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Nanostructuring and Age Hardening in TiSiCN, ZrAlN, and TiAlN Thin Films
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology. (Thin Film Physics Division)
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 [en]
thin films, age hardening, spinodal decomposition, TiSiCN, ZrAlN, TiAlN, Transmission electron microscopy, Atom probe tomography
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-56221Local ID: LIU-TEK-LIC-2010:13ISBN: 978-91-7393-370-4 (print)OAI: oai:DiVA.org:liu-56221DiVA: diva2:357194
Presentation
(English)
Opponent
Supervisors
Available from: 2010-11-16 Created: 2010-05-02 Last updated: 2016-08-31Bibliographically approved
List of papers
1. Microstructure evolution and age hardening in (Ti,Si)(C,N) thin films deposited by cathodic arc evaporation
Open this publication in new window or tab >>Microstructure evolution and age hardening in (Ti,Si)(C,N) thin films deposited by cathodic arc evaporation
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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.

Keyword
Age hardening, Transmission Electron Microscopy, Thin films, TiSiCN, Arc evaporation, Mechanical properties
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-60522 (URN)10.1016/j.tsf.2010.08.150 (DOI)000285125300024 ()
Available from: 2010-10-15 Created: 2010-10-15 Last updated: 2017-12-12Bibliographically approved
2. Age hardening in arc-evaporated ZrAlN thin films
Open this publication in new window or tab >>Age hardening in arc-evaporated ZrAlN thin films
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2010 (English)In: Scripta Materialia, ISSN 1359-6462, E-ISSN 1872-8456, Vol. 62, no 10, 739-741 p.Article in journal (Refereed) Published
Abstract [en]

Zr0.44Al0.56N1.20 films were deposited by reactive arc evaporation on WC-Co substrates. As-deposited films have a defect-rich NaCl-cubic and wurtzite phase mixture. During annealing at 1100 degrees C the films undergo simultaneous recovery of the ZrN-rich c-ZrAlN nanoscale domains and formation of semicoherent w-ZrAlN nanobricks, while the excess nitrogen is released. This process results in an age hardening effect as high as 36%, as determined by nanoindentation. At 1200 degrees C, the w-AlN recrystallizes and the hardening effect is lost.

Place, publisher, year, edition, pages
Amsterdam: Elsevier Science B.V., 2010
Keyword
PVD, Nanoindentation, TEM, Hardness, Thin films
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-54847 (URN)10.1016/j.scriptamat.2010.01.049 (DOI)000276295800004 ()
Available from: 2010-04-16 Created: 2010-04-16 Last updated: 2017-12-12Bibliographically approved
3. Spinodal Decomposition of Ti0.33Al0.67N Thin Films Studied by Atom Probe Tomography
Open this publication in new window or tab >>Spinodal Decomposition of Ti0.33Al0.67N Thin Films Studied by Atom Probe Tomography
(English)Manuscript (preprint) (Other academic)
Abstract [en]

The decomposition of Ti0.33Al0.67N thin films deposited by cathodic arc evaporation have been studied by atom probe tomography.  As-deposited films were found to deviate slightly from a random solid solution, and so be in the earliest stage of decomposition. After annealing at 900 °C for 2 h the films exhibited a spinodally decomposed nanostructure, in an intermediate stage. N was found to preferentially segregate to the Al-rich domains in the annealed sample, causing the TiN-domains to be understoichiometric.  A possible Kirkendall effect was detected for the annealed sample, with a modulation of the local stoichiometry by 1-2 at. % along the decomposition gradient.

Keyword
thin films, TiAlN, cathodic arc evaporation, atom probe tomography, spinodal decomposition
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-60524 (URN)
Available from: 2010-10-15 Created: 2010-10-15 Last updated: 2010-11-16

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