Al capping layers for nondestructive x-ray photoelectron spectroscopy analyses of transition-metal nitride thin films
- Thin Film Physics Division, Department of Physics (IFM), Linköping University, SE-581 83 Linköping (Sweden)
- Thin Film Physics Division, Department of Physics (IFM), Linköping University, SE-581 83 Linköping, Sweden and Materials Science Department and Frederick Seitz Materials Research Laboratory, University of Illinois, Urbana, Illinois 61801 (United States)
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, the authors 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 (1) air-exposed for ≤10 min prior to insertion into the ultrahigh-vacuum (UHV) XPS system; (2) air-exposed and subject to ion etching, using different ion energies and beam incidence angles, in the XPS chamber prior to analysis; or (3) Al-capped in-situ in the deposition system prior to air-exposure and loading into the XPS instrument. The authors show that thin, 1.5–6.0 nm, Al capping layers provide effective barriers to oxidation and contamination of TiN surfaces, thus allowing nondestructive 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.
- OSTI ID:
- 22392204
- Journal Information:
- Journal of Vacuum Science and Technology. A, Vacuum, Surfaces and Films, Vol. 33, Issue 5; Other Information: (c) 2015 American Vacuum Society; Country of input: International Atomic Energy Agency (IAEA); ISSN 0734-2101
- Country of Publication:
- United States
- Language:
- English
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