University of Oulu

E. Kokkonen, M. Kaipio, H.-E. Nieminen, F. Rehman, V. Miikkulainen, M. Putkonen, M. Ritala, S. Huotari, J. Schnadt, and S. Urpelainen, "Ambient pressure x-ray photoelectron spectroscopy setup for synchrotron-based in situ and operando atomic layer deposition research", Review of Scientific Instruments 93, 013905 (2022) https://doi.org/10.1063/5.0076993

Ambient pressure x-ray photoelectron spectroscopy setup for synchrotron-based in situ and operando atomic layer deposition research

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Author: Kokkonen, E.1; Kaipio, M.2; Nieminen, H.-E.2;
Organizations: 1MAX IV Laboratory, Lund University, Box 118, 221 00 Lund, Swed
2Department of Chemistry, University of Helsinki, FI-00014 Helsinki, Finland
3Division of Synchrotron Radiation Research, Department of Physics, Lund University, P.O. Box 118, 221 00 Lund, Sweden
4Department of Chemistry and Materials Science, Aalto University, 00076 Aalto, Finland
5Department of Chemistry, University of Helsinki, 00014 Helsinki, Finland
6Department of Physics, University of Helsinki, 00014 Helsinki, Finland
7MAX IV Laboratory, Lund University, Box 118, 221 00 Lund, Sweden
8Division of Synchrotron Radiation Research, Department of Physics, Lund University, Box 118, 221 00 Lund, Sweden
9Nano and Molecular Systems Research Unit, University of Oulu, 90014 Oulu, Finland
Format: article
Version: published version
Access: open
Online Access: PDF Full Text (PDF, 5.9 MB)
Persistent link: http://urn.fi/urn:nbn:fi-fe2022041128044
Language: English
Published: American Institute of Physics, 2022
Publish Date: 2022-04-11
Description:

Abstract

An ambient pressure cell is described for conducting synchrotron-based x-ray photoelectron spectroscopy (XPS) measurements during atomic layer deposition (ALD) processes. The instrument is capable of true in situ and operando experiments in which it is possible to directly obtain elemental and chemical information from the sample surface using XPS as the deposition process is ongoing. The setup is based on the ambient pressure XPS technique, in which sample environments with high pressure (several mbar) can be created without compromising the ultrahigh vacuum requirements needed for the operation of the spectrometer and the synchrotron beamline. The setup is intended for chemical characterization of the surface intermediates during the initial stages of the deposition processes. The SPECIES beamline and the ALD cell provide a unique experimental platform for obtaining new information on the surface chemistry during ALD half-cycles at high temporal resolution. Such information is valuable for understanding the ALD reaction mechanisms and crucial in further developing and improving ALD processes. We demonstrate the capabilities of the setup by studying the deposition of TiO₂ on a SiO₂ surface by using titanium(IV) tetraisopropoxide and water as precursors. Multiple core levels and the valence band of the substrate surface were followed during the film deposition using ambient pressure XPS.

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Series: Review of scientific instruments
ISSN: 0034-6748
ISSN-E: 1089-7623
ISSN-L: 0034-6748
Volume: 93
Article number: 013905
DOI: 10.1063/5.0076993
OADOI: https://oadoi.org/10.1063/5.0076993
Type of Publication: A1 Journal article – refereed
Field of Science: 114 Physical sciences
116 Chemical sciences
215 Chemical engineering
216 Materials engineering
221 Nanotechnology
Subjects:
Funding: The ALD cell is a result of collaboration between the University of Helsinki (Finland) and the MAX IV Laboratory and funded by the Faculty of Science, University of Helsinki and Academy of Finland (Grant No. 295696) under the operations collaboration agreement between Finland (FIMAX consortium) and the MAX IV Laboratory. Research conducted at MAX IV, a Swedish national user facility, is supported by the Swedish Research Council under Contract No. 2018-07152, the Swedish Governmental Agency for Innovation Systems under Contract No. 2018-04969, and Formas under Contract No. 2019-02496. M.P. acknowledges funding from the Academy of Finland by the profiling action on Matter and Materials (Grant No. 318913). M.R. acknowledges funding from the Academy of Finland (Grant No. 309552). J.S. acknowledges funding from Vetenskapsrådet (Swedish Research Council) under Grant No. 2017-03871.
Copyright information: © 2022 Author(s). All article content, except where otherwise noted, is licensed under a Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/).
  https://creativecommons.org/licenses/by/4.0/