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Reactive Sputtering of Complex Multi-Component Nitride Thin Films Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology 1852 Reactive Sputtering of Complex Multi-component Nitride Thin Films KRISTINA VON FIEANDT ACTA UNIVERSITATIS UPSALIENSIS ISSN 1651-6214 ISBN 978-91-513-0744-2 UPPSALA urn:nbn:se:uu:diva-392704 2019 Dissertation presented at Uppsala University to be publicly examined in Polhemssalen, Ångströmslaboratoriet, Lägerhyddsvägen 1, Uppsala, Friday, 25 October 2019 at 09:15 for the degree of Doctor of Philosophy. The examination will be conducted in English. Faculty examiner: Professor Jean-Francois Pierson (University of Lorraine). Abstract von Fieandt, K. 2019. Reactive Sputtering of Complex Multi-component Nitride Thin Films. Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology 1852. 71 pp. Uppsala: Acta Universitatis Upsaliensis. ISBN 978-91-513-0744-2. The ever-increasing demand on improvement of protective nitride thin films has led to an expansion of the research field into multi-element based materials. The work in this thesis has focused on exploring new complex, multi-component nitride thin films based on three different material systems: Al-Ge-N, Hf-Nb-Ti-V-Zr-N and Al-Cr-Nb-Y-Zr-N. All films were synthesised by reactive dc magnetron sputtering and characterised with regard to structure and material properties, in particular the mechanical, optical and corrosion properties. The Al-Ge-O-N coatings exhibited amorphisation of the structure upon oxygen addition, via the formation of a crystalline (Al1-xGex)(N1-yOy) solid solution phase for low O contents. The mechanical properties were improved, and hardness values up to 29 GPa were achieved for low O and Ge concentrations, most likely due to nanocomposite hardening. The optical absorption edge was tuneable towards shorter and longer wavelengths with increasing the O and Ge content respectively. Annealing to 850°C showed indications of increased thermal stability for the quaternary Al-Ge-O-N films compared to the ternary Al-Ge-N films. Coatings in the Hf-Nb-Ti-V-Zr-N system were found to be highly crystalline featuring a single solid solution phase with NaCl-type structure for low Hf content, whereas an additional, tetragonally distorted, phase appeared for higher Hf contents. The mechanical properties, such as hardness and Young’s modulus increased with increasing Hf content, although the values were relatively low compared to those for transition metal nitrides in general. The Al-Cr-Nb-Y-Zr-N films also crystallised in the NaCl-type structure for the films with high nitrogen contents, i.e. between 46 and 51 at.%. However, partial elemental segregation was present, mainly for yttrium, both within the grains and in the column boundaries. XPS results suggested that yttrium was in a metallic state, while the remaining elements were present in a nitrided environment. The partial segregation could possibly explain the observed ductile behaviour of the nitride films. Electrochemical tests showed that the corrosion resistance increased with increased nitrogen content and the films performed in some cases better than a hyper-duplex stainless steel. This thesis demonstrates that solid solutions are formed for three relatively different nitride material systems when varying the composition. The solubilities of the solid solution phases were found to be limited as shown by amorphisation, partial elemental segregation or formation of a two-phase material. The limited solubility and the phase changes can be used to design the material properties. Kristina von Fieandt, Department of Chemistry - Ångström, Inorganic Chemistry, Box 538, Uppsala University, SE-751 21 Uppsala, Sweden. © Kristina von Fieandt 2019 ISSN 1651-6214 ISBN 978-91-513-0744-2 urn:nbn:se:uu:diva-392704 (http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-392704) Till mamma List of Papers This thesis is based on the following papers, which are referred to in the text by their Roman numerals1. I Influence of oxygen content on structure and material prop- erties of reactively sputtered Al-Ge-O-N thin films K. Johansson, E. Lewin Journal of Alloys and Compounds, 738, 515-527 (2018) II In situ formation of Ge nanoparticles by annealing of Al-Ge- N thin films followed by HAXPES and XRD K. von Fieandt, F. O. L. Johansson, O. Balmes, R. Lindblad, L. Riekehr, A. Lindblad, E. Lewin Inorganic Chemistry, 58, 16, 11100-11109 (2019) III Multicomponent Hf-Nb-Ti-V-Zr nitride coatings by reactive sputtering K. Johansson, L. Riekehr, S. Fritze, E. Lewin Surface & Coatings Technology, 349, 529-539 (2018) IV Multi-component (Al,Cr,Nb,Y,Zr)N thin films by reactive magnetron sputter deposition for increased hardness and corrosion resistance K. von Fieandt, E-M. Paschalidou, A. Srinath, P. Soucek, L. Riekehr, L. Nyholm, E. Lewin Submitted V Influence of N content on structure and mechanical proper- ties of multi-component Al-Cr-Nb-Y-Zr based thin films by reactive magnetron sputtering K. von Fieandt, L. Riekehr, B. Osinger, S. Fritze, E. Lewin In manuscript 1 Note that some papers are published in my former family name Johansson VI Corrosion in Al-Cr-Nb-Y-Zr-N multi-component alloys: What role does the nitrogen content play? A. Srinath, K. von Fieandt, R. Lindblad, S. Fritze, M. Korvela, J. Petersson, E. Lewin, L. Nyholm In manuscript Reprints were made with permission from the respective publishers My contribution to the papers I I planned the study and synthesised all samples. I performed all analyses and participated in all discussions. I wrote the main part of the manuscript while receiving input from the co-author. II I took part in planning the study and synthesised all samples. I performed all characterisations, except the TEM analysis, par- ticle size distribution analysis and the HAXPES data analysis. I participated in all discussions and wrote the manuscript while receiving input from the co-authors. III I planned the study and synthesised all samples. I performed all characterisations, except the TEM analysis. I participated in all discussions and wrote the main part of the manuscript while re- ceiving input from the co-authors. IV I planned the study and synthesised all samples. I did the XRD, SEM, XPS and electrical resistivity measurements. I partici- pated in all discussions and wrote the manuscript while receiv- ing input from the co-authors. V I planned the study and synthesised all samples. I performed all characterisations, except the TEM analysis. I participated in all discussions and wrote the main part of the manuscript while re- ceiving input from the co-authors. VI I took part in planning the study and synthesised all samples. I performed the XRD and SEM analysis and took part in the HAXPES measurements. I participated in most discussions and wrote parts of the manuscript. Disclaimer: Parts of this thesis are based on my licentiate thesis entitled Mul- ticomponent Nitride Thin Films by Reactive Magnetron Sputtering (Uppsala University, 2018) In this thesis some results are included that are not parts of any publication or manuscript. These results concern the material stability for Al-Ge-O-N and Al-Cr-Nb-Y-Zr-N based films. I performed all these experiments and charac- terisations. Other publications to which the author has contributed but which are not in- cluded in the present thesis: I On the growth, orientation and hardness of chemical vapor deposition Ti(C,N) L. von Fieandt, K. Johansson, T. Larsson, M. Boman, E. Lin- dahl Thin Solid Films, 645, 19-25 (2018) II Corrosion properties of CVD grown Ti(C,N) coatings in 3.5 wt-% NaCl environment L. von Fieandt, K. Johansson, E. Lindahl, T. Larsson, M. Bo- man, D. Rehnlund Corrosion Engineering Science and Technology, 53, 4, 316-320 (2018) III Influence of deposition temperature on the phase evolution of HfNbTiVZr high-entropy thin films S. Fritze, C. M. Koller, L. von Fieandt, P. Malinovskis, K. Jo- hansson, E. Lewin, P. H. Mayrhofer, U. Jansson Materials, 12, 4, 587 (2019) IV NbxTi1-xN low timing jitter single-photon detectors with unity internal detection efficiency at 1550 nm and 2.5 K Z. Julien, J. Chang, S. Steinhauer, K. von Fieandt, J. W. N. Los, G. Visser, N. Kalhor, T. Lettner, A. W. Elshaari, I. Esmaeil Za- deh, V. Zwiller. Accepted for publication in Optics Express (2019) Contents Introduction ................................................................................................... 11 Material systems ........................................................................................... 13 Nitride materials ....................................................................................... 13 Multi-component nitrides ......................................................................... 14 Oxynitride materials ................................................................................. 16 Al-Ge-N and Al-Ge-O-N ......................................................................... 17 Hf-Nb-Ti-V-Zr-N ..................................................................................... 18 Al-Cr-Nb-Y-Zr-N ..................................................................................... 18 Methods ........................................................................................................ 20 Thin film synthesis - reactive sputter deposition ...................................... 20 Analysis .................................................................................................... 23 Structural and chemical analysis ........................................................
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