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Surface directed spinodal decomposition at TiAlN / TiN interfaces
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, The Institute of Technology.
Functional Materials, Department Materials Science, Saarland University, Saarbrücken, Germany.
Linköping University, Department of Physics, Chemistry and Biology. Linköping University, The Institute of Technology.
Functional Materials, Department Materials Science, Saarland University, Saarbrücken, Germany.
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2013 (English)In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 113, no 11, 114305-1-114305-8 p.Article in journal (Refereed) Published
Abstract [en]

In contrast to the monolithic c-Ti1-xAlxN, the isostructural spinodal decomposition to c-AlN and c-TiN of the c-Ti1-xAlxN/TiN multilayers have the same onset temperature regardless of composition (x=0.50 and 0.66). The onset is also located at a lower temperature compared to the monoliths with the same Al-content, revealed by differential scanning calorimetry. Zcontrast STEM imaging shows a decomposed structure of the multilayers at a temperature where it is not present in the monoliths. Atom probe tomography reveal the formation of an AlN-rich layer followed by a TiN-rich area parallel to the interface in the decomposed Ti0.34Al0.66N/TiN coating, consistent with surface directed spinodal decomposition. Phase field simulations predict such behavior and show that the surface directed spinodal decomposition is affected by in the internal interfaces, as deposited elemental fluctuations, coherency stresses and alloy composition.

Place, publisher, year, edition, pages
American Institute of Physics (AIP), 2013. Vol. 113, no 11, 114305-1-114305-8 p.
Keyword [en]
Surface directed spinodal decomposition, Titanium aluminium nitride, Phase field simulations, Atom probe tomography
National Category
Physical Sciences
Identifiers
URN: urn:nbn:se:liu:diva-84704DOI: 10.1063/1.4795155ISI: 000316545200054OAI: oai:DiVA.org:liu-84704DiVA: diva2:561227
Available from: 2012-10-17 Created: 2012-10-17 Last updated: 2017-11-07Bibliographically approved
In thesis
1. Thermal stability and mechanical properties of TiAlN-based multilayer and monolithic coatings
Open this publication in new window or tab >>Thermal stability and mechanical properties of TiAlN-based multilayer and monolithic coatings
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis explores the thermal stability, microstructure, mechanical properties and cutting performance of multilayer and monolithic cubic TiAlN hard coatings. The aim is to increase the understanding of how the coatings’ microstructure and properties are affected by a layered structure when exposed to high temperatures.

The coatings were deposited on cemented carbide substrates, using a full scale industrial reactive cathodic arc evaporation system at Seco Tools AB. The thermal stability was investigated by differential scanning calorimetry and the microstructure was characterized with analytical transmission electron microscopy, x-ray diffractometry and atom probe tomography. The mechanical properties and cutting performance were studied by nanoindentation and metal machining, respectively.

The decomposition of cubic TiAlN transpire in two steps, first by an isostructural decomposition to cubic AlN- and cubic TiN-rich domains, which is followed by a phase transformation of cubic AlN to hexagonal AlN. In this work I show that the isostructural decomposition occurs in two stages, namely: Spinodal decomposition (initial stage) and coarsening (latter stage). During the initial stage, the phase separation proceeds with a constant size of the AlN- and TiN-rich domains, with a measured wavelength of ~2.8 nm. The time needed for the initial stage depends on the temperature as well as the composition. Following the spinodal decomposition, the AlN- and TiN-rich domains coarsen. The coarsening process is kinetically limited by diffusion and is not dependent on the composition.

If the cubic TiAlN is grown as a multilayer coating, with TiN as the alternating layer type, the decomposition behavior will be different. The isostructural spinodal decomposition in the multilayers starts at a lower temperature compared to the monolithic TiAlN, while the subsequent transformation from cubic AlN to hexagonal AlN is delayed to higher temperatures. The TiN-layers confine the coarsening of the hexagonal AlN resulting in smaller domains. Mechanical testing reveals that, despite the 60 vol. % of the softer TiN, the asdeposited multilayers show a similar or slightly higher hardness than the monolithic Ti0.34Al0.66N. In addition, the multilayers show a more pronounced age hardening compared to the monoliths.

For short annealing times (<1 min) at 850 °C a layer rich in AlN followed by areas rich in TiN is observed parallel to the TiAlN/TiN interfaces in the multilayer stack. This microstructural feature indicates the presence of surface directed spinodal decomposition in the multilayer coatings. The lack of a layered structure further into the TiAlN-layer is due to the growth induced elemental fluctuations, which trigger an earlier onset of the coarsening. The coherency stresses generated across the multilayer interfaces also influence the decomposition. However, in this case the surface directed spinodal decomposition is the dominating mechanism for the altered thermal stability.

Finally, during metal machining of AISI-316L stainless steel the Ti0.34Al0.66N/TiN multilayers, regardless of period, show an improved crater wear resistance compared to a Ti0.34Al0.66N monolith. The multilayer  structure and the local coherency across the multilayer interfaces, seen in the as-deposited state, is present also after the metal machining. It is further revealed that the Ti0.34Al0.66N layer decomposes to AlN- and TiN-rich domains during the cutting operation.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. 76 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1474
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-84705 (URN)978-91-7519-801-9 (ISBN)
Public defence
2012-11-16, Planck, Fysikhuset, Campus Valla, Linköpings univeristet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2012-10-17 Created: 2012-10-17 Last updated: 2013-10-02Bibliographically approved
2. Defect-engineered (Ti,Al)N thin films
Open this publication in new window or tab >>Defect-engineered (Ti,Al)N thin films
2017 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis investigates the effect of point defects (nitrogen vacancies and interstitials) and multilayering ((Ti,Al)N/TiN) on the phase transformations in cathodic arc-evaporated cubic (Ti,Al)N thin films at elevated temperatures. Special attention is paid to the evolution of the beneficial spinodal decomposition into c-TiN and c-AlN, the detrimental formation of wurtzite AlN and the potential application as hard coating in cutting tools.

c-(Ti1-xAlx)Ny thin films with varying Al fractions and N content (y = 0.93 to 0.75) show a delay in the spinodal decomposition when increasing the amount of N vacancies. This results in a 300 °C upshift in the age hardening and a delay in the w-AlN formation, while additions of self-interstitials enhance phase separation. High temperature interaction between hard metal substrates and thin films is more pronounced when increasing N deficiency through diffusion of substrate elements into the film. Low N content films (y = 0.58 to 0.40) showed formation of additional phases such as Ti4AlN3, Ti2AlN, Al5Ti2 and Al3Ti during annealing and a transformation from Ti2AlN to Ti4AlN3 via intercalation. The multilayer structure of TiN/TiAlN results in surfacedirected spinodal decomposition that affects the decomposition behavior. Careful use of these effects appears as a promising method to improve cutting tool performance.

Abstract [de]

Diese Arbeit untersucht den Effekt von Punktdefekten (Stickstoffleerstellen und Zwischengitteratome) und Multilagen ((Ti,Al)N/TiN) auf die Phasenumwandlung in lichtbogenverdampften kubischen (Ti,Al)N-Dünnschichten bei erhöhten Temperaturen. Besonderes Augenmerk liegt auf der Entwicklung der vorteilhaften spinodalen Entmischung in c-TiN und c-AlN und der nachteiligen Bildung von Wurtzit-AlN, sowie der möglichen Anwendung als Hartstoffbeschichtung von Schneidwerkzeugen.

c-(Ti1-xAlx)Ny mit unterschiedlichem Al-Anteil und N-Gehalten von y = 0,93 bis 0,75 zeigt mit zunehmenden Stickstoffleerstellen eine Verzögerung der spinodalen Entmischung. Dadurch verschiebt sich die Ausscheidungshärtung um 300 °C zu höheren Temperaturen und die w-AlN-Bildung wird verzögert, während der Einbau von Eigenzwischengitteratomen die Entmischung beschleunigt. Die Hochtemperaturwechselwirkung zwischen Hartmetallsubstrat und Dünnschicht durch Diffusion von Substratelementen in die Schicht nimmt mit steigendem Stickstoffdefizit zu. Stickstoffarme Schichten (y = 0,58 bis 0,40) zeigen während der Wärmebehandlung zusätzliche Phasen wie Ti4AlN3, Ti2AlN, Al5Ti2 und Al3Ti und eine Umwandlung von Ti2AlN in Ti4AlN3 durch Interkalation. Die Multischichtstruktur von TiN/TiAlN führt zu einer oberflächengerichteten spinodalen Entmischung, die das Entmischungsverhalten beeinflusst. Ein gezielter Einsatz dieser Effekte erscheint als ein vielsprechender Weg, um die Leistungsfähigkeit von Schneidwerkzeugen zu verbessern.

Abstract [sv]

I denna avhandling behandlas inverkan av punktdefekter (kvävevakanser och interstitialer) och multilagring ((Ti,Al)N/TiN) på högtemperaturfasomvandlingar i tunna arcförångade skikt av kubiska (Ti,Al)N. Störst vikt har lagts på utvecklingen av det fördelaktiga spinodala sönderfallet till c-TiN och c-AlN, den ofördelaktiga omvandlingen till w-AlN och potentialen som hårda skikt i verktygstillämpningar.

Tunna c-(Ti1-xAlx)Ny skikt med olika Al-andel och en N-halt mellan (y = 0.93 och 0.75) uppvisar ökad undertryckning av det spinodala sönderfallet med ökat kvävevakanshalt. Detta resulterar i bildandet av w-AlN skiftas upp i temperatur vilket gör att åldershärdningen höjs med 300 °C. Däremot medför närvaron av självinterstitialer ett snabbare sönderfall. Växelverkan mellan hårdmetallsubstraten och de tunna skikten vid hög temperatur ökar med minskad kvävehalt i skiten genom diffusion av atomer från substratet in i filmen. Filmer med låg kvävehalt (y = 0.58 till 0.40) bildar även andra faser så som Ti4AlN3, Ti2AlN, Al5Ti2 och Al3Ti under värmebehandling och fasomvandlingen från Ti2AlN till Ti4AlN3 sker via en mekanism kallad intercalation. Multilagring av TiN/TiAlN resulterar i ett ytriktad spinodalt sönderfall vilket påverkar det totala sönderfallsförloppet. Nyttjande av dessa resultat syns som lovande vägar till förbättrade verktygsegenskaper.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2017. 73 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1878
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-142116 (URN)10.3384/diss.diva-142116 (DOI)9789176854563 (ISBN)
Public defence
2017-11-14, House D3 3, Saarland University, DE-66123 Saarbrücken, Germany, Saarbrücken, 14:15 (English)
Opponent
Supervisors
Available from: 2017-10-23 Created: 2017-10-23 Last updated: 2017-10-23Bibliographically approved

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Knutsson, AxelAsp Grönhagen, KlaraOdén, Magnus

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