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Layer Formation by Resputtering in Ti-Si-C Hard Coatings during Large Scale Cathodic Arc Deposition
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, Nanostructured Materials. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology. Seco Tools AB, Sweden.
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2011 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 205, no 15, 3923-3930 p.Article in journal (Refereed) Published
Abstract [en]

This paper presents the physical mechanism behind the phenomenon of self-layering in thin films made by industrial scale cathodic arc deposition systems using compound cathodes and rotating substrate fixture. For Ti-Si-C films, electron microscopy and energy dispersive x-ray spectrometry reveals a trapezoid modulation in Si content in the substrate normal direction, with a period of 4 to 23 nm dependent on cathode configuration. This is caused by preferential resputtering of Si by the energetic deposition flux incident at high incidence angles when the substrates are facing away from the cathodes. The Ti-rich sub-layers exhibit TiC grains with size up to 5 nm, while layers with high Si-content are less crystalline. The nanoindentation hardness of the films increases with decreasing layer thickness.

Place, publisher, year, edition, pages
Elsevier , 2011. Vol. 205, no 15, 3923-3930 p.
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-61991DOI: 10.1016/j.surfcoat.2011.02.007ISI: 000289606000004OAI: oai:DiVA.org:liu-61991DiVA: diva2:370950
Note

Original Publication: Anders Eriksson, Jianqiang Zhu, Naureen Ghafoor, Mats Johansson, Jacob Sjölen, Jens Jensen, Magnus Odén, Lars Hultman and Johanna Rosén, Layer Formation by Resputtering in Ti-Si-C Hard Coatings during Large Scale Cathodic Arc Deposition, 2011, Surface & Coatings Technology, (205), 15, 3923-3930. http://dx.doi.org/10.1016/j.surfcoat.2011.02.007 Copyright: Elsevier Science B.V., Amsterdam. http://www.elsevier.com/

Available from: 2010-11-18 Created: 2010-11-18 Last updated: 2017-12-12
In thesis
1. Cathodic Arc Synthesis of Ti-Si-C-N Thin Films from Ternary Cathodes
Open this publication in new window or tab >>Cathodic Arc Synthesis of Ti-Si-C-N Thin Films from Ternary Cathodes
2010 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

Cathodic arc deposition is a powerful technique for thin film synthesis, associated with explosive phase transformations resulting in an energetic and highly ionized plasma. This Thesis presents film growth through arc deposition from compound cathodes of Ti3SiC2, providing source material for plasma and films rich in Si and C. The interest for the resulting Ti-Si-C-N films is inspired by the two ternaries Ti-Si-N and Ti-C-N, both successfully applied as corrosion  and wear resistant films, with a potential for synergistic effects in the quarternary system.

When using a rotating substrate fixture setup, which is common in high capacity commercial deposition systems, the repeated passage though the plasma zone results in growth layers in the films. This effect has been observed in several coating systems, in deposition of various materials, but has not been explained in detail. The here investigated layers are characterized by a compositional modulation in Si and Ti content, which is attributed primarily to preferential resputtering in segments of rotation when the plasma has high incidence angle towards the substrate normal. For depositions in a non-reactive environment, the films consist of primarily understoichiometric TiCx, Ti, and silicide phases, and display a modest hardness (20-30 GPa) slightly improved by a decreasing layer thickness. Hence, the side effects of artificial layering from substrate rotation in deposition systems should be recognized.

Adding N2 to the deposition process results in reactive growth of nitride material, formed in a wide range of compositions, and thereby enabling investigation of films in little explored parts of the Ti-Si-C-N system. The structure and properties of such films, comprising up to 12 at% Si and 16 at% C, is highly dependent on the supply of N2 during deposition. Superhard (45-50 GPa) cubic-phase (Ti,Si)(C,N) films with a nanocrystalline feathered structure is formed at N-content of 25-30 at%. At higher N2 deposition pressure, C and Si segregate to column and grain boundaries and the cubic phase assumes a more pronounced nitride character. This transformation is accompanied by substantially reduced film hardness to 20 GPa. Ti-Si-C-N films thus display a rich variety of structures with favorable mechanical properties, but in the regime of high Si and C content, the amount of N must be carefully controlled to avoid undesirable formation of weak grain boundary phases based on Si, C and N.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2010. 37 p.
Series
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1456
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-61994 (URN)LIU-TEK-LIC-2010:27 (Local ID)978-91-7393-273-8 (ISBN)LIU-TEK-LIC-2010:27 (Archive number)LIU-TEK-LIC-2010:27 (OAI)
Presentation
2010-12-09, Planck, Fysikhuset, Campus Valla, Linköping University, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2010-12-01 Created: 2010-11-18 Last updated: 2010-12-01Bibliographically approved
2. Cathodic Arc Synthesis of Ti-Si-C-N Thin Films: Plasma Analysis and Microstructure Formation
Open this publication in new window or tab >>Cathodic Arc Synthesis of Ti-Si-C-N Thin Films: Plasma Analysis and Microstructure Formation
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This Thesis explores the arc deposition process and films of Ti-Si-C-N, inspired by the two ternary systems Ti-Si-N and Ti-C-N, both successfully applied as corrosion and wear resistant films. The correlation between cathode, plasma, and film properties are studied for a comprehensive view on film formation. Novel approaches to adapt arc deposition to form multi-element films are investigated, concluding that the source of C is not a determining factor for film growth. Thus, cubic-phase films of similar properties can be synthesized from processes with either 1) ternary Ti-Si-C cathodes, including the Ti3SiC2 MAX phase, in N2 atmosphere or 2) Ti-Si cathodes in a mixture of N2 and CH4. With the Ti3SiC2 cathodes, superhard (45-50 GPa) cubic-phase (Ti,Si)(C,N) films can be deposited. The structure is nanocrystalline and feather-like, with high Si and C content of 12 and 16 at%, respectively. To isolate the effects of Si on film structure, magnetron sputtered Ti-Si-N films of comparatively low defect density was studied. These films show a strong preference for {200}  growth orientation, and can be grown as a single phase solid solution on MgO(001) substrates up to ~9 at% Si, i.e. considerably higher than the ~5 at% Si above which a feather-like nanocrystalline structure forms in arc deposited films. On (011) and (111) growth surfaces, the films self-organize into TiN columns separated by segregated crystalline-to-amorphous SiNx. The conditions for film growth by arc were investigated through plasma studies, showing that plasma properties are dependent on cathode composition as well as phase structure. Plasma generation from Ti-Si cathodes, with up to 25 at% Si, show higher average ion charge states of Ti and Si compared to plasma from elemental cathodes, which may be related to TiSix phases of higher cohesive energies. The ion energy distributions range up to 200 eV. Furthermore, compositional discrepancies between plasma ions and film infer significant contributions to film growth from Si rich neutral species. This is further supported by depositions with a macroparticle filter, intended for growth of films with low surface roughness, where Si and C contents lower than the stoichiometry of Ti3SiC2 cathodes was measured in both plasma and films. Also the substrate geometry is critical for the film composition in plasma based film deposition, as evidenced by the formation of artificial layering from rotating substrate fixtures common in high capacity arc deposition systems. The layers are characterized by modulations in composition and crystallinity, primarily attributed to preferential resputtering in high ion incidence angle segments repeated through rotation.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2013. 55 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1495
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-86259 (URN)978-91-7519-714-2 (ISBN)
Public defence
2013-01-14, Visionen, B-huset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2012-12-12 Created: 2012-12-12 Last updated: 2016-08-31Bibliographically approved

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Eriksson, AndersZhu, JianqiangGhafoor, NaureenJohansson, MatsJensen, JensOdén, MagnusHultman, LarsRosén, Johanna

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