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

Kokkonen, E. LU orcid ; Kaipio, Mikko ; Nieminen, Heta Elisa ; Rehman, F. LU ; Miikkulainen, V. ; Putkonen, Matti ; Ritala, M. ; Huotari, Simo ; Schnadt, J. LU orcid and Urpelainen, Samuli (2022) In Review of Scientific Instruments 93(1).
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... (More)
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. (Less)
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author
; ; ; ; ; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Review of Scientific Instruments
volume
93
issue
1
article number
013905
publisher
American Institute of Physics (AIP)
external identifiers
  • pmid:35104956
  • scopus:85123032953
ISSN
1089-7623
DOI
10.1063/5.0076993
language
English
LU publication?
yes
id
a2ebceee-c2ee-47ab-8b20-3102cd6f643f
date added to LUP
2022-02-09 11:54:15
date last changed
2023-11-10 01:44:05
@article{a2ebceee-c2ee-47ab-8b20-3102cd6f643f,
  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.}},
  author       = {{Kokkonen, E. and Kaipio, Mikko and Nieminen, Heta Elisa and Rehman, F. and Miikkulainen, V. and Putkonen, Matti and Ritala, M. and Huotari, Simo and Schnadt, J. and Urpelainen, Samuli}},
  issn         = {{1089-7623}},
  language     = {{eng}},
  month        = {{01}},
  number       = {{1}},
  publisher    = {{American Institute of Physics (AIP)}},
  series       = {{Review of Scientific Instruments}},
  title        = {{Ambient pressure x-ray photoelectron spectroscopy setup for synchrotron-based in situ and operando atomic layer deposition research}},
  url          = {{http://dx.doi.org/10.1063/5.0076993}},
  doi          = {{10.1063/5.0076993}},
  volume       = {{93}},
  year         = {{2022}},
}