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Hf-Al-Si-N multilayers deposited by reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target using high-flux, low-energy modulated substrate bias: film growth and properties
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
Air Force Research Laboratory, Materials and Manufacturing Directorate, Wright-Patterson AFB, Ohio, USA.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.ORCID iD: 0000-0002-4898-5115
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
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2014 (English)Manuscript (preprint) (Other academic)
Abstract [en]

Hf1−x−yAlxSiyN (0≤x≤0.14, 0≤y≤0.13) single layers and multilayer films are grown on Si(001) at a substrate temperature Ts=250 °C using ultrahigh vacuum magnetically-unbalanced reactive magnetron sputtering from a single Hf0.6Al0.2Si0.2 target in a 5%-N2/Ar atmosphere at a total pressure of 20 mTorr (2.67 Pa). The composition and nanostructure of Hf1−x−yAlxSiyN is controlled during growth by varying the ion energy (Ei) of the ions incident at the film surface, keeping the ion-to-metal flux ratio (Ji/JMe) constant at 8. By sequentially switching Ei between 10 and 40 eV, Hf0.77Al0.10Si0.13N/Hf0.78Al0.14Si0.08N multilayers with bilayer periods Λ = 2-20 nm are grown, in which the Si2p bonding state changes from predominantly Si-Si bonds for films grown at Ei = 10 eV, to mainly Si-N bonds at Ei = 40 eV. Multilayer hardness values increase monotonically from 20 GPa with Λ = 20 nm to 27 GPa with Λ = 2 nm, while multilayer fracture toughness increases with increasing Λ. Multilayers with Λ = 10 nm have the optimized property combination of being bothrelatively hard, H∼24 GPa, and fracture tough.

Place, publisher, year, edition, pages
2014.
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-106575OAI: oai:DiVA.org:liu-106575DiVA: diva2:716732
Available from: 2014-05-12 Created: 2014-05-12 Last updated: 2016-08-31Bibliographically approved
In thesis
1. 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, HannaGreczynski, GrzegorzJensen, JensLu, JunGreene, J.E.Petrov, IvanHultman, Lars

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