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Microstructure evolution and age hardening in (Ti,Si)(C,N) thin films deposited by cathodic arc evaporation
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.ORCID iD: 0000-0002-2286-5588
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2010 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 519, no 4, 1397-1403 p.Article in journal (Refereed) Published
Abstract [en]

Ti1 − xSixCyN1 − y films have been deposited by reactive cathodic arc evaporation onto cemented    carbide substrates. The films were characterized by X-ray diffraction, elastic recoil detection analysis, transmission electron microscopy, energy-dispersive X-ray spectroscopy, electron-energy loss spectroscopy and nanoindentation. Reactive arc evaporation in a mixed CH4 and N2 gas gave    films with 0 ≤ x ≤ 0.13 and 0≤y≤0.27. All films had the NaCl-structure with a dense columnar microstructure, containing a featherlike pattern of nanocrystalline grains for high Si and C contents. The film hardness was 32–40GPa. Films with x > 0 and y > 0 exhibited age-hardening up to 35–44 GPa when isothermally annealed up to 900 °C. The temperature threshold for over-ageing was decreased to 700 °C with increasing C and Si content, due to migration of Co, W and Cr from the substrate to the film, and loss of Si. The diffusion pathway was tied to grain boundaries provided by the featherlike substructure.

Place, publisher, year, edition, pages
2010. Vol. 519, no 4, 1397-1403 p.
Keyword [en]
Age hardening, Transmission Electron Microscopy, Thin films, TiSiCN, Arc evaporation, Mechanical properties
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-60522DOI: 10.1016/j.tsf.2010.08.150ISI: 000285125300024OAI: oai:DiVA.org:liu-60522DiVA: diva2:357181
Available from: 2010-10-15 Created: 2010-10-15 Last updated: 2017-12-12Bibliographically approved
In thesis
1. Nanostructuring and Age Hardening in TiSiCN, ZrAlN, and TiAlN Thin Films
Open this publication in new window or tab >>Nanostructuring and Age Hardening in TiSiCN, ZrAlN, and TiAlN Thin Films
2010 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis explores nanostructuring in TiSiCN, ZrAlN, and TiAlN thin films deposited by cathodic arc evaporation onto cemented carbide substrates, with intended applications for cutting tools. The three systems were found to exhibit age hardening upon annealing, by different mechanisms, into the superhard regime (≥30 GPa), as determined by a combination of electron microscopy, X-ray diffraction, atom probe tomography, erda, and nanoindentation tech- niques. TiSiCN forms nanocomposite films during growth by virtue of Si segregation to the surface of TiCN nanocrystallites while simultaneously pro- moting renucleation. Thus, the common columnar microstructure of TiCN and low-Si-content (≤5 at. %) TiSiN-films is replaced by a “feather-like” nanos- tructure in high-Si-content (≥10 at. %) TiSiCN films. The presence of C promotes the formation of this structure, and results in an accelerated age hardening beginning at temperatures as low as 700 °C. The thermal stability of the TiSiCN films is, however, decreased compared to the TiSiN system by the loss of Si and interdiffusion of substrate species; C was found to ex- acerbate these processes, which became active at 900 °C. The ZrAlN system forms a two-phase nanostructure during growth consisting of cubic ZrAlN and wurtzite ZrAlN. Upon annealing to 1100 °C, the c-Zr(Al)N portion of the films recovers and semicoherent brick-like w-(Zr)AlN structures are formed. Age hardening by 36 % was obtained before overageing sets in at 1200 °C. As-deposited and annealed solid solution Ti0.33Al0.67N thin films were characterized for the first time by atom probe tomography. The as-deposited film was found to be at the very initial stage of spinodal decomposition, which continued during annealing of the film at 900 °C for 2 h. N preferentially segregates to Al-rich domains in the annealed sample, causing a compositional variation between Ti-rich and Al-rich domains, to maintain the stoichiometry for the developing AlN phase. That effect also compensates for some of the coherency strain formed between cubic domains of TiN and AlN. Finally, a possible Kirkendall effect caused by an imbalance in the metal interdiffusion during the spinodal decomposition was discovered.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2010. 36 p.
Series
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1442
Keyword
thin films, age hardening, spinodal decomposition, TiSiCN, ZrAlN, TiAlN, Transmission electron microscopy, Atom probe tomography
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-56221 (URN)LIU-TEK-LIC-2010:13 (Local ID)978-91-7393-370-4 (ISBN)LIU-TEK-LIC-2010:13 (Archive number)LIU-TEK-LIC-2010:13 (OAI)
Presentation
(English)
Opponent
Supervisors
Available from: 2010-11-16 Created: 2010-05-02 Last updated: 2016-08-31Bibliographically approved
2. Inside The Miscibility Gap: Nanostructuring and Phase Transformations in Hard Nitride Coatings
Open this publication in new window or tab >>Inside The Miscibility Gap: Nanostructuring and Phase Transformations in Hard Nitride Coatings
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis is concerned with self-organization phenomena in hard and wear resistant transition-metal nitride coatings, both during growth and during post deposition thermal annealing. The uniting physical principle in the studied systems is the immiscibility of their constituent parts, which leads, under certain conditions, to structural variations on the nanoscale. The study of such structures is challenging, and during this work atom probe tomography (apt) was developed as a viable tool for their study. Ti0.33Al0.67N was observed to undergo spinodal decomposition upon annealing to 900 °C, by the use of apt in combination with electron microscopy. The addition of C to TiSiN was found to promote and refine the feather-like microstructure common in the system, with an ensuing decrease in thermal stability. An age-hardening of 36 % was measured in arc evaporated Zr0.44Al0.56N1.20, which was a nanocomposite of cubic, hexagonal, and amorphous phases. Magnetron sputtering of Zr0.64Al0.36N at 900 °C resulted in a self-organized and highly ordered growth of a two-dimensional two-phase labyrinthine structure of cubic ZrN and wurtzite AlN.The structure was analyzed and recovered by apt, although the ZrN phase suffered from severe trajectory aberrations, rendering only the Al signal useable.The initiation of the organized growth was found to occur by local nucleation at 5-8 nm from the substrate, before which random fluctuations in Al/Zr content increased steadily from the substrate. Finally, the decomposition of solid-solution TiB0.33N0.67 was found, by apt, to progress through the nucleation of TiB0.5N0.5 and TiN, followed by the transformation of the former into hexagonal TiB2.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. 69 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1472
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-84263 (URN)978-91-7519-809-5 (ISBN)
Public defence
2012-10-19, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2012-10-03 Created: 2012-10-03 Last updated: 2016-08-31Bibliographically approved

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Johnson, LarsRogström, LinaJohansson, MatsOdén, MagnusHultman, Lars

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