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Growth of Hard Amorphous Ti-Al-Si-N Thin Films by Cathodic Arc Evaporation
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Seco Tools AB, SE-737 82 Fagersta, Sweden.
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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2013 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 235, no 25, 376-385 p.Article in journal (Refereed) Published
Abstract [en]

Ti(1−x−y)AlxSiyNz (0.02≤x≤0.46, 0.02≤y≤0.28, and 1.08≤z≤1.29) thin films were grown on cemented carbide substrates in an industrial scale cathodic arc evaporation system using Ti-Al-Si compound cathodes in a N2 atmosphere. The microstructure of the as-deposited films changes from nanocrystalline to amorphous by addition of Al and Si to TiN. Upon incorporation of 12 at% Si and 18 at% Al, the films assume an x-ray amorphous state. Post-deposition anneals show that the films are thermally stable up to 900 ◦C. The films exhibit age hardening up to 1000 ◦C with an increase in hardness from 21.9 GPa for as-deposited films to 31.6 GPa at 1000 ◦C. At 1100 ◦C severe out-diffusion of Co and W from the substrate occur, and the films recrystallize into c-TiN and w-AlN.

Place, publisher, year, edition, pages
2013. Vol. 235, no 25, 376-385 p.
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-80199DOI: 10.1016/j.surfcoat.2013.07.014ISI: 000329596100048OAI: oai:DiVA.org:liu-80199DiVA: diva2:546132
Available from: 2012-08-22 Created: 2012-08-22 Last updated: 2017-12-07Bibliographically approved
In thesis
1. Growth and Characterization of Amorphous TiAlSiN and HfAlSiN Thin Films
Open this publication in new window or tab >>Growth and Characterization of Amorphous TiAlSiN and HfAlSiN Thin Films
2012 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

This Thesis explores amorphous transition metal nitrides for cutting tool applications. The aim is to extend the knowledge on amorphous nitride thin lms, to describe the growth process, and to explore ways of characterizing these novel complex materials.

Thin lms of Ti-Al-Si-N and Hf-Al-Si-N were fabricated using industrial cathodic arc evaporation and magnetically-unbalanced reactive magnetron sputtering, respectively. The microstructure of the lms was studied using x-ray diraction (XRD) and transmission electron microscopy (TEM), while compositional analysis of the lms was performed by spectroscopic techniques (EDS, SIMS, and RBS). The mechanical properties were investigated by nanoindentation.

The Ti-Al-Si-N lms were grown on cemented carbide substrates using Ti-Al-Si compound cathodes in an N2 atmosphere. High Al and Si concentrations in the lms (i.e., 12 at% Si and 18 at% Al) promote renucleation and result in x-ray amorphous lms. High resolution TEM (HRTEM) reveals isolated grains, ~2 nm in size, embedded in an amorphous matrix. Annealing experiments show that the lms are thermally stable up to 900 oC. They exhibit age hardening, with an increase in hardness from 21.9 GPa for as-deposited lms to 31.6 GPa at 1000 oC. At 1100 oC severe out-diusion of Co and W from the substrate occurs, and the lms recrystallize into c-TiN and w-AlN.

The single layer Hf-Al-Si-N and multilayer Hf-Al-Si-N/HfN lms were grown on Si(001) substrates from a single Hf0:60Al0:20Si0:20 alloy target in an N2/Ar atmosphere. The composition and nanostructure of the lms was controlled during growth by independently varying the ion energy (Ei) and the ion-to-metal flux ratio (Ji=JMe). With Ji/JMe=8, the nanostructure and composition of the lms changes from x-ray amorphous with a Hf content of 0.6, to an amorphous matrix with encapsulated nanocrystals with 0.66≤Hf≤0.84, to nanocrystalline with 0.96≤Hf≤1.00, when increasing Ei from 15 to 65 eV. Varying Ji=JMe with Ei=13 eV yields electron-diraction amorphous lms at substrate temperatures of 100 oC. Hf-Al-Si-N/HfN multilayers with periods Λ=2-20 nm exhibit enhanced fracture toughness compared to polycrystalline VN, TiN, and Ti0:5Al0:5N reference samples; multilayer hardness values increase from 20 GPa with Λ=20 nm to 27 GPa with Λ=2 nm.

̴

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. 44 p.
Series
Linköping Studies in Science and Technology. Thesis, ISSN 0280-7971 ; 1542
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-80211 (URN)LIU-TEK-LIC-2012:27 (Local ID)978-91-7519-843-9 (ISBN)LIU-TEK-LIC-2012:27 (Archive number)LIU-TEK-LIC-2012:27 (OAI)
Presentation
2012-09-07, Jordan/Fermi, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (Swedish)
Opponent
Supervisors
Available from: 2012-08-22 Created: 2012-08-22 Last updated: 2016-08-31Bibliographically approved
2. Growth and Characterization of Amorphous Multicomponent Nitride Thin Films
Open this publication in new window or tab >>Growth and Characterization of Amorphous Multicomponent Nitride Thin Films
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis explores deposition of amorphous thin films based on the two transition metal nitride systems, TiN and HfN. Additions of Si, Al and B have been investigated using three different deposition techniques: dc magnetron sputtering, cathodic arc evaporation, and high power impulse magnetron sputtering (HIPIMS). The effect of elemental composition, bonding structure, growth temperature, and low-energy ion bombardment during growth has been investigated and correlated to the resulting microstructure and mechanical properties of the films. The thermal stability has been investigated by annealing experiments.

Deposition by cathodic arc evaporation yields dense and homogeneous coatings with essentially fully electron-diffraction amorphous structures with additions of either Al+Si, B+Si or B+Al+Si to TiN. The B-containing coatings have unusually few macroparticles. Annealing experiments show that Ti-Al-Si-N coatings have an age hardening behavior, which is not as clear for B-containing coatings. Compositional layering, due to rotation of the sample fixture during deposition, is present but not always visible in the as-deposited state. The layering acts as a template for renucleation during annealing. The coatings recrystallize by growth of TiN-rich  domains.

Amorphous growth by conventional dc magnetron sputtering is possible over a wide range of compositions for Ti-B-Si-N thin films. The Ti content in the films is reduced compared to the content in the sputtering target. Without Si, the films consist of a BN onion-like structure surrounding TiN nanograins. With additions of Si the films eventually grows fully amorphous. The growth temperature has only minor effect on the microstructure, due to the limited surface diffusion at the investigated temperature range (100-600 °C). Ion assisted growth leads to nanoscale densification of the films and improved mechanical properties.

Ti-B-Si-N thin films are also deposited by a hybrid technique where dc magnetron sputtering is combined with HIPIMS. Here, the Ti:B ratio remains equal to the target composition. Films with low Si content are porous with TiN nanograins separated by BN-rich amorphous channels and have low hardness. Increasing Si contents yield fully electron-amorphous films with higher hardness.

Finally, Hf-Al-Si-N single-layer and multilayer films are grown by dc magnetron sputtering from a single Hf-Al-Si target. Amorphous growth is achieved when the growth temperature was kept at its minimum. Low-energy substrate bias modulation is used to grow nanocomposite/nanocolumnar multilayers from the single Hf-Al-Si target, where the layers has essentially the same composition but different Si bonding structure, and different degree of crystallinity.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2014. 92 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1595
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-106576 (URN)10.3384/diss.diva-106576 (DOI)978-91-7519-337-3 (ISBN)
Public defence
2014-05-28, Planck, Fysikhuset, Campus Valla, Linköping, 10:00 (English)
Opponent
Supervisors
Available from: 2014-05-12 Created: 2014-05-12 Last updated: 2016-08-31Bibliographically approved

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Fager, HannaJohansson, MatsOdén, MagnusHultman, Lars

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