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Influence of sputter damage on the XPS analysis of metastable nanocomposite coatings
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Materials Chemistry, Inorganic Chemistry. (oorganisk kemi)
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Materials Science, Surface and Interface Science.
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2009 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 204, no 4, 455-462 p.Article in journal (Refereed) Published
Abstract [en]

X-ray photoelectron spectroscopy (XPS) is a standard method of determining chemical bonding in e.g. nanocomposites. We demonstrate that sputter-cleaning of the sample prior to analysis can substantially alter the attained information. We present an in-depth analysis of sputter damage on binary and ternary TiC-based coatings in the Ti–Ni–C system. XPS was performed after sputter etching with different ion energies (0.15–4 keV). Results are compared to data from the bulk of undamaged samples attained using high kinetic energy XPS. We observe substantial sputter damage, strongly dependent on sputter energies and coating stability. Metastable samples exhibit severe sputter damage after etching with 4 keV. Additional samples from other Ti–Me–C (Me = Al, Fe, Cu or Pt) systems were also examined, and notable sputter damage was observed. This suggests that accurate analysis of any metastable nanocomposite requires careful consideration of sputter damages.

Place, publisher, year, edition, pages
Elsevier B.V. , 2009. Vol. 204, no 4, 455-462 p.
Keyword [en]
Sputtering, X-ray photoelectron spectroscopy (XPS), Nanocomposite, Metastable phases, Sputtering artifacts
National Category
Chemical Sciences
Research subject
Inorganic Chemistry
URN: urn:nbn:se:uu:diva-109019DOI: 10.1016/j.surfcoat.2009.08.006ISI: 000271337500010OAI: oai:DiVA.org:uu-109019DiVA: diva2:242249
Department of Materials Chemistry, The Ångström Laboratory, Uppsala University, Box 538, SE-751 21 Uppsala, Sweden Department of Physics, The Ångström Laboratory, Uppsala University, Box 530, SE-751 21 Uppsala, Sweden Available from: 2009-10-07 Created: 2009-10-07 Last updated: 2014-05-14
In thesis
1. Design of carbide-based nanocomposite coatings
Open this publication in new window or tab >>Design of carbide-based nanocomposite coatings
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In this thesis research on synthesis, microstructure and properties of carbide-based coatings is reported. These coatings are electrically conducting, and can be tailored for high hardness, low friction and wear, along with load-adaptive behaviour. Tailoring these properties is achieved by controlling the relative phase content of the material. Coatings have been synthesised by dc magnetron sputtering, and their structures have been characterised, mainly by X-ray photoelectron spectroscopy and X-ray diffraction.

It has been shown that nanocomposites comprising of a nanocrystalline transition metal carbide (nc-MeCx, Me = Ti, Nb or V) and an amorphous carbon (a-C) matrix can result in low contact resistance in electrical contacts. Such materials also exhibit low friction and high resistance to wear, making them especially suitable for application in sliding contacts. The lowest contact resistance is attained for small amounts of the amorphous carbon phase.

It has been shown that specific bonding structures are present in the interface between nc-TiCx and the a-C phases in the nanocomposite.  It was found in particular that Ti3d and C2p states are involved, and that considerable charge transfer occurs across the interface, thereby influencing the structure of the carbide.

Further design possibilities were demonstrated for TiCx-based nanocomposites by alloying them with weakly carbide-forming metals, i.e., Me = Ni, Cu or Pt.  Metastable supersaturated solid solution carbides, (T1-xMex)Cy, were identified to result from this alloying process. The destabilisation of the TiCx-phase leads to changes in the phase distribution in the deposited nanocomposites, thus providing further control over the amount of carbon phase formed. Additional design possibilities became available through the decomposition of the metastable (Ti1-xMex)Cy phase through an appropriate choice of annealing conditions, yielding either more carbon phase or a new metallic phase involving Me. This alloying concept was also studied theoretically for all 3d transition metals using DFT techniques.

It has also been demonstrated that Ar-ion etching (commonly used in the analysis of carbide based nanocomposites) can seriously influence the result of the analysis, especially for materials containing metastable phases. This implies that more sophisticated methods, or considerable care are needed in making these analyses, and that many of the earlier published results could well be in error.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2009. 83 p.
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 682
chemistry, thin film, dc magnetron sputtering, carbide, nanocomposite, PVD, solid solution
National Category
Chemical Sciences Inorganic Chemistry
Research subject
Inorganic Chemistry
urn:nbn:se:uu:diva-109427 (URN)978-91-554-7636-6 (ISBN)
Public defence
2009-11-27, Häggsalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 10:15 (English)
Available from: 2009-11-06 Created: 2009-10-15 Last updated: 2014-01-21Bibliographically approved

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