In an electron fluid, both resistive and viscous mechanisms can be present. In systems with perfect translational invariance momentum is a conserved quantity, and as the electrons carry both charge and momentum, the current cannot decay. Predictions from theories at the particle physics-condensed matter physics interface using the `AdS/CFT' correspondence suggest that hydrodynamic charge flow might exist in some exotic metallic states. In the high-Tc cuprates the T-linear resistivity in the strange metal regime is conjectured to be due to hydrodynamic effects. In this dissertation, I start out drawing a theoretical outline of the hydrodynamic theory of electron transport in solids. In the search for a high purity metal that can host such a hydrodynamic electron transport, we looked at the non-magnetic delafossite oxides PdCoO2 and PtCoO2, which have the highest conductivities of any known oxides, and whose key properties I will review. As the signatures of viscosity can only be realised in transport through boundary scattering, the samples had to be taken down to the mesoscopic limit, where the momentum conserving and relaxing scattering mean free paths of the material are comparable to the channel width. I will discuss the focussed ion beam (FIB) micro-structuring technique that I have implemented to fabricate the mesoscopic devices. To interpret the transport in the mesoscopic regime, a comprehensive understanding of the bulk transport is first necessary and I will present my measurements of the magnetoresistance and Hall effect in both materials, which show deviations from the predictions of standard models highlighting some intriguing physics even in the bulk limit. Finally, I will present the data from magnetotransport measurements at the mesoscopic limit. Magnetic field introduces a variable length scale, the cyclotron radius, in the system which can be used to tune through different transport regimes. I will discuss the ballistic and hydrodynamic signatures in the transport that becomes accessible through magnetic field tuning in the mesoscopic samples of the delafossites PdCoO2 and PdCoO2.

L’objectif principal de ce travail est d’optimise la tomographie par coupe sériée dans un microscope ‘FIB’, en utilisant soit l’imagerie électronique du microscope à balayage (tomographie FIB-MEB), soit la diffraction des électrons rétrodiffusés (tomographie dite EBSD 3D). Dans les 2 cas, des couches successives de l’objet d’étude sont abrasées à l’aide du faisceau ionique, et les images MEB ou EBSD ainsi acquises séquentiellement sont utilisées pour reconstruire le volume du matériau. A cause de différentes sources de perturbation incontrôlées, des dérives sont généralement présentes durant l'acquisition en tomographie FIB-MEB. Nous avons ainsi développé une procédure in situ de correction des dérives afin de garder automatiquement la zone d'intérêt (ROI) dans le champ de vue. Afin de reconstruction le volume exploré, un alignement post-mortem aussi précis que possible est requis. Les méthodes actuelles utilisant la corrélation-croisée, pour robuste que soit cette technique numérique, présente de sévères limitations car il est difficile, sinon parfois impossible de se fier à une référence absolue. Ceci a été démontré par des expériences spécifiques ; nous proposons ainsi 2 méthodes alternatives qui permettent un bon alignement. Concernant la tomographie EBSD 3D, les difficultés techniques liées au pilotage de la sonde ionique pour l'abrasion précise et au repositionnement géométrique correct de l’échantillon entre les positions d'abrasion et d’EBSD conduisent à une limitation importante de la résolution spatiale avec les systèmes commerciaux (environ 50 nm)3. L’EBSD 3D souffre par ailleurs de limites théoriques (grand volume d'interaction électrons-solide et effets d'abrasion. Une nouvelle approche, qui couple l'imagerie MEB de bonne résolution en basse tension, et la cartographie d'orientation cristalline en EBSD avec des tensions élevées de MEB est proposée. Elle a nécessité le développement de scripts informatiques permettant de piloter à la fois les opérations d’abrasion par FIB et l’acquisition des images MEB et des cartes EBSD. L’intérêt et la faisabilité de notre approche est démontrée sur un cas concret (superalliage de nickel). En dernier lieu, s’agissant de cartographie d’orientation cristalline, une méthode alternative à l’EBSD a été testée, qui repose sur l’influence des effets de canalisation (ions ou électrons) sur les contrastes en imagerie d’électrons secondaires. Cette méthode corrèle à des simulations la variation d’intensité de chaque grain dans une série d’images expérimentales obtenues en inclinant et/ou tournant l’échantillon sous le faisceau primaire. Là encore, la méthode est testée sur un cas réel (polycritsal de TiN) et montre, par comparaison avec une cartographie EBSD, une désorientation maximale d'environ 4° pour les angles d’Euler. Les perspectives d’application de cette approche, potentiellement beaucoup plus rapide que l’EBSD, sont évoquées. / The aim of current work is to optimize the serial-sectioning based tomography in a dual-beam focused ion beam (FIB) microscope, either by imaging in scanning electron microscopy (so-called FIB-SEM tomography), or by electron backscatter diffraction (so-called 3D-EBSD tomography). In both two cases, successive layers of studying object are eroded with the help of ion beam, and sequentially acquired SEM or EBSD images are utilized to reconstruct material volume. Because of different uncontrolled disruptions, drifts are generally presented during the acquisition of FIB-SEM tomography. We have developed thus a live drift correction procedure to keep automatically the region of interest (ROI) in the field of view. For the reconstruction of investigated volume, a highly precise post-mortem alignment is desired. Current methods using the cross-correlation, expected to be robust as this digital technique, show severe limitations as it is difficult, even impossible sometimes to trust an absolute reference. This has been demonstrated by specially-prepared experiments; we suggest therefore two alternative methods, which allow good-quality alignment and lie respectively on obtaining the surface topography by a stereoscopic approach, independent of the acquisition of FIB-SEM tomography, and realisation of a crossed ‘hole’ thanks to the ion beam. As for 3D-EBSD tomography, technical problems, linked to the driving the ion beam for accurate machining and correct geometrical repositioning of the sample between milling and EBSD position, lead to an important limitation of spatial resolution in commercial softwares (~ 50 nm)3. Moreover, 3D EBSD suffers from theoretical limits (large electron-solid interaction volume for EBSD and FIB milling effects), and seems so fastidious because of very long time to implement. A new approach, coupling SEM imaging of good resolution (a few nanometres for X and Y directions) at low SEM voltage and crystal orientation mapping with EBSD at high SEM voltage, is proposed. This method requested the development of computer scripts, which allow to drive the milling of FIB, the acquisition of SEM images and EBSD maps. The interest and feasibility of our approaches are demonstrated by a concrete case (nickel super-alloy). Finally, as regards crystal orientation mapping, an alternative way to EBSD has been tested; which works on the influence of channelling effects (ions or electrons) on the imaging contrast of secondary electrons. This new method correlates the simulations with the intensity variation of each grain within an experimental image series obtained by tilting and/or rotating the sample under the primary beam. This routine is applied again on a real case (polycrystal TiN), and shows a max misorientation of about 4° for Euler angles, compared to an EBSD map. The application perspectives of this approach, potentially faster than EBSD, are also evoked.

Dehnungssensoren werden zur Überwachung von sicherheitsrelevanten Bauteilen, besonders in Bauteilen aus faserverstärkten Polymermatrixverbundwerkstoffen eingesetzt. Durch deren Integration in das Bauteilinnere werden sie vor schädigenden mechanischen sowie korrosiven Einwirkungen geschützt. Dies gewährleistet eine zuverlässige sowie dauerhafte Funktion. Verschiedene Ansätze zur Weiterentwicklung integrierbarer Dehnungssensoren werden international untersucht. Die Verringerung des Sensordurchmessers auf Abmaße im Bereich des Durchmessers von Verstärkungsfasern ist dabei ein bedeutendes Entwicklungsziel. Insbesondere bei der Integration in Bauteile aus faserverstärkten Kunststoffen sorgen zum Durchmesser von Fasern vergleichbare Sensordurchmesser für eine optimale Sensoranbindung. Die Bildung von Harznestern sowie schwächender Unstetigkeiten kann mittels dünner Sensoren verhindert werden. Dies gewährleistet eine artefaktefreie Dehnungsmessung. Drei verschiedene Ansätze für neuartige Dehnungssensoren mit kleinem Querschnitt wurden in dieser Arbeit untersucht. / Strain sensors are used for structural health monitoring issues, certainly in parts with high safety requirements made of fibre-reinforced plastic composites. The integration of these sensors inside the parts protects them against any mechanical and corrosive impact. The sensor functionality can be enhanced by integration. There is a lot of international research effort to further develop integratable strain sensors. Different approaches are currently pursued. This thesis presents the results of investigations on three different approaches for novel strain sensors. The main goal of these investigations was to minimise the sensor diameter down to the diameter of reinforcing fibres. The small diameter allows for an optimum and artefact free integration of the sensors. The formation of resin nests and notches to the material structure can be prevented by integrating sensor with a smaller diameter. The strain measurement and monitoring is enhanced and more reliable then.

Dehnungssensoren werden zur Überwachung von sicherheitsrelevanten Bauteilen, besonders in Bauteilen aus faserverstärkten Polymermatrixverbundwerkstoffen eingesetzt. Durch deren Integration in das Bauteilinnere werden sie vor schädigenden mechanischen sowie korrosiven Einwirkungen geschützt. Dies gewährleistet eine zuverlässige sowie dauerhafte Funktion. Verschiedene Ansätze zur Weiterentwicklung integrierbarer Dehnungssensoren werden international untersucht. Die Verringerung des Sensordurchmessers auf Abmaße im Bereich des Durchmessers von Verstärkungsfasern ist dabei ein bedeutendes Entwicklungsziel. Insbesondere bei der Integration in Bauteile aus faserverstärkten Kunststoffen sorgen zum Durchmesser von Fasern vergleichbare Sensordurchmesser für eine optimale Sensoranbindung. Die Bildung von Harznestern sowie schwächender Unstetigkeiten kann mittels dünner Sensoren verhindert werden. Dies gewährleistet eine artefaktefreie Dehnungsmessung. Drei verschiedene Ansätze für neuartige Dehnungssensoren mit kleinem Querschnitt wurden in dieser Arbeit untersucht. / Strain sensors are used for structural health monitoring issues, certainly in parts with high safety requirements made of fibre-reinforced plastic composites. The integration of these sensors inside the parts protects them against any mechanical and corrosive impact. The sensor functionality can be enhanced by integration. There is a lot of international research effort to further develop integratable strain sensors. Different approaches are currently pursued. This thesis presents the results of investigations on three different approaches for novel strain sensors. The main goal of these investigations was to minimise the sensor diameter down to the diameter of reinforcing fibres. The small diameter allows for an optimum and artefact free integration of the sensors. The formation of resin nests and notches to the material structure can be prevented by integrating sensor with a smaller diameter. The strain measurement and monitoring is enhanced and more reliable then.

An experimental method was further developed to quantify the anisotropy of multi-site fatigue crack initiation behaviors in high strength Al alloys by four-point bend fatigue testing under stress control. In this method, fatigue crack initiation sites (fatigue weak-links, FWLs) were measured on the sample surface at different cyclic stress levels. The FWL density in an alloy could be best described using a three-parameter Weibull function of stress, though other types of sigmoidal functions might also be used to quantify the relationship between FWL density and stress. The strength distribution of the FWLs was derived from the Weibull function determined by fitting the FWLs vs. stress curve experimentally obtained. As materials properties, the FWL density and strength distribution could be used to evaluate the fatigue crack nucleation behaviors of engineering alloys quantitatively and the alloy quality in terms of FWL density and strength distribution. In this work, the effects of environment, types of microstructural heterogeneities and loading direction on FWLs were all studied in detail in AA7075-T651, AA2026-T3511, and A713 Al alloys, etc. It was also found that FWLs should be quantified as a Weibull-type function of strain instead of stress, when the applied maximum cyclic stress exceeded the yield strength of the tested alloys. In this work, four-point bend fatigue tests were conducted on the L-T (Rolling-Transverse), L-S (Rolling-Short transverse) and T-S planes of an AA7075-T651 alloy plate, respectively, at room temperature, 20 Hz, R=0.1, in air. The FWL populations, measured on these surfaces, were a Weibull-type function of the applied maximum cyclic stress, from which FWL density and strength distribution could be determined. The alloy showed a significant anisotropy of FWLs with the weak-link density being 11 mm-2, 15 mm-2 and 4 mm-2 on the L-T, L-S and T-S planes, respectively. Fatigue cracks were predominantly initiated at Fe-containing particles on the L-T and L-S planes, but only at Si-bearing particles on the T-S plane, profoundly demonstrating that the pre-fractured Fe-containing particles were responsible for crack initiation on the L-T and L-S planes, since the pre-fracture of these particles due to extensive deformation in the L direction during the prior rolling operation could only promote crack initiation when the sample was cyclically stressed in the L direction on both the L-T and L-S planes. The fatigue strengths of the L-T, L-S and T-S planes of the AA7075 alloy were measured to be 243.6, 273.0 and 280.6 MPa, respectively. The differences in grain and particle structures between these planes were responsible for the anisotropy of fatigue strength and FWLs on these planes. Three types of fatigue cracks from particles, type-I: the micro-cracks in the particles could not propagate into the matrix, i.e., type-II: the micro-cracks were fully arrested soon after they propagated into the matrix, and type-III: the micro-cracks became long cracks, were observed in the AA7075-T651 alloy after fatigue testing. By cross-sectioning these three-types of particles using Focused Ion Beam (FIB), it was found that the thickness of the particles was the dominant factor controlling fatigue crack initiation at the particles, namely, the thicker a pre-fractured Fe-containing particle, the easier it became a type-III crack on the L-T and L-S planes. On the T-S plane, there were only types-I and III Si-bearing particles at which crack were initiated. The type-I particles were less than 6.5 μm in thickness and type-III particles were thicker than 8.3 μm. Cross-sectioning of these particles using FIB revealed that these particles all contained gas pores which promoted crack initiation at the particles because of higher stress concentration at the pores in connection with the particles. It was also found that fatigue cracks did not always follow the any specific crystallographic planes within each grain, based on the Electron Backscatter Diffraction (EBSD) measurement. Also, the grain orientation did not show a strong influence on crack initiation at particles which were located within the grains. The topography measurements with an Atomic Force Microscope (AFM) revealed that Fe-containing particles were protruded on the mechanically polished surface, while the Si-bearing particles were intruded on the surface, which was consistent with hardness measurements showing that Si-bearing particles were softer (4.030.92 GPa) than Fe-containing ones (8.9 0.87 GPa) in the alloy. To verify the 3-D effects of the pre-fractured particles on fatigue crack initiation in high strength Al alloys, rectangular micro-notches of three different types of dimensions were fabricated using FIB in the selected grains on the T-S planes of both AA2024-T351 and AA7075-T651 Al alloys, to mimic the three types of pre-fractured particles found in these alloys. Fatigue testing on these samples with the micro-notches verified that the wider and deeper the micro-notches, the easier fatigue cracks could be initiated at the notches. In the AA2024-T351 samples, cracks preferred to propagate along the {111} slip plane with the smallest twist angle and relatively large Schmid factor. These experimental data obtained in this work could pave a way to building a 3-D quantitative model for quantification of fatigue crack initiation behaviors by taking into account the driving force and resistance to short crack growth at the particles in the surface of these alloys.

Patch antennas are fundamental elements in many microwave communications systems. However, patch antennas receive/transmit signals over a very narrow bandwidth (typically a maximum of 3% bandwidth). Design modifications directed toward bandwidth expansion generally yield 10% to 40% bandwidth. The series varactor tuned patch antenna configuration was the bandwidth enhancement method explored in this research; this configuration is implemented by dividing a patch antenna into multiple sections and placing varactors across the resultant gaps. In addition to yielding a large bandwidth, the configuration has a number of ancillary benefits, including straightforward integration and design flexibility. Through the research represented by this work, the properties of the series varactor tuned patch antenna, herein referred to as the Fragmented Patch Antenna (or FPA), were explored and optimized. As a result, an innovative patch antenna was produced that yielded 63.4% frequency tuning bandwidth and covered a frequency range between 2.8 and 5.4 GHz. The wide bandwidth was achieved through a detailed parametric study. The products of this study were the discovery of multiple tuning resonances that were used to expand the tuning bandwidth and the understanding/documentation of the significance of specific antenna dimensions. Measurement results were obtained through the fabrication of a prototype antenna using semiconductor varactors. In the second research phase, the construction of capacitors using the tunable permittivity material Barium Strontium Titanate (BST) was investigated. Using this material in conjunction with nano-fabrication techniques, varactors were developed that had good estimated performance characteristics and were considered appropriate for integration into adaptive microwave circuitry, such as the tunable antenna system. The varactors were constructed by using Focused Ion Beam (FIB) milling to create a nano-scale capacitive gap in a transmission line. A combination of end-point current detection (EPD) and cross-section scanning electron (SEM) and ion beam (FIB) microscope images were used to optimize the milling procedure. The future extensions of this work include the integration of the BST varactors with the antenna design; the configuration of the developed BST varactors lends itself to a straightforward integration with the FPA antenna.

La zircone 3Y-TZP présente un grand intérêt pour les applications dentaires, en implantologie orale, elle semble être un matériau extrêmement prometteur: elle allie une biocompatibilité à un aspect esthétique satisfaisant et présente aussi des propriétés mécaniques très supérieures aux autres céramiques. Ces bonnes propriétés mécaniques sont intimement liées à la microstructure du matériau, elle-même directement liée aux procédés d’élaboration comme nous l’a rappelé l’alarmante série de ruptures de plus de 800 têtes de prothèses de hanche en zircone au début des années 2000, due au phénomène de vieillissement de ce matériau. Cependant, les études cliniques menées à ce jour ne font toujours pas état des interrelations existant entre la microstructure, les propriétés mécaniques et la sensibilité au vieillissement. Il était donc primordial de valider et d’appliquer les connaissances acquises dans le domaine des sciences des matériaux pour l’application de la zircone 3Y-TZP en implantologie oral. C’est l’objectif de notre première publication. Nous avons également développé, dans notre deuxième publication, un protocole d’évaluation permettant dans un premier temps, d’évaluer l’effet de l’état de surface et de la microstructure sur la résistance mécanique d’implants neufs, puis de suivre leurs cinétiques de vieillissement tout en analysant l’évolution de la microstructure et son influence sur la résistance mécanique au cours du vieillissement. Tout cela permettant in fine, de prédire la durabilité d’un type d’implant. Nous avons par la suite, développé un programme informatique permettant la détection et la quantification du vieillissement pour un volume donné. Cette détection de la zone vieillie ou transformée est basée sur des modifications microstructurales caractéristiques engendrées lors du vieillissement. Enfin, nous avons pu mettre en évidence l’occurrence du phénomène de vieillissement in vivo, par l’analyse d’explants issus d’une étude clinique et démontrer leur probable implication dans ces cas d’échec. Le logiciel informatique de traitement d’image développé a été également, appliqué aux explants dans le but de mettre en lumière et d’expliciter l’occurrence du phénomène de vieillissement in vivo, afin de sensibiliser les acteurs de ce marcher aux problématiques rencontrées et d’optimiser de ce dispositif médical, à la lumière des connaissances actuelles. / 3Y-TZP zirconia is gaining interest in oral implantology, it seems to be a promising material with good biocompatibility, esthetic appearance and also the highest mechanical properties for a ceramic. These mechanical properties are closely related to the microstructure of the material itself directly related to production processes as we recalled the alarming series of breaks of more than 800 heads of zirconia hip replacements in the early 2000, due to the aging phenomenon of the material. However, clinical studies to date are still not state of the interrelationships between microstructure, mechanical properties and sensitivity to aging. It was therefore important to validate and apply the knowledge gained in the field of materials science for the application of 3Y-TZP zirconia oral implantology. This is the goal of our first publication. We also have developed in our second publication, a protocol to assess the effect of the surface modification and microstructure on the mechanical strength of new implants and follow their kinetics of aging and also, the evolution of the microstructure and its influence on the mechanical strength during aging, to predict the durability of a type of implant. We have subsequently developed a computer program for the detection and quantification of the aging for a given volume. This detection of the aged or transformed area is based on microstructural modifications produced during aging. Finally, we have been able to demonstrate the occurrence of the phenomenon of aging in vivo, by analyzing explants from a clinical study and demonstrate their involvement in the case of dental implant failure. The image processing developed was also applied to the explants in order to highlight and explain the occurrence of in vivo aging phenomenon. The objective is to optimize this medical device, in the light of current knowledge.

Transmission Electron Microscopy (TEM) on light element materials and soft matters is problematic due to electron irradiation damage and low contrast. In this doctoral thesis techniques were developed to address some of those issues and successfully characterize these materials at high resolution. These techniques were demonstrated on graphene flakes, DNA/magnetic beads and a number of water containing biomaterials. The details of these studies are given below. A TEM based method was presented for thickness characterization of graphene flakes. For the thickness characterization, the dynamical theory of electron diffraction is used to obtain an analytical expression for the intensity of the transmitted electron beam as a function of thickness. From JEMS simulations (experiments) the absorption constant λ in a low symmetry orientation was found to be ~ 208 nm (225 ± 9 nm). When compared to standard techniques for thickness determination of graphene/graphite, the method has the advantage of being relatively simple, fast and requiring only the acquisition of bright-field (BF) images. Using the proposed method, it is possible to measure the thickness change due to one monolayer of graphene if the flake has uniform thickness over a larger area. A real-space TEM study on magnetic bead-DNA coil interaction was conducted and a statistical analysis of the number of beads attached to the DNA-coils was performed. The average number of beads per DNA coil was calculated around 6 and slightly above 2 for samples with 40 nm and 130 nm beads, respectively. These results are in good agreement with magnetic measurements. In addition, the TEM analysis supported an earlier hypothesis that 40 nm beads are preferably attached interior of the DNA-coils while 130 nm beads closer to the exterior of the coils. A focused ion-beam in-situ lift-out technique for hydrated biological specimens was developed for cryo-TEM. The technique was demonstrated on frozen Aspergillus niger spores which were frozen with liquid nitrogen to preserve their cellular structures. A thin lamella was prepared, lifted out and welded to a TEM grid. Once the lamella was thinned to electron transparency, the grid was cryogenically transferred to the TEM using a cryo-transfer bath. The structure of the cells was revealed by BF imaging. Also, a series of energy filtered images was acquired and C, N and Mn elemental maps were produced. Furthermore, 3 Å lattice fringes of the underlying Al support were successfully resolved by high resolution imaging, confirming that the technique has the potential to extract structural information down to the atomic scale. The experimental protocol is ready now to be employed on a large variety of samples e.g. soft/hard matter interfaces.

Ion irradiation of tetrahedral amorphous carbon (ta-C) thin films induces a carbon phase transformation from the electrically insulating sp3 hybridization into the conducting sp2 hybridization. In this work, a detailed study on the electrical resistivity and the microstructure of areas, irradiated with several ion species at 30 keV energy is presented. Continuous ion bombardment yields a drastic drop of the resistivity as well as significant structural modifications of the evolving sp2 carbon phase. It is shown that the resistivity lowering can be attributed to the degree of graphitization in the film. Furthermore, the structural ordering processes are correlated with the ion deposited energy density. It is therefore revealed that the ion-induced phase transformation in ta-C films is a combination of sp3-to-sp2 conversion of carbon atoms and ion-induced ordering of the microstructure into a more graphite-like arrangement. All experiments were done with focused ion beam (FIB) systems by applying FIB lithography of electrical van-der-Pauw test structures. FIB lithography on ta-C layers is presented as a fast and easy technique for the preparation of electrically active micro- and nanostructures in an insulating carbon matrix.

Nowadays, the systems that allow simultaneous employment of both focused electron and ion beams are very important tools in the field of micro- and nanotechnology. In addition to imaging and analysis, they can be used for lithography, which is applied for preparation of structures with required shapes and dimensions at the micrometer and nanometer scale. The first part of the thesis deals with one lithographic method – focused electron or ion beam induced deposition, for which a suitable adjustment of exposition parameters is searched and quality of deposited metal structures in terms of shape and elemental composition studied. Subsequently, attention is paid also to other types of lithographic methods (electron or ion beam lithography), which are applied in preparation of etching masks for the subsequent selective wet etching of silicon single crystals. In addition to optimization of mentioned techniques, the application of etched silicon surfaces for, e.g., selective growth of metal structures has been studied. The last part of the thesis is focused on functional properties of selected 2D or 3D structures.