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Al capping layers for non-destructive x-ray photoelectron spectroscopy analyses of transition-metal nitride thin films
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. (Thin Film Physics)ORCID iD: 0000-0002-4898-5115
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. (Thin Film Physics)
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. (Thin Film Physics)
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. (Thin Film Physics)ORCID iD: 0000-0002-2837-3656
2015 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 33, 05E101-1-05E101-9 p., 05E101Article in journal (Refereed) Published
Abstract [en]

X-ray photoelectron spectroscopy (XPS) compositional analyses of materials that have been air exposed typically require ion etching in order to remove contaminated surface layers. However, the etching step can lead to changes in sample surface and near-surface compositions due to preferential elemental sputter ejection and forward recoil implantation; this is a particular problem for metal/gas compounds and alloys such as nitrides and oxides. Here, we use TiN as a model system and compare XPS analysis results from three sets of polycrystalline TiN/Si(001) films deposited by reactive magnetron sputtering in a separate vacuum chamber. The films are either (a) air-exposed for ? 10 min prior to insertion into the ultra-high-vacuum (UHV) XPS system; (b) air-exposed and subject to ion etching, using different ion energies and beam incidence angles, in the XPS chamber prior to analysis; or (c) Al-capped in-situ in the deposition system prior to air-exposure and loading into the XPS instrument.We show that thin, 1.5-6.0 nm, Al capping layers provide effective barriers to oxidation and contamination of TiN surfaces, thus allowing non-destructive acquisition of high-resolution core-level spectra representative of clean samples, and, hence, correct bonding assignments. The Ti 2p and N 1s satellite features, which are sensitive to ion bombardment, exhibit high intensities comparable to those obtained from single-crystal TiN/MgO(001) films grown and analyzed in-situ in a UHV XPS system and there is no indication of Al/TiN interfacial reactions. XPS-determined N/Ti concentrations acquired from Al/TiN samples agree very well with Rutherford backscattering and elastic recoil analysis results while ion-etched air-exposed samples exhibit strong N loss due to preferential resputtering. The intensities and shapes of the Ti 2p and N 1s core level signals from Al/TiN/Si(001) samples do not change following long-term (up to 70 days) exposure to ambient conditions indicating that the thin Al capping layers provide stable surface passivation without spallation.

Place, publisher, year, edition, pages
American Vacuum Society , 2015. Vol. 33, 05E101-1-05E101-9 p., 05E101
Keyword [en]
XPS; TiN; capping layers; oxidation protection; sputtering; surface passivation
National Category
Condensed Matter Physics
Identifiers
URN: urn:nbn:se:liu:diva-118598DOI: 10.1116/1.4916239ISI: 000361229000001OAI: oai:DiVA.org:liu-118598DiVA: diva2:815857
Funder
VINNOVA, 2005-02666EU, European Research Council, 227754Knut and Alice Wallenberg Foundation, 2011.0143Swedish Research Council, 2014-5790
Available from: 2015-06-02 Created: 2015-06-02 Last updated: 2017-12-04Bibliographically approved

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Greczynski, GrzegorzPetrov, IvanGreene, Joseph EHultman, Lars

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