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

E. Kokkonen, Mikko Kaipio, Heta Elisa Nieminen, F. Rehman, V. Miikkulainen, Matti Putkonen, M. Ritala, Simo Huotari, J. Schnadt, Samuli Urpelainen

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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.
Original languageEnglish
Article number013905
JournalReview of Scientific Instruments
Issue number1
Publication statusPublished - 2022 Jan 10

Subject classification (UKÄ)

  • Atom and Molecular Physics and Optics
  • Accelerator Physics and Instrumentation
  • Condensed Matter Physics
  • Nano Technology

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