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Characterization of amorphous and nanocomposite Nb–Si–C thin films deposited by DC magnetron sputtering
Uppsala University, Sweden.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.ORCID iD: 0000-0003-1785-0864
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2013 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 545, 272-278 p.Article in journal (Refereed) Published
Abstract [en]

Two series of Nb–Si–C thin films of different composition have been deposited using DC magnetron sputtering. In the first series the carbon content was kept at about 55 at.% while the Si/Nb ratio was varied and in the second series the C/Nb ratio was varied instead while the Si content was kept at about 45 at.%. The microstructure is strongly dependent on Si content and Nb–Si–C films containing more than 25 at.% Si exhibit an amorphous structure as determined by X-ray diffraction. Transmission electron microscopy, however, induces crystallisation during analysis, thus obstructing a more detailed analysis of the amorphous structure. X-ray photo-electron spectroscopy suggests that the amorphous films consist of a mixture of chemical bonds such as Nb–Si, Nb–C, and Si–C. The addition of Si results in a hardness decrease from 22 GPa for the binary Nb–C film to 18 – 19 GPa for the Si-containing films, while film resistivity increases from 211 μΩcm to 3215 μΩcm. Comparison with recently published results on DC magnetron sputtered Zr–Si–C films, deposited in the same system using the same Ar-plasma pressure, bias, and a slightly lower substrate temperature (300 °C instead of 350 °C), shows that hardness is primarily dependent on the amount of Si–C bonds rather than type of transition metal. The reduced elastic modulus on the other hand shows a dependency on the type of transition metal for the films. These trends for the mechanical properties suggest that high wear resistant (high H/E and H3/E2 ratio) Me–Si–C films can be achieved by appropriate choice of film composition and transition metal.

Place, publisher, year, edition, pages
Elsevier , 2013. Vol. 545, 272-278 p.
Keyword [en]
Magnetron sputtering, Carbide, Amorphous structure, Structure characterization, Mechanical properties, Electrical properties
National Category
Engineering and Technology
URN: urn:nbn:se:liu:diva-100023DOI: 10.1016/j.tsf.2013.08.066ISI: 000324820800045OAI: diva2:659447

Funding Agencies|Vinnova (Swedish Governmental Agency for Innovation Systems) through the VINN Excellence Centre FunMat||Swedish Research Council (VR)||

Available from: 2013-10-25 Created: 2013-10-25 Last updated: 2016-08-31
In thesis
1. Transition metal carbide nanocomposite and amorphous thin films
Open this publication in new window or tab >>Transition metal carbide nanocomposite and amorphous thin films
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis explores thin films of binary and ternary transition metal carbides, in the Nb-C, Ti-Si-C, Nb-Si-C, Zr-Si-C, and Nb-Ge-C systems. The electrical and mechanical properties of these systems are affected by their structure and here both nanocomposite and amorphous thin films are thus investigated. By appropriate choice of transition metal and composition the films can be designed to be multifunctional with a combination of properties, such as low electric resistivity, low contact resistance and high mechanical strength. Electrical contacts are one example of application that has been of special interest in this thesis. Since some industrially important substrates used in electrical contacts soften at higher temperature, all films were deposited with dc magnetron sputtering at a low substrate temperature (200-350 °C).

I show that the electrical resistivity and mechanical properties of composites consisting of nanocrystalline NbC grains (nc-NbC) in a matrix of amorphous C (a-C) depend strongly on the amount of amorphous C. The best combination of hardness (23 GPa) and electrical resistivity (260 μΩ*cm) are found in films with ~15 at.% a-C phase. This is a higher hardness and lower resistivity than measured for the more well studied Ti-C system if deposited under similar conditions. The better results can be explained by a thinner matrix of amorphous C phase in the case of NbC. The nc-NbC/a-C is therefore interesting as a material in electrical contacts.

Si can be added to further control the structure and thereby the properties of binary Me-C systems. There are however, different opinions in the literature of whether Si is incorporated on the Ti or C site in the cubic NaCl (B1) structure of TiC. In order to understand how Si is incorporated in a Me-Si-C material I use a model system of epitaxial TiCx (x ~0.7). In this model system a few atomic percent of Si can be incorporated in the cubic TiC structure. The experimental results together with theoretical stability calculations suggest that the Si is positioned at the C sites forming Ti(Si,C)x. The calculation further shows a strong tendency for Si segregation, which is seen at higher Si contents in the experiments, where Si starts segregate out from the TiCx to the grain boundaries causing a loss of epitaxy.

If Si is added to an Nb-C nanocomposite, it hinders the grain growth and thus a reduced size of the NbC grains is observed. The Si segregates to the amorphous matrix forming a-SiC. At the same time the resistivity increases and the hardness is reduced. With even higher amounts of Si (>25 at.%) into the Nb-Si-C material, grain growth is no longer possible and the material becomes amorphous. In order to separate between effects from the addition of Si and the choice of transition metal I compare the Nb-Si-C system to already published results for the Zr-Si-C system. I find that the hardness of the material depends on the amount of strong Si-C bonds rather than the type of transition metal. The reduced elastic modulus is, however, dependent on the choice of transition metal. I therefore suggest that it is possible to make Me-Si-C films with high wear resistance by an appropriate choice of transition metal and composition.

Electron microscopy was of importance for determining amorphous structures of Nb-Si-C and Zr-Si-C at high Si contents. However, the investigations were obstructed by electron beam induced crystallization. Further investigations show that the energy transferred from the beam electrons to C and Si atoms in the material is enough to cause atomic displacements. The displacements cause volume fluctuations and thereby enhance the mobility of all the atoms in the material. The result is formation of MeC grains, which are stable to further irradiation.

Finally, I have studied substitution of Ge for Si in a ternary system looking at Nb-Ge-C thin films. I show that the films consist of nc-NbC/a-C/a-Ge and that Ge in a similar way to Si decreases the size of the crystalline NbC grains. However, a transition to a completely amorphous material is not seen even at high Ge contents (~30 at.%). Another dissimilarity is that while Si bonds to C and forms a matrix of a-SiC, Ge tends to bond to Ge.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2014. 50 p.
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1576
National Category
Natural Sciences
urn:nbn:se:liu:diva-104929 (URN)10.3384/diss.diva-104929 (DOI)978-91-7519-398-4 (print) (ISBN)
Public defence
2014-03-28, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Available from: 2014-03-03 Created: 2014-03-03 Last updated: 2016-08-31Bibliographically approved

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