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Solid state formation of Ti4AlN3 in cathodic arc deposited (Ti1-xAlx)N-y alloys
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. Saarland University, Germany.
Saarland University, Germany.
Linköping University, Department of Physics, Chemistry and Biology, Nanostructured Materials. Linköping University, Faculty of Science & Engineering. SECO Tools AB, Sweden.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.ORCID iD: 0000-0003-1785-0864
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2017 (English)In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 129, 268-277 p.Article in journal (Refereed) Published
Abstract [en]

Reactive cathodic arc deposition was used to grow substoichiometric solid solution cubic c-(Ti1-xAlx)N-y thin films. The films were removed from the substrate and then heated in an argon environment to 1400 degrees C. Via solid state reactions, formation of MAX phase Ti4AlN3 was obtained. Additional phases such as Ti2AlN, c-TiN, w-AIN, Al5Ti2 and Al3Ti were also present during the solid state reaction. Ti4AlN3 formation was observed in samples with an Al metal fraction x amp;lt; 0.63 and a nitrogen content 0.4 amp;lt; y amp;lt; 0.6. Regardless of the initial composition, formation of Ti4AlN3 started in Ti2AlN crystal plates in the temperature range between 1200 and 1400 degrees C. Accompanying the onset of Ti4AlN3 was the presence of an intermediate structure identified as Ti6Al2N4, consisting of alternating layers of intergrown Ti2AlN and Ti4AlN3 phases with a half-unit-cell stacking. We suggest that the formation of Ti4AlN3 occurred via intercalation of aluminum and nitrogen along the basal plane accompanied by a simultaneous detwinning process. In addition we propose that this formation mechanism can be used to obtain MAX phases of high n order. (C) 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Place, publisher, year, edition, pages
PERGAMON-ELSEVIER SCIENCE LTD , 2017. Vol. 129, 268-277 p.
Keyword [en]
MAX phase; Intergrown phase; Thin films; Solid state reaction; Intercalation
National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:liu:diva-137593DOI: 10.1016/j.actamat.2017.03.001ISI: 000400033900026OAI: oai:DiVA.org:liu-137593DiVA: diva2:1097444
Note

Funding Agencies|European Unions Erasmus Mundus doctoral program DocMASE; Swedish Research Council [621-2012-4401]; Swedish government strategic research area grant AFM SFO MatLiU [2009-00971]; VINNOVA (M - Era.net project MC2) [2013-02355]; European Research Council under the European Communitys Seventh Framework Program (FP) [335383]; DFG; federal state government of Saarland [INST 256/298-1 FUGG, INST 256/431-1 FUGG]; European Regional Development Fund [AME-Lab C/4-EFRE-13/2009/Br]

Available from: 2017-05-22 Created: 2017-05-22 Last updated: 2017-10-23
In thesis
1. 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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