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High temperature behavior of arc evaporated ZrAlN and TiAlN thin films
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Hard coatings can extend the life time of a tool substantially and enable higher cutting speeds which increase the productivity in the cutting application. The aim with this thesis is to extend the understanding on how the microstructure and mechanical properties are affected by high temperatures similar to what a cutting tool can reach during operation.

Thin films of ZrAlN and TiAlN have been deposited using cathodic arc-evaporation. The microstructure of as-deposited and annealed films has been studied using electron microscopy and x-ray scattering. The thermal stability has been characterized by calorimetry and thermogravity and the mechanical properties have been investigated by  nanoindentation.

The microstructure of Zr1−xAlxN thin films was studied as a function of composition, deposition conditions, and annealing temperature. The structure was found to depend on the Al content where a low (x < 0.38) Al-content results in cubic-structured ZrAlN while for x > 0.70 the structure is hexagonal. For intermediate Al contents (0.38 < x < 0.70), a  nanocomposite structure with a mixture of cubic, hexagonal and amorphous phases is obtained.

The cubic ZrAlN phase transforms by nucleation and growth of hexagonal AlN when annealed above 900 C. Annealing of hexagonal ZrAlN thin films (x > 0.70) above 900 C causes formation of AlN and ZrN rich domains within the hexagonal lattice. Annealing of nanocomposite ZrAlN thin films results in formation of cubic ZrN and hexagonal AlN. The transformation is initiated by nucleation and growth of cubic ZrN at temperatures of 1100 C while the AlN-rich domains are still amorphous or nanocrystalline. Growth of hexagonal AlN is suppressed by the high nitrogen content of the films and takes place at annealing temperatures of 1400 C.

In the more well known TiAlN system, the initial stage of decomposition is spinodal with formation of cubic structured domains enriched in TiN and AlN. By a combination of in-situ xray scattering techniques during annealing and phase field simulations, both the microstructure that evolves during decomposition and the decomposition rate are found to depend on the composition. The results further show that early formation of hexagonal AlN domains during decomposition can cause formation of strains in the cubic TiAlN phase.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. , 78 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1428
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-75176ISBN: 978-91-7519-956-6 (print)OAI: oai:DiVA.org:liu-75176DiVA: diva2:504322
Public defence
2012-03-22, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2012-02-20 Created: 2012-02-20 Last updated: 2016-08-31Bibliographically approved
List of papers
1. 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: 2016-08-31Bibliographically approved
2. Thermal stability and mechanical properties of arc evaporated ZrN/ZrAlN multilayers
Open this publication in new window or tab >>Thermal stability and mechanical properties of arc evaporated ZrN/ZrAlN multilayers
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2010 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 519, no 2, 694-699 p.Article in journal (Refereed) Published
Abstract [en]

ZrN1.20/Zr0.44Al0.56N1.20 multilayer films as well as ZrN1.17 and Zr0.44Al0.56N1.20 films were deposited by reactive arc evaporation on WC–Co substrates. Samples were post-deposition annealed for 2 h at 800–1200 °C. As-deposited and heat treated films were characterized by scanning transmission electron microscopy, X-ray diffraction and nanoindentation. The thermal stability was studied using a combination of differential scanning calorimetry, thermogravimetry, and mass spectrometry. The as-deposited Zr0.44Al0.56N1.20 film exhibits a nanocomposite structure of cubic and wurtzite ZrAlN. During annealing, the formation of ZrN- and AlN-rich domains results in age hardening of both the Zr0.44Al0.56N1.20 and the ZrN/ZrAlN multilayers. The age hardening is enhanced in the ZrN/ZrAlN multilayer due to straining of the ZrAlN sublayers in which a maximum hardness of 31 GPa is obtained after annealing at 1100 °C.

Place, publisher, year, edition, pages
Elsevier, 2010
Keyword
Thin films; Zr-Al-N; Multilayer; Arc evaporation; TEM; Hardness
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-62984 (URN)10.1016/j.tsf.2010.08.119 (DOI)000284499500025 ()
Available from: 2010-12-08 Created: 2010-12-08 Last updated: 2016-08-31
3. Phase transformations in nanocomposite ZrAlN thin films during annealing
Open this publication in new window or tab >>Phase transformations in nanocomposite ZrAlN thin films during annealing
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2012 (English)In: Journal of Materials Research, ISSN 0884-2914, E-ISSN 2044-5326, Vol. 27, no 13, 1716-1724 p.Article in journal (Refereed) Published
Abstract [en]

Nanocomposite Zr0.52Al0.48N1.11 thin films consisting of crystalline grains surrounded by an amorphous matrix were deposited using cathodic arc evaporation. The structure evolution after annealing of the films was studied using high-energy x-ray scattering and transmission electron microscopy. The mechanical properties were characterized by nanoindentation on as-deposited and annealed films. After annealing in temperatures of 1050-1400 C nucleation and grain growth of cubic ZrN takes place in the film. This increases the hardness, which reaches a maximum while parts of the film remain amorphous. Grain growth of the hexagonal AlN phase occurs above 1400 C.

Place, publisher, year, edition, pages
Cambridge University Press, 2012
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-75171 (URN)10.1557/jmr.2012.122 (DOI)000307187900007 ()
Note

funding agencies|Swedish Research Council (VR)||VINNEX center of Excellence on Functional Nanoscale Materials (FunMat)||U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences|DE-AC02-06CH11357|Linnaeus Grants||

Available from: 2012-02-20 Created: 2012-02-20 Last updated: 2017-12-07Bibliographically approved
4. Influence of chemical composition and deposition conditions on microstructure evolution during annealing of arc evaporated ZrAlN thin films
Open this publication in new window or tab >>Influence of chemical composition and deposition conditions on microstructure evolution during annealing of arc evaporated ZrAlN thin films
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2012 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 30, no 3, 031504- p.Article in journal (Refereed) Published
Abstract [en]

The influence of substrate bias and chemical composition on the microstructure and hardness of arc evaporated Zr1−xAlxN films with 0.12 < x < 0.74 is investigated. A cubic ZrAlN phase is formed at low aluminum contents (x < 0.38) whereas for a high Al-content, above x=0.70, a single-phase hexagonal structure is obtained. For intermediate Al-contents, a two-phase structure is formed. The cubic structured films exhibit higher hardness than the hexagonal structured ones. A low bias results in N-rich films with a partly defect-rich microstructure while a higher substrate bias decreases the grain size and increases the residual stress in the cubic ZrAlN films. Recrystallization and out-diffusion of nitrogen from the lattice in the cubic ZrAlN films takes place during annealing at 800 C, which results in an increased hardness. The cubic ZrAlN phase is stable to annealing temperatures of 1000 C while annealing at higher temperature results in nucleation and growth of hexagonal AlN. In the high Al-content ZrAlN films, formation of ZrN- and AlN-rich domains within the hexagonal lattice during annealing at 1000 C improves the mechanical properties.

Place, publisher, year, edition, pages
American Vacuum Society, 2012
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-75172 (URN)10.1116/1.3698592 (DOI)000303602800015 ()
Note

funding agencies|VINN Excellence Center on Functional Nanoscale Materials (FunMat)||

Available from: 2012-02-20 Created: 2012-02-20 Last updated: 2017-12-07Bibliographically approved
5. Auto-organizing ZrAlN/ZrAlTiN/TiN multilayers
Open this publication in new window or tab >>Auto-organizing ZrAlN/ZrAlTiN/TiN multilayers
2012 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 520, no 21, 6451-6454 p.Article in journal (Refereed) Published
Abstract [en]

The structural evolution during annealing of arc evaporated ZrAlN/ZrN andZrAlN/TiN multilayers is studied. On annealing, ZrN- and AlN-rich domains form within the ZrAlN sublayers. In the ZrAlN/TiN film, interdiffusion at the ZrAlN/TiN interfaces cause formation of a new cubic Zr(Al,Ti)N phase when annealed at temperatures above 900 C. The formation of this metastable phase results in a substantial increase in hardness of the film, which is retained to annealing temperatures of 1100 C. In the ZrAlN/ZrN film no secondary phases are formed and for annealing at temperatures above 800 C grain growth of the ZrN grains results in decreased hardness.

Place, publisher, year, edition, pages
Elsevier, 2012
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-75173 (URN)10.1016/j.tsf.2012.06.052 (DOI)000307286100001 ()
Note

funding agencies|VINN Excellence Center on Functional Nanoscale Materials (FunMat)||

Available from: 2012-02-20 Created: 2012-02-20 Last updated: 2017-12-07Bibliographically approved
6. Strain evolution during spinodal decomposition of TiAlN thin films
Open this publication in new window or tab >>Strain evolution during spinodal decomposition of TiAlN thin films
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2012 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 520, no 17, 5542-5549 p.Article in journal (Refereed) Published
Abstract [en]

We use a combination of in-situ x-ray scattering experiments during annealing and phase-field simulations to study the strain and microstructure evolution during decomposition of TiAlN thin films. The evolved microstructure is observed to depend on composition, where the larger elastic anisotropy of higher Al content films causes formation of elongated AlN and TiN domains. The simulations show strain formation in the evolving cubic-AlN and TiN domains, which is a combined effect of increasing lattice mismatch and elastic incompatibility between the domains. The experimental results show an increased compressive strain in the TiAlN phase during decomposition due to the onset of transformation to hexagonal-AlN.

Place, publisher, year, edition, pages
Elsevier, 2012
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-75174 (URN)10.1016/j.tsf.2012.04.059 (DOI)000305770200010 ()
Available from: 2012-02-20 Created: 2012-02-20 Last updated: 2017-12-07Bibliographically approved
7. Microstructure evolution during annealing of TiAlN-coatings: A combined in-situ SAXS and phase field study
Open this publication in new window or tab >>Microstructure evolution during annealing of TiAlN-coatings: A combined in-situ SAXS and phase field study
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2011 (English)Manuscript (preprint) (Other academic)
Abstract [en]

This paper describes in detail the microstructure evolution of Ti0.33Al0.67N and Ti0.50Al0.50N coatings during isothermal annealing studied by in-situ small angle x-ray scattering (SAXS) in combination with phase field simulations. We show that the decomposition occurs in two stages consistent with spinodal decomposition. During the initial stage, the phase segregation proceeds with a constant size of AlN- and TiN-rich domains with a radius of ~0.7 nm for 5 and 20 min at 900 and 850 C respectively in the Ti0.50Al0.50N alloy. The length of the initial stage depends on the temperature as well as the composition, and is shorter for the higher Al content coating. Following the initial stage, the AlN- and TiN-rich domains coarsen. The decomposition process is discussed in terms of Gibbs free energy, diffusion, and gradient energies. Scanning transmission electron microscopy and energy dispersive x-ray spectroscopy of the post annealed coatings confirm a decomposed microstructure with coherent domains rich in AlN and TiN of the same size as determined by SAXS.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-75175 (URN)
Available from: 2012-02-20 Created: 2012-02-20 Last updated: 2013-10-02Bibliographically approved

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