The self-assembly of magnesium aluminate spinel as a result of dewetting an overlaid thin film of (chiefly) gold was investigated. Thin films of gold were deposited on single-crystalline spinel substrates and were heat-treated to dewet gold film which led to self-assembly of intricate structures consisting of faceted spherical particles atop of frustums. The current work was conducted in continuation of previous studies which reported formation of such intricate structures. The most recent studies had evidently overruled a pure gold self-assembly scenario as was pointed out in preliminary investigations. It was in fact proven that these structures consist of three distinct parts: (i) a single or polycrystalline gold faceted sphere, (ii) quasi-phase interfacial bilayer, and (iii) a crystalline MgAl2O4 necking structure spontaneously risen from spinel substrate. In the current work, samples were produced through different film deposition methods of sputter, thermal evaporation, and e-beam evaporation coating which underwent thermal annealing to induce dewetting of gold film and subsequent self-assembly of intricate structures. Several characterization methods such as electron microscopy, X-ray energy dispersive spectroscopy, electron energy loss spectroscopy, and atom probe tomography were utilized to survey the different features of the intricate structures with focus on chemical analysis of the gold-spinel interface. The results rejected the previous findings about formation of interface complexion at the boundary of gold-spinel. It was found out that gold-spinel interface is in fact an ordinary metal-oxide boundary with sharp atomic distinction and no inter-diffusion or formation of interfacial complexion. It was further discovered that dewetting pure gold thin films does not result in formation of spinel self-assembly and existence of elemental impurities of copper (Cu) in the initial film is vital in development of such structures. Finally, it was concluded that chemical composition of metallic overlayer and the heat treatment parameters most fundamentally influence formation and physical characteristics of those self-assembled structures. / Thesis / Master of Applied Science (MASc)

Afin d’améliorer la durée de vie des micro-relais MEMS ohmiques, plusieurs traitements de surface de films minces d’or sont réalisés pour augmenter leur dureté tout en conservant une résistance électrique de contact faible.Les revêtements ultrafins de ruthénium (20 à 100 nm) déposés sur l’or augmentent la dureté des surfaces de contact d’un facteur 15. L’implantation ionique de bore ou d’azote (3,5 ppm à 10 % atomique) à une profondeur de 100 nm dans le film mince d’or permet d’atteindre un gain en dureté de 75%. Le contrôle (AFM, EBSD et DRX) de la microstructure induite met en évidence le durcissement par solution solide par insertion. Mais au-delà de 1% atomique, les atomes d’azote quittent le réseau cristallin de l’or pour former des précipités de nitrure d’or.L’analyse AFM (rugosité et diamètre) des empreintes résiduelles (quelques μm²) réalisées par nano-indentation sphérique, imitant le cyclage et le fluage des surfaces de contact de ces MEMS, démontre l’apport de ces traitements de surface. De plus, leurs résistances électriques de contact, mesurées par nano-indentation instrumentée reproduisant un micro-contact identique à un dispositif réel, sont similaires à celle de l’or pur.La modélisation discrète mécanique du contact rugueux est ajustée à la mesure de la déformation mécanique de nano-rugosités en comparant les relevés topographiques réalisés par AFM avant et après nano-indentation sphérique. La comparaison entre la modélisation et la mesure de la résistance électrique de contact indique que pour les gammes de force utilisées dans les micro-relais MEMS (inférieure au mN), seule une fraction allant de 2% à 9% de la surface de contact réelle est conductrice. / Ohmic MEMS switches made by gold thin films are promising devices but their mechanical contacts are one of the critical concerns for enhancing reliability. For this reason, surface processes are investigated in this work to improve both mechanical and electrical contact resistance (ECR) of MEMS gold contacts. Ruthenium ultra-thin films (20 to 100 nm) deposited on a top of gold layer increase surface hardness by a factor of fifteen. In parallel, surface implantations of both boron (<10% atomic) or nitrogen (<0.1% atomic) into gold reveals a solid solution hardening by insertion, thus increasing the hardness of initial film by about 75% and 25%, respectively. Notably, above 0.1% atomic of nitrogen, atoms precipitate from the tetra or octahedral sites of gold inducing a decrease of hardness.Static and multi load/unload spherical nano-indentation are performed on treated gold thin films to simulate the mechanical actuation of ohmic MEMS switches. Analysis of residual imprints (about few µm²) from treated surface exhibits both minimal local deformation and adhesion forces that reduce stiction probability. In-situ measurement of ECR for treated gold by instrumented nano-indentation, reproducing the design of MEMS, is in the same range of pure gold-to-gold configuration.A new mechanical discrete model of rough contact is introduced, confronted and validated to the experimental mechanical surface deformation obtained by comparison of AFM images before and after spherical nano-indentation. An electrical discrete model is added and fitted to the ECR measurements. In ohmic MEMS switch load range (< 1 mN), the conductive area is found to be about 2% to 9% of the real contact area.

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