate batch size.
Issue Date: 24-May-2018
Date Available: 31-May-2018
DDC Class: 570 Biowissenschaften; Biologie
540 Chemie
Subject(s): atomic layer deposition
in situ gravimetric
mesoporous silica
ligand exchange
fixed bed
particle coating
Sponsor/Funder: DFG, TH 662/19-1, Open Access Publizieren 2017 - 2018 / Technische Universität Berlin
Journal Title: Nanomaterials
Publisher: MDPI
Publisher Place: Basel
Volume: 8
Issue: 6
Article Number: 365
Publisher DOI: 10.3390/nano8060365
Page Start: 1
Page End: 14
ISSN: 2079-4991
Appears in Collections:FG Metallorganische Chemie und Anorganische Materialien » Publications

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