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In Situ Formation of Ge Nanoparticles by Annealing of Al-Ge‑N ThinFilms Followed by HAXPES and XRD
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Inorganic Chemistry.ORCID iD: 0000-0001-7266-0022
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Molecular and Condensed Matter Physics.ORCID iD: 0000-0002-6471-1093
MAX IV Laboratory, Lund University, PO Box 118, SE-22100 Lund, Sweden.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Inorganic Chemistry.
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2019 (English)In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 58, no 16, p. 11100-11109Article in journal (Refereed) Published
Abstract [en]

Ge nanoparticles embedded in thin films have attracted a lot of attention due to their promising optical and electronic properties that can be tuned by varying the particle size and choice of matrix material. In this study, Ge nanoparticle formation was investigated for Al-Ge-N based thin films by simultaneous measurements of HAXPES and grazing incidence XRD during in situ annealing in vacuum conditions. As-deposited Al-Ge-N thin films, synthesized by reactive dc magnetron sputtering, consisted of a nanocrystalline (Al1–xGex)Ny solid solution and an amorphous tissue phase of Ge3Ny. Upon annealing to 750 °C, elemental Ge was formed shown by both HAXPES and XRD measurements, and N2 gas was released as measured by a mass spectrometer. Postannealed ex situ analysis by SEM and TEM showed that the elemental Ge phase formed spherical nanoparticles on the surface of the film, with an average size of 210 nm. As the annealing temperature increased further to 850 °C, the Ge particles on the film surface evaporated, while the phase segregation of Ge still could be observed within the film. Thus, these results show the possibility for a controlled synthesis of Ge nanoparticles through annealing of Al-Ge-N thin films to produce materials suitable for use in electronic or optoelectronic devices.

Place, publisher, year, edition, pages
2019. Vol. 58, no 16, p. 11100-11109
National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-392698DOI: 10.1021/acs.inorgchem.9b01631ISI: 000482173300075PubMedID: 31381309OAI: oai:DiVA.org:uu-392698DiVA, id: diva2:1349292
Funder
Swedish Research Council, 2014-6463EU, FP7, Seventh Framework Programme, INCA 600398Available from: 2019-09-08 Created: 2019-09-08 Last updated: 2019-10-08Bibliographically approved
In thesis
1. Reactive Sputtering of Complex Multi-component Nitride Thin Films
Open this publication in new window or tab >>Reactive Sputtering of Complex Multi-component Nitride Thin Films
2019 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

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.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2019. p. 71
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1852
National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:uu:diva-392704 (URN)978-91-513-0744-2 (ISBN)
Public defence
2019-10-25, Polhemssalen, Ångströmslaboratoriet, Lägerhyddsvägen 1, Uppsala, 09:15 (English)
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Supervisors
Available from: 2019-10-04 Created: 2019-09-08 Last updated: 2019-10-15

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von Fieant, KristinaJohansson, Fredrik O. L.Lindblad, RebeckaRiekehr, LarsLindblad, AndreasLewin, Erik

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