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Gallium oxide (Ga2O3) has been the subject of extensive research activity due to its ultrawide bandgap and large breakdown field, which make it promising for next-generation applications in deep ultraviolet detection and power electronics. β-Ga2O3 is the most thermally stable and well-studied polymorph of Ga2O3. However, during the past decade, the metastable orthorhombic κ-Ga2O3 has emerged as an equally impressive candidate material owing to its high crystal symmetry and ferroelectric and spontaneous polarization properties. Several studies have reported the growth and characterization of κ-Ga2O3 films using different epitaxial growth methods. However, the existing literature still lacks reports on the processing of this material for future device applications. Therefore, in this thesis, we investigate the effects of high-temperature treatment and plasma exposure on the structural and optical properties of mist chemical vapor deposition (mist-CVD)-grown κ-Ga2O3 films. Using high-temperature X-ray diffraction (HT-XRD), we show that the films remain phase-pure up to an annealing temperature of 800 ˚C, after which β-phase peaks start to appear and eventually show a complete transition to β-Ga2O3 at 875 ˚C. Additionally, we show using detailed high-resolution transmission electron microscopy (HRTEM) and XRD analyses that annealing at 700 ˚C in ambient air is effective in improving the crystal quality of the κ-Ga2O3 layer by relieving in-plane strains and epitaxial stacking faults. Moreover, since dry etching is needed for the anisotropic patterning of materials for device applications, it is necessary to investigate the effects of plasma exposure on the near-surface properties of the material in order to keep its damage to a minimum. Therefore, we studied the impacts of plasma exposure during dry etching on the chemical structure, crystallinity, and optical properties of κ-Ga2O3 by using a variety of characterization methods. We observed how varying the etching parameters using BCl3/Ar can affect the near-surface properties of the material, which play a key role in modifying the performance of future devices. Specifically, we found that both RIE/ICP power and BCl3/Ar ratio can influence the surface stoichiometry and the concentration of native defect density, which affect the material’s structural and optical properties. Additionally, we reported for the first time on κ-Ga2O3 ICP-RIE process optimization using a BCl3/Ar gas mixture. By tuning the process parameters, the optimized recipe had a high etch rate of 130 nm/min, showed a surface roughness reduction of 56%, and produced vertical sidewall profiles for ridge device structures.

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Condition based monitoring of Thermal Protection Systems (TPS) is necessary for safe operations of space shuttles. In the current research Terahertz radiation (T-ray) has been used to detect mechanical and heat induced damages in TPS tiles. Voids and cracks inside the foam tile are denoted as mechanical damage while property changes due to long and short term exposures of tiles to high heat are denoted as heat induced damage.Ultrasonic waves cannot detect cracks and voids inside the tile because the tile material (silica foam) has high attenuation for ultrasonic energy. Instead, electromagnetic terahertz radiation can easily penetrate into the foam material and detect the internal voids although this electromagnetic radiation finds it difficult to detect delaminations between the foam tile and the substrate plate. Thus these two technologies are complementary to each other for TPS inspection.Ultrasonic and T-ray field modeling in free and mounted tiles with different types of mechanical and thermal damages has been the focus of this research. Shortcomings and limitations of FEM method in modeling 3D problems especially at high-frequencies has been discussed and a newly developed semi-analytical technique called Distributed Point Source Method (DPSM) has been used for this purpose.A FORTRAN code called DPSM3D has been developed to model both ultrasonic and electromagnetic problems using the conventional DPSM method. DPSM has been extended from ultrasonic applications to electromagnetic to model THz Gaussian beams, multilayered dielectrics and Gaussian beam-scatterer interaction problems. Since the conventional DPSM has some drawbacks, to overcome it two modification methods called G-DPSM and ESM have been proposed.The conventional DPSM in the past was only capable of solving time harmonic (frequency domain) problems. In this research DPSM has been extended to model DPSM transient problems. This modified technique has been denoted as t-DPSM.Using DPSM, scattering of focused ultrasonic fields by single and multiple cavities in fluid&solid media is studied. A comparison between the radiation forces generated by the ultrasonic energies reflected from two small cavities versus a single big cavity is also carried out.

Currently, it is very challenging to accurately monitor the response of patients to radiation therapy over the course of treatment. The initial response to ionizing radiation occurs in the cells at a molecular level, and effects of the response are not typically noticeable on short time scales. Surface-enhanced Raman Spectroscopy, or SERS, has proven to be a useful technique in the analysis of tissues and cells at a molecular level. Specifically, the use of targeted SERS probes allows for the detection of specific proteins on the cell membrane. The work presented here looks to assess the feasibility of using targeted SERS probes and two-dimensional SERS microscopy to measure the response of tumour cells to ionizing radiation, by identifying changes in the distribution of membrane proteins following exposure to clinically relevant doses of ionizing radiation (≤ 60Gy). Two different types of targeted SERS probes were investigated, based on the work of Grubisha et al. ([1]; Type I) and Qian et al. ([2]; Type II), both containing a gold nanoparticle core. In a simplified cellular experiment, biotin on the surface of biotinylated OVCAR5 cells was targeted with streptavidin-SERS probes, and the Type-II SERS probes showed the most promising results. However, SERS maps still provided less characteristic spectral signal than expected, and challenges remain in the development of a reproducible cellular imaging technique. Despite difficulties in cellular imaging, the functionality of the Type-II SERS probes was verified separately, using gold slides with a biotin monolayer in place of cells. Following verification, the SERS intensities provided by differently sized clusters of the SERS probes were characterized. To begin, both SERS maps and scanning electron microscope (SEM) images of gold slides were acquired after incubation with Type-II SERS probes for multiple times (1hr, 2hr, 3hr, 12hr). Data analysis of the SEM images provided a measure of the physical distribution of the SERS probes on the surface of the slide, while analysis of the SERS maps provided information about the spectral distribution of the probes. By relating the information provided by the SEM images and SERS maps, a simple polynomial relationship between SERS intensity and the number of clustered SERS probes providing the enhancement was determined, providing a framework for quantifiable SERS imaging. Finally, an independent experiment was devised to ensure that exposure to clinically relevant doses of ionizing radiation would affect the ability of the targeted protein to bind to SERS probes, thus leading to measurable differences in SERS maps of irradiated and unirradiated cells. A series of experiments utilizing the enzyme-linked immunosorbant assay (ELISA) was performed to test the effect of ionizing radiation-induced damage on the ability of streptavidin to bind to biotin, and the results confirmed that a noticeable reduction in binding could be detected at doses as low as 10 Gy. The results of this work demonstrate that following the development of a suitable cell/SERS probe incubation technique, Type-II SERS probes would be appropriate for use in quantifiable SERS imaging. Also, it is suggested that a measurable change in protein function will be present when comparing SERS maps of control cells to those of cells irradiated to clinically relevant doses. / Graduate

Zirconium and its alloys have been used extensively in both light and heavy water reactors where neutron irradiation is known to cause microstructural evolution, leading to degradation of mechanical properties and dimensional instabilities. Dimensional instabilities due to irradiation growth are particularly crucial for Zr alloy Excel which is the proposed candidate material for the conceptual CANDU-Super Critical Water Cooled Reactors (SCWR) pressure tube. This study employs the in-situ ion irradiation technique and transmission electron microscopy to investigate the irradiation induced microstructural evolution in Zr and Zr alloy Excel. The current study is presented as a manuscript format dissertation comprised of five manuscript chapters. Chapter 3 reports the formation of irradiation induced prismatic defects directly from cascade collapse in pure Zr at low dose (0.008 dpa) in a temperature range of 300oC-500oC. The morphology and yield of these defects are found to be temperature and dose dependent. In Chapter 4, irradiating Zircaloy-2 under similar conditions to pure Zr, reveals that nucleation rate of small prismatic loops increases, whereas their growth is suppressed which indicates that these defect clusters are not only temperature dependent but also impurity dependent. Chapters 5, 6 and 7 report the irradiation induced microstructural changes at various temperatures up to a dose of 10 dpa, in several microstructures of Zr alloy Excel, achieved by different solution treatments. The major focus of these experimental studies was the formation of <c>-component loops in α-phase; decomposition of β-phase; and irradiation induced microchemical changes. It was found that nucleation and growth of <c>-component loops is strongly dependent on irradiation temperature, parent microstructure, and presence of alloying elements. <c>-component loops nucleate above a threshold incubation dose which decreases with an increase of irradiation temperature. Energy dispersive X-ray spectroscopy (EDS) mapping on irradiated microstructures revealed the formation of small Sn clusters in α-phase which have a significant effect on the morphology of <c>-component loops. Fe plays an important role in the nucleation of <c>-component loops, as it distributes itself during irradiation either from β-phase or from pre-existing secondary phase precipitates in α-phase. Furthermore irradiation induced decomposition of β-phase was observed in the form of ω-phase precipitation and irradiation induced clustering of alloying elements. / Thesis (Ph.D, Mechanical and Materials Engineering) -- Queen's University, 2013-12-31 23:50:30.352

Une des limitations du fonctionnement des grandes chaines lasers de puissance telle que le Laser MegaJoule, est la problématique de l’endommagement laser des composants optiques. Différents phénomènes physiques qui dépendent à la fois des propriétés des matériaux, de leurs conditions de fabrication/ préparation et des paramètres d’irradiation laser peuvent conduire à un amorçage de dommages sur la surface ou dans le volume, qui vont croître lors d’irradiations successives. Ce phénomène limite la montée en puissance, affecte la durée de vie des composants optiques et le coût de maintenance des chaînes laser. Il peut également être à l’origine de graves problèmes de sécurité. Pour remédier à cette croissance des dommages et augmenter la durée de vie des composants en silice, un procédé laser dit de «stabilisation » est étudié dans le cadre de cette thèse, l’objectif étant de traiter les dommages pour arrêter leur croissance sous tirs répétés afin de recycler les optiques endommagées. Ce processus consiste en une fusion, suivie d’une évaporation locale, par dépôt d’énergie localisé par un faisceau laser CO2, de la zone fracturée de silice. Nous nous sommes intéressés particulièrement à la stabilisation de dommages laser sur silice par un procédé de micro-usinage par laser CO2 dans le but de traiter des dommages de dimensions millimétriques. Cette technique est basée sur une micro-ablation rapide de la silice durant laquelle le faisceau laser est balayé à la surface du composant afin de former un cratère de forme ajustable (typiquement conique) englobant le site endommagé. Un banc d’expérimentations a ainsi été mis en place à l’Institut Fresnel pour développer et étudier ce procédé. Différents travaux numériques et expérimentaux ont également été menés pour valider et optimiser la technique. Nos travaux ont montré l’efficacité de ce procédé de micro-usinage par laser CO2 pour arrêter la croissance de dommages de plusieurs centaines de microns de largeur et de profondeur. Pour parvenir à cet objectif nous nous sommes appuyés sur la modélisation des phénomènes physiques mis en jeu lors des expériences de stabilisation en utilisant le logiciel de simulation multi-physique COMSOL. D’une part, le modèle thermique, développé au cours de cette thèse, permet de calculer la distribution de température dans le matériau pendant le tir laser avec ou sans mouvement du faisceau. Combinées à une approche thermodynamique, ces simulations thermiques permettent de décrire les transformations de la silice lors de l’irradiation afin de prédire la morphologie des cratères formés dans le verre. D’autre part, la partie mécanique du modèle permet de simuler la position et la valeur des contraintes résiduelles, générées dans le matériau autour du cratère CO2, lors de l’élévation de température suivie du refroidissement rapide. D’autres expériences concernant le traitement de fractures liées au polissage, ou des défauts de fabrication de réseaux de silice sont également traités dans ce manuscrit. / One limitation of the operation of large power lasers chains such as Laser MegaJoule, is the issue of laser damage of optical components. Different physical phenomena which depend on both the properties of materials, their conditions of manufacture / preparation and laser irradiation parameters can lead to damage initiation on the surface or in the volume, which will grow under successive irradiation. This effect limits the output power, affects the lifetime of the optical components and the maintenance cost of the laser. It can also cause serious safety problems. To address this issue and increase the lifetime of fused silica components, a laser process called "stabilization" is studied in this thesis, the aim being to treat the damage sites to stop their growth under repeated pulses for recycling damaged optics. This process consists of melting, followed by local evaporation by localized energy deposition by a CO2 laser beam of the damage site. We focused particularly on the stabilization of silica components by a micromachining process using a CO2 laser in order to treat millimeter size damages. This technique is based on fast micro-ablation of the silica during which the laser beam is scanned on the component surface to form an adjustable form of crater (typically conical) including the damaged site. A bench of experiments has been set up at the Fresnel Institute to develop and study this process. Various numerical and experimental works were also conducted to validate and optimize the technique. Our work has shown the efficiency of this micro-machining process by CO2 laser to stop the growth of damage to several hundred microns wide and deep. To achieve this goal we relied on modeling of physical phenomena involved in stabilization experiments using the COMSOL Multiphysics simulation software. First, the thermal model developed in this thesis is used to calculate the temperature distribution in the material during laser irradiation with or without movement of the beam. Combined with a thermodynamic approach, these thermal simulations can describe the transformation of silica during irradiation and predict the morphology of craters formed in the glass. Secondly, the mechanical part of the model can simulate the position and value of residual stress generated in the material around the crater after the temperature rise followed by rapid cooling. Other experiments on the treatment of fractures related to polishing on silica surfaces, or manufacturing defects on silica gratings are covered in this manuscript.