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Main Title: Atomic layer deposition on porous powders with in situ gravimetric monitoring in a modular fixed bed reactor setup
Author(s): Strempel, Verena E.
Naumann d’Alnoncourt, Raoul
Drieß, Matthias
Rosowski, Frank
Type: Article
Abstract: A modular setup for Atomic Layer Deposition (ALD) on high-surface powder substrates in fixed bed reactors with a gravimetric in situ monitoring was developed. The design and operation are described in detail. An integrated magnetically suspended balance records mass changes during ALD. The highly versatile setup consists of three modular main units: a dosing unit, a reactor unit, and a downstream unit. The reactor unit includes the balance, a large fixed bed reactor, and a quartz crystal microbalance. The dosing unit is equipped with a complex manifold to deliver gases and gaseous reagents including three different ALD precursors, five oxidizing or reducing agents, and two purge gas lines. The system employs reactor temperatures and pressures in the range of 25-600 °C and 10−3 to 1 bar, respectively. Typically, powder batches between 100 mg and 50 g can be coated. The capabilities of the setup are demonstrated by coating mesoporous SiO2 powder with a thin AlOx (submono) layer using three cycles with trimethylaluminium and H2O. The self-limiting nature of the deposition has been verified with the in situ gravimetric monitoring and full saturation curves are presented. The process parameters were used for a scale-up in a large fixed bed reactor. The samples were analyzed with established analytics such as X-ray diffraction, N2 adsorption, transmission electron microscopy, and inductively coupled plasma optical emission spectrometry.
Subject(s): atomic layer deposition
fixed bed reactor
metal oxide
Issue Date: 19-Jul-2017
Date Available: 15-May-2020
Language Code: en
DDC Class: 660 Chemische Verfahrenstechnik
Sponsor/Funder: DFG, 53182490, EXC 314: Unifying Concepts in Catalysis
Journal Title: Review of Scientific Instruments
Publisher: American Institute of Physics (AIP)
Volume: 88
Issue: 7
Article Number: 074102
Publisher DOI: 10.1063/1.4992023
EISSN: 1089-7623
ISSN: 0034-6748
Notes: This article may be downloaded for personal use only. Any other use requires prior permission of the author and AIP Publishing. This article appeared in Review of Scientific Instruments 88, 074102 (2017) and may be found at
TU Affiliation(s): Verbundforschung » Exzellenzcluster (EXC) » BasCat Joint Lab
 » BasCat Joint Lab
Fak. 2 Mathematik und Naturwissenschaften » Inst. Chemie » FG Metallorganische Chemie und Anorganische Materialien
Appears in Collections:Technische Universität Berlin » Publications

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