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Determining role of W+ ions in the densification of TiAlWN thin films grown by hybrid HiPIMS/DCMS technique 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. Univ Illinois, IL 61801 USA.ORCID iD: 0000-0002-2955-4897
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.ORCID iD: 0000-0002-2837-3656
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.ORCID iD: 0000-0002-4898-5115
2023 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 41, no 1, article id 013407Article in journal (Refereed) Published
Abstract [en]

Hybrid high-power impulse and dc magnetron co-sputtering (HiPIMS/DCMS) with substrate bias synchronized to the high mass metal-ion fluxes was previously proposed as a solution to reduce energy consumption during physical vapor deposition processing and enable coatings on temperature-sensitive substrates. In this approach, no substrate heating is used (substrate temperature is lower than 150 C-o) and the thermally activated adatom mobility, necessary to grow dense films, is substituted by overlapping collision cascades induced by heavy ion bombardment and consisting predominantly of low-energy recoils. Here, we present direct evidence for the crucial role of W+ ion irradiation in the densification of Ti0.31Al0.60W0.09N films grown by the hybrid W-HiPIMS/TiAl-DCMS co-sputtering. The peak target current density J(max) on the W target is varied from 0.06 to 0.78 A/cm(2) resulting in more than fivefold increase in the number of W+ ions per deposited metal atom, eta = W+/(W + Al + Ti) determined by time-resolved ion mass spectrometry analyses performed at the substrate plane under conditions identical to those during film growth. The DCMS is adjusted appropriately to maintain the W content in the films constant at Ti0.31Al0.60W0.09N. The degree of porosity, assessed qualitatively from cross-sectional SEM images and quantitatively from oxygen concentration profiles as well as nanoindentation hardness, is a strong function of eta ( J m a x ). Layers grown with low eta values are porous and soft, while those deposited under conditions of high eta are dense and hard. Nanoindentation hardness of Ti0.31Al0.60W0.09N films with the highest density is & SIM;33 GPa, which is very similar to values reported for layers deposited at much higher temperatures (420-500 C-o) by conventional metal-ion-based techniques. These results prove that the hybrid HiPIMS/DCMS co-sputtering with bias pulses synchronized to high mass metal ion irradiation can be successfully used to replace conventional solutions. The large energy losses associated with heating of the entire vacuum chamber are avoided, by focusing the energy input to where it is in fact needed, i.e., the workpiece to be coated.

Place, publisher, year, edition, pages
A V S AMER INST PHYSICS , 2023. Vol. 41, no 1, article id 013407
National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:liu:diva-191188DOI: 10.1116/6.0002320ISI: 000906004900002OAI: oai:DiVA.org:liu-191188DiVA, id: diva2:1730166
Note

Funding Agencies|Swedish Research Council VR [2018-03957]; Swedish Energy Agency [51201-1]; Aforsk Foundation Grant [22-4]; Knut and Alice Wallenberg Foundation [KAW2016.0358, KAW2019.0290]; Carl Tryggers Stiftelse [CTS 20:150]; Competence Center Functional Nanoscale Materials (FunMat-II) VINNOVA Grant [2016-05156]; Swedish Research Council VR-RFI [2017-00646_9]; Swedish Foundation for Strategic Research [RIF14-0053]

Available from: 2023-01-24 Created: 2023-01-24 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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Li, XiaoPetrov, IvanHultman, LarsGreczynski, Grzegorz
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