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Towards energy-efficient physical vapor deposition: Mapping out the effects of W+ energy and concentration on the densification of TiAlWN thin films grown with no external heating
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
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Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering. Univ Illinois, IL 61801 USA; Univ Illinois, IL 61801 USA; Natl Taiwan Univ Sci & Technol, Taiwan.ORCID iD: 0000-0002-2955-4897
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2021 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 424, article id 127639Article in journal (Refereed) Published
Abstract [en]

Hybrid high power impulse/direct current magnetron sputtering (HiPIMS/DCMS) film growth technique with metal-ion-synchronized substrate bias allows for significant energy savings as compared to conventional PVD methods. For carefully selected type of metal ion irradiation, taking into account ion mass, ionization potential, and reactivity towards working gas, fully dense and hard films can be obtained with no intentional substrate heating. The thermally-driven adatom mobility, which is an essential densification mechanism in conventional film growth that takes place at elevated temperatures, is replaced with that supplied by effective low-energy recoil creation. In this contribution we explore effects of the high-mass W+ irradiation, which has proven to be the most efficient in densifying Ti0.50Al0.50N layers, serving here as a model system, grown with no substrate heating. We study the effects of two essential parameters: W+ energy EW+ and W concentration x, on film porosity, phase content, nanostructure, and mechanical properties. EW+ varies from similar to 90 to similar to 630 eV (controlled by substrate bias voltage amplitude V-s) and x from 0.02 to 0.12 (controlled by the HiPIMS pulse length), while the HiPIMS peak target current is kept constant. Results reveal that a strong coupling exists between the W+ incident energy and the minimum W concentration required to grow dense layers.

Place, publisher, year, edition, pages
Elsevier Science SA , 2021. Vol. 424, article id 127639
Keywords [en]
Thin films; TiAlN; Magnetron sputtering; HiPIMS; Low temperature
National Category
Condensed Matter Physics
Identifiers
URN: urn:nbn:se:liu:diva-179830DOI: 10.1016/j.surfcoat.2021.127639ISI: 000697567600010OAI: oai:DiVA.org:liu-179830DiVA, id: diva2:1600468
Note

Funding Agencies|Swedish Research Council VRSwedish Research Council [2018-03957]; Swedish Energy AgencySwedish Energy Agency [51201-1]; Knut and Alice Wallenberg FoundationKnut & Alice Wallenberg Foundation [KAW2016.0358]; Competence Center Functional Nanoscale Materials (FunMat-II) VINNOVA grantVinnova [2016-05156]; Carl Tryggers Stiftelse for Vetenskaplig Forskning [CTS 20:150, CTS 15:219, CTS 14:431]; Swedish research council VR-RFISwedish Research Council [2017-00646_9]; Swedish Foundation for Strategic ResearchSwedish Foundation for Strategic Research [RIF14-0053]

Available from: 2021-10-05 Created: 2021-10-05 Last updated: 2023-05-24
In thesis
1. Toward Energy-efficient Physical Vapor Deposition: Routes for Replacing Substrate Heating during Magnetron Sputtering by Employing Metal Ion Irradiation
Open this publication in new window or tab >>Toward Energy-efficient Physical Vapor Deposition: Routes for Replacing Substrate Heating during Magnetron Sputtering by Employing Metal Ion Irradiation
2023 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In this Thesis, magnetron sputtering is perfected as an environmental-friendly deposition technique. I performed systematic studies of a novel approach - hybrid high-power impulse and dc magnetron co-sputtering (HiPIMS/DCMS) with metal-ion-synchronized substrate bias pulses. The technique relies on the use of high-mass metal ion irradiation from the HiPIMS source to densify material deposited by the primary metal targets that operate in the DCMS mode. Thermally-driven adatom mobility, conventionally used to obtain high-quality layers, is replaced by low-energy recoils that are effectively created upon heavy metal ion bombardment of the growing film surface. As a result, the need for external heating is effectively eliminated and the useful growth temperature can be as low as 130 °C.   

Ti-Al-N is chosen as a model materials system for the studies in this thesis due to its relevance for industrial applications and well-known challenges for phase stability control. The role of the metal ion mass on densification, phase content, nanostructure, and mechanical properties of metastable cubic Ti0.50Al0.50N-based thin films is investigated. Three series of (Ti1-yAly)1-xMexN (Me = Cr, Mo, W) films are grown with x varied intentionally by adjusting the DCMS power. There is a strong dependence of film properties on the mass of the HiPIMS-generated metal ions. All layers deposited with Cr+ irradiation exhibit porous nanostructure, high oxygen content, and poor mechanical properties. In contrast, (Ti1-yAly)1-xWxN films are fully-dense even with the lowest W concentration, x = 0.09.  

A strong coupling is found between W+ incident energy Ew+ and minimum W concentration x required to grow dense (Ti1-yAly)1-xWxN layers. With lower x, higher Ew+ is needed to obtain dense films. (Ti1-yAly)1-xWxN film growth is also studied as a function of the relative Al content on the metal lattice, y = Al / (Al + Ti), covering the entire range up to the achievable solubility limit of y ~ 0.67. High-Al content films that are desired in industrial applications (as the high temperature oxidation resistance increases with increasing y) are demonstrated, while precipitation of the softer hexagonal AlN phase is avoided. It is shown that the W+ irradiation from HiPIMS source can be used to grow high-Al content layers with high hardness and low residual stress, while avoiding wurtzite AlN precipitation.  

The critical parameter that controls the growth is shown to be the average momentum transfer per deposited metal adatom. W+ ion irradiation is shown to have a determining role in the densification of TiAlWN films grown by hybrid W-HiPIMS/TiAl-DCMS co-sputtering. Films with the same composition were grown as a function of the number of W+ ions per deposited metal atom, η = W+/ (W + Al + Ti). The latter was varied in a wide range by altering the peak target current density on the W target, as confirmed by time-resolved ion mass spectrometry analyses performed at the substrate plane. I demonstrate that the degree of porosity and the nanoindentation hardness are strong functions of η.   

Finally, high-temperature properties of TiAlWN films grown by hybrid W-HiPIMS/TiAl-DCMS co-sputtering with no external substrate heating is explored, as motivated by application requirements, where the temperature of cutting inserts during machining exceeds 900 °C. A new age hardening mechanism was discovered with Guinier-Preston (GP) zone formation in a ceramic material. Layers with low Al content maintain high hardness well above the annealing temperature characteristic of spinodal decomposition. The evidence from electron microscopy, ab initio calculations, and molecular dynamics simulations, shows that the GP effect originates from the formation of atomic-plane-thick W discs populating {111} planes of the cubic matrix. The results demonstrate for the model materials system of TiAlN that the process energy consumption can be reduced by as much as 64% with respect to conventional methods, with no compromise on coating quality. 

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2023. p. 40
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 2328
Keywords
PVD, Magnetron sputtering, Thin films, HiPIMS, TiAlN, Energy efficiency
National Category
Materials Chemistry
Identifiers
urn:nbn:se:liu:diva-194088 (URN)10.3384/9789180752428 (DOI)9789180752411 (ISBN)9789180752428 (ISBN)
Public defence
2023-09-01, Planck, F-building, Campus Valla, Linköping, 09:15 (English)
Opponent
Supervisors
Note

Funding: The research was primarily financed by the Swedish Research Council (VR) Grant 2018-03957 and the Swedish Energy Agency Grant 51201-1. Additional support was also received from a Knut and Alice Wallenberg Foundation Scholar Grant (Hultman: KAW2016.0358), the Competence Center Functional Nanoscale Materials (FunMat-II) VINNOVA grant 2016-05156,  the VINNOVA grant 2019-04882, the Carl Tryggers Stiftelse contracts CTS 17:166, CTS 15:219 and CTS 14:431.The work supported by the Swedish research council VR-RFI (2017-00646_9) for the accelerator-based ion-technological center and from the Swedish Foundation for Strategic Research (Per Persson: RIF14-0053) for the Tandem accelerator laboratory in Uppsala University is also acknowledged.

Updates:2023-05-24 The thesis was first published online. 2023-05-29 The cover was changed in the published version to match the printed version. Before this date the PDF has been downloaded 38 times.

Available from: 2023-05-24 Created: 2023-05-24 Last updated: 2023-08-01Bibliographically approved

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