L’effet Hall quantique (EHQ) apparaissant dans des gaz bidimentionnels d’électrons places à basse température et sous fort champ magnétique a révolutionné la métrologie des résistances depuis sa découverte en 1980 par Klaus von Klitzing. Cet effet apporte une représentation de l’ohm uniquement basé sur la constante de Planck et la charge de l’électron. En 2004, le graphène, un arrangement purement bi-dimensionnel d’atomes de carbone en nid d’abeille, dans lequel les porteurs de charge se comportent comme des fermions de Dirac, a permis de mettre à jour une nouvel effet Hall quantique. Du point de vue de la métrologie des résistances l’EHQ dans le graphène est très prometteur car plus robuste que celui apparaissant dans les hétérostructures semi-conductrices. Ceci pourrait mener à la création d’un étalon de résistance plus pratique, fonctionnant à plus haute température et plus faible champ magnétique ce qui serait un avantage notable pour une dissémination accrue d’un étalon de résistance précis vers les acteurs industriels. Dans ce manuscrit une étude complète de l’impact des défauts linéaires, omniprésent dans le graphène crû par dépôt chimique en phase vapeur sur métal, dans le régime d’effet Hall quantique est menée. Nous avons montré que ces défauts linéaires mènent à des processus de dissipation non-conventionnels qui viennent altérer la quantification de la résistance de Hall. Cette étude pointe vers l’utilisation de monocristaux pour les prochaines investigations du graphène CVD pour une application en métrologie des résistances. La deuxième partie de ce manuscrit est dédiée à l’étude du graphène crû par dépôt chimique en phase vapeur sur carbure de silicium. Nous avons comparé précisément la résistance de Hall d’un échantillon de graphène entre 10 et 19 T à la température de 1.4 K avec celle donnée par un étalon de résistance en GaAs/AlGaAs avec une incertitude relative de ( -2 ± 4 ) × 10⁻¹⁰. Pour la première fois un étalon de résistance en graphène a pu fonctionner dans les mêmes conditions de température et de champs magnétique que celui fabriqué en GaAs/AlGaAs et de plus sur un intervalle de champ magnétique plus de dix fois plus grand. Nous avons également étudié les processus de dissipation apparaissant dans cet échantillon de graphène. Cette étude montre que la longueur de localisation des porteurs de charge sature à une valeur proche de l’extension de la fonction d’onde et ce sur une grande plage de champs magnétique, ce qui soulève des questions intéressantes concernant le désordre présent dans ce type de graphène. Finalement dans un second échantillon provenant de la même technique de fabrication nous avons comparé précisément la résistance de Hall de l’échantillon de graphène avec celle d’un étalon de résistance en GaAs/AlGaAs. Il apparait que la résistance de Hall dans l’échantillon de graphène est quantifié avec une précision métrologique pour des champs magnétiques allant jusqu’à 3.5 T, des températures atteignant 9 K et reste dans un état non dissipatif jusqu’à des courants de 500 µA. Ceci ouvre une voie directe à la réalisation d’étalons quantiques de résistance réalisés en graphène. / The quantum Hall effect (QHE) observed in two dimensional electron gas placed at low temperature and under a strong perpendicular magnetic field, has revolutionized the resistance metrology since its discovery in 1980 by Klaus von Klitzing. It provides a representation of the ohm based on the Planck constant and the electron charge only. In 2004, graphene, a purely two dimensional arrangement of carbon atoms in an honeycomb lattice, where the charge carriers behave as Dirac fermions, has revealed a new flavor of the QHE. From the metrological point of view the QHE in graphene is very promising since it is much more robust than the effect appearing in conventional semiconductors and it could lead to a more convenient resistance standard operating at higher temperature and lower magnetic induction which is an advantage for a broader dissemination of a precise standard towards industrial end-users. In this manuscript, a complete study about the impact in the QHE regime of line defects such as wrinkles or grain boundaries, ubiquitous in graphene grown by chemical vapor deposition on metal is treated. We show that these line defects lead to a non conventional dissipation mechanism that jeopardize the quantum Hall effect accuracy pointing to the use of wrinkle-free monocrystals for further metrological studies. The second part of my manuscript is focused on monolayer graphene grown by chemical vapor deposition on silicon carbide. We precisely compared the Hall resistance of the graphene sample from 10 T to 19 T at the temperature of 1.4 K with a GaAs/AlGaAs resistance standard with a relative uncertainty of ( -2 ± 4 ) × 10⁻¹⁰. For the first time a graphene-based standard was able to operate in the same temperature and magnetic field conditions as semiconductor-based one, furthermore, on a magnetic range more than ten times larger. We thus made a careful study of the dissipation mechanisms taking place in this sample and measured precisely the magnitude of the localization length in the QHE regime that saturate interestingly at the extension of the charge carrier wavefunction itself, opening interesting questions about the close link between Hall quantization and localization physics in graphene grown on SiC. Finally in a second sample grown using the same technique we precisely compared the Hall resistance of the graphene sample and a GaAs/AlGaAs resistance standard that turned out to be in agreement at the metrological level for magnetic fields as low as 3.5 T current as high as 500 µA and temperature as high 9 K. This paves the way for the realization of easy to use quantum Hall resistance standards made out of graphene.

L'objectif de ce travail de thèse est de démontrer le potentiel des calorimètres métalliques magnétiques pour la spectrométrie bêta via une mesure du spectre du 63-Ni. Ce nucléide fait partie des émetteurs bêta pour lesquels la théorie est connue et les calculs crédibles. Nous proposons une méthode d'observation expérimentale du spectre, à basse énergie surtout, permettant de valider les calculs théoriques.Un traitement des données spécifique à l'établissement d'un spectre continu a été établi et optimisé, prenant en compte les paramètres d'une mesure cryogénique avec un calorimètre métallique magnétique et les exigences de la spectrométrie bêta.Deux types de sources ont été réalisés, un dépôt sous forme de sel de nickel à partir d'une goutte séchée de solution de NiCl2 et un dépôt métallique de nickel issu d'une électrodéposition. Les sources électrodéposées se sont révélées être le type de source adéquate pour la spectrométrie du 63-Ni.Les performances des calorimètres métalliques magnétiques, parmi lesquelles le fort rendement de détection ou le faible seuil en énergie, permettent d'obtenir des résultats suffisamment précis pour la validation expérimentale des calculs théoriques. / The aim of this thesis is to demonstrate the potential of metallic magnetic calorimeters for beta spectrometry by measuring the spectrum of 63-Ni. This nuclide is one of the beta emitters for which theory is well-known and calculation reliable. We propose a method for experimental observation, especially at low energies, which allows to validate the theoretical calculation.A dedicated data analysis has been established and optimized. It takes into account the parameters of a cryogenic measurement and also the specific requirements of beta spectrometryTwo types of sources have been realized, a deposit of nickel salt from a dried drop of a solution of NiCl2 and a metallic electroplated source of Ni. The electroplated sources turn out to be the appropriate type of source for 63-Ni spectrometry.The performances of metallic magnetic calorimeters, such as high detection efficiency and low energy threshold, lead to results precise enough to validate experimentally the theory.

Cette thèse porte sur l'endommagement laser de composants optiques en silice amorphe en régime nanoseconde. Ce matériau diélectrique est l'un des plus couramment utilisés en optique et notamment sur des installations laser de haute énergie telles que le Laser MégaJoule. Afin de garantir le fonctionnement nominal d'une installation, l'endommagement laser des composants optiques doit être compris et maîtrisé. Ce phénomène induit une modification irréversible du matériau modifiant la propagation du faisceau. Dans le régime nanoseconde, l'endommagement laser de la silice est corrélé à la présence de défauts précurseurs qui sont une conséquence de la synthèse et du polissage des composants. L'interaction de ces précurseurs avec le laser va dépendre des caractéristiques de ce dernier. Une première étude est consacrée à la métrologie des impulsions utilisées en laboratoire pour étudier l'endommagement laser. Une seconde étude porte sur les mécanismes d'amorçage des dommages sur la face de sortie des composants optiques faits de silice. Une dernière partie porte sur l'influence de la propagation non linéaire sur l'endommagement surfacique et volumique des composants épais faits de silice. / In this thesis, laser-induced damage phenomenon in fused silica components is investigated in the nanosecond regime. This material is one of the most widely used in optics, particularly on high-energy laser facilities such as the Laser MégaJoule. In order to ensure the nominal operation of this kind of laser facility, laser-induced damage on optical components has to be understood and controlled. This phenomenon consists in an irreversible modification of the material. In the nanosecond regime, laser-induced damage is tightly correlated to the presence of precursor defects which are a consequence of the synthesis and the polishing of the components. The interaction between these precursor defects and the laser pulses strongly depends on the laser characteristics. The first study focuses on the metrology of the laser beam used in laboratory to study laser-induced damage. The second one consists in a parametric study of the initiation mechanism on the rear surface of fused silica components. The last part deals with the influence of nonlinear propagation on laser induced damage on the surface and in the volume of thick fused silica samples.

Global planarization is one of the major demands of the semiconductor industry. Chemical mechanical polishing (CMP) is the planarization method of choice use to achieve the required stringent tolerances essential for successful fabrication of next generation Integrated Circuits (IC). The predominant reason for CMP defects is the shear and normal stresses during polishing to which the material is subjected. Understanding the process of CMP and factor that contribute to overall stress addition during polishing requires an approach that encompasses all the four major categories of variables, namely: a) machine parameters, b) material properties, c) polishing pad characteristics, and d) polishing slurry performance. In this research, we studied the utilized in-situ technique involving acoustic emission (AE) signal monitoring and coefficient of friction (COF) monitoring using a CETRTM Bench Top CMP Tester to evaluate the impact of variation in machine parameters on the CMP process. The mechanical and tribological properties of different candidate materials have been evaluated bring potential challenges in their integration to the fore. The study also involves destructive and non destructive testing of polishing pads performed for characterization and optimization of polishing pad architecture. Finally, the investigation concludes proposing novel nanoparticle CMP slurry which has a predominant chemical component in its polishing mechanism. It was found that the decrease in the mechanical shear and normal loading by: a) operating the process in the low stress regime, b) using potential materials that are mechanically stronger, c) using polishing pads with lesser variation in specific gravity and with a surface that is has its mechanical properties fine tuned to those of the wafer, and d) deploying polishing slurry with a significant chemical component mechanical removal, are some of the approaches that can be employed to meet the future challenges of the CMP process and reduce the defect associated with it.

[pt] Não obstante os sofisticados avanços em tecnologias ópticas, ainda não existem fontes de luz artificial capazes de simular de forma adequada a luz do dia natural. Alcançar um padrão de iluminação como este representará uma redução nos custos de produção, em função de retrabalhos gerados por avaliações visuais pouco confiáveis, e nas divergências comerciais relacionadas a produtos que têm como característica de controle a cor, tais como artigos têxteis, gráficos, de merchandising etc. A presente pesquisa de mestrado em metrologia relaciona-se à avaliação metrológica das fontes luminosas e cabines de iluminação disponíveis no mercado e à sua adequação às normas que definem especificações técnicas, com o propósito de estimular introdução de inovação tecnológica em novos desenvolvimentos industriais capazes de melhorar o desempenho desses aparatos. A pesquisa contribui, também, com o desenvolvimento de um diagnóstico do acervo de normas técnicas disponíveis aplicáveis à padronização de sistemas de iluminação; investigação de lâmpadas fluorescentes usualmente utilizadas como simuladores de luz do dia e avaliação metrológica de cabines de iluminação disponíveis no mercado. Em particular, medições foram realizadas em um sistema espectroradiométrico de alta definição, que utiliza um monocromador duplo com capacidade de dispersão do feixe de 2 nm/mm. Ensaios e análises de repetitividade e reprodutibilidade conduzidas no sistema de medição espectroradiométrico permitiu quantificar a variabilidade associada a cada lote de fabricação dos simuladores de luz do dia, comercializados na forma de lâmpadas fluorescentes disponíveis no mercado nacional. Caracterizada a variação da distribuição espectral ao longo do eixo das fontes luminosas investigadas (lâmpadas) foi possível desenvolver uma análise do impacto induzido na uniformidade da iluminação obtida em cabines industrializadas, assim definindo um fator de diferenciação de interesse técnico e comercial. A pesquisa revelou que nenhum dos simuladores de luz do dia testados atingiu os requisitos mínimos estabelecidos para a comparação visual de cores, quando avaliados com base em normas e práticas internacionais. Foram ainda realizadas medições para se verificar a influência dos elementos construtivos das cabines na distribuição espectral de potência na área de avaliação. Fundamentado nas 1578 medições realizadas em condições laboratoriais que simulam ambientes industriais, a pesquisa comprova que alterações nas características construtivas das cabines possuem impacto no resultado da classificação das distribuições espectrais de potência, criando assim uma condição facilitadora para que as especificações normativas sejam atingidas, mesmo com a utilização de lâmpadas fluorescentes disponíveis no mercado e de preço reduzido. / [en] Notwithstanding the complex advances in optical technologies, there are still no artificial light sources capable of adequately simulating the natural daylight. Reaching such a lighting standard will represent a reduction of the production costs, in view of the rework caused by not so reliable visual evaluations, and of the commercial conflicts related to products that have colour as one of their control characteristics, such as textile, graphics and merchandising articles. The present Master degree metrology research is related to the metrological evaluation of the lighting sources and light booths available in the market (commercially available), and to their conformity to the technical specifications standards, aiming to stimulate the introduction of technological innovation to new industrial developments eligible to enhance the performance of these apparatus. The research has also contributed to the development of a diagnosis of the collection of the existing technical standards applied to the standardisation of lighting systems; to the investigation of fluorescent lamps generally used as daylight simulators, and to the metrological evaluation of light booths available in the market (commercially available). Particularly, analyses were done with a highly precise spectroradiometric system that uses a double monochromator with capacity for beam dispersion of 2 nm/mm. Tests and analyses on repeatability and reproducibility made with the spectroradiometric measurement system let to quantify the variety associated with each manufactured set of daylight simulators, commercialised as fluorescent lamps available at the local market. Having the spectral distribution determined throughout the axis of the studied lighting sources (lamps) it was possible to develop an analysis of the impact caused at the lighting uniformity obtained for industrial light booths, and so, specifying a distinctive factor technically and commercially interesting. The research revealed that, when evaluated considering the international practices and standards, none of the daylight simulators tested achieved the minimum requirement indicated for the visual comparison of colours. In addition, measurements were done to verify the influence of the light booths building pieces at the power spectral distribution within the evaluation area. Based on 1578 measurements done at laboratorial conditions simulating industrial environment, the research proves that changes in the building characteristics of the light booths produce an impact at the result of the power spectral distribution classification, creating, thus, a smooth condition for the attendance of the standards specifications, even when using low-cost fluorescents lamps available in the market.

[pt] A presente dissertação apresenta o desenvolvimento de um transdutor de pressão de alta sensibilidade, desenvolvido para aplicações biomédicas. O transdutor é baseado em um sensor de magnetoimpedância gigante (MIG), anteriormente desenvolvido, pelo Laboratório de Biometrologia da PUC-Rio. O conhecimento a cerca das principais características do fenômeno MIG serviu de guia para as ações que foram tomadas, a fim de se estabelecer uma configuração que apresentasse maior sensibilidade ao transdutor. Mesmo que algumas dificuldades encontradas, principalmente devidas a características acústicas não levadas em consideração, apontem para a necessidade de aperfeiçoamentos, com a configuração desenvolvida no presente trabalho já é possível obter o registro do pulso arterial carotídeo. Comparações entre o transdutor ora desenvolvido e com outros transdutores de pressão existentes no mercado também destinados a aplicações biomédicas, apontam para uma sensibilidade do transdutor ora desenvolvido de magnitude igual ou mesmo superior aos convencionais. / [en] This dissertation presents a high sensitivity pressure transducer, developed for biomedical applications. The transducer is based on a Giant Magnetoimpedance (GMI) sensor previously developed at the Laboratory of Biometrology of PUC-Rio. Knowing the main characteristics of the phenomenon and of the GMI strips used, the configuration which should yield the highest possible sensitivity has been implemented. Even though some enhancements in the acoustic characteristics of the transducer are still necessary, it was already possible to record the carotid arterial pulse. Comparing the transducer herein presented with other pressure transducers also destined to biomedical applications, it already has a sensitivity of the same order of magnitude or even higher.

I present several new methods for the characterisation of ultrashort pulses using interferometry. A generalisation of the concatenation algorithm for spectral shearing interferometry enables interferograms taken at multiple shears to be combined. This improves the precision of the reconstructed phase in the presence of detector noise, and enables the relative phase between disjoint spectral components to be obtained without decreasing the spectral resolution. The algorithm is applied to experimental data from two different implementations of spectral shearing interferometry for ultrashort optical pulses. In one, the shears are acquired sequentially, and in the other they are acquired simultaneously. I develop a form of spatio-temporal ultrashort pulse characterisation which performs both spatial and spectral shearing interferometry simultaneously. It requires a similar geometrical setup to common implementations of spectral phase interferometry for direct electric-field reconstruction, but provides complete amplitude and phase characterisation in time and one spatial dimension. I develop the theory of lateral shearing interferometry for spectrally resolved wavefront sensing of extended ultraviolet and soft x-ray pulses generated using high-harmonic generation. A comprehensive set of wavefront measurements of harmonics 13-25 in Krypton show good agreement with theory, validating the technique. I propose and numerically demonstrate quantum-path interferometry mediated by a weak control field for high harmonic generation. This is a general technique for measuring the amplitude and relative phases of each contributing quantum path. The control field perturbatively modulates the phase of each path. The differing sensitivity of each path to the parameters of the control field allows their contributions to be distinguished from one another.

Laser processing has the advantage of minimal sample contact and thus little tool wear over time compared to conventional machining. However, this leads to the difficulty of real-time depth monitoring and control. To help understand the process and achieve automation of laser micromachining, a coherent imaging technique adapted from spectral domain optical coherence tomography (SD-OCT) is applied “inline”with a machining laser to monitor the depth changing information. The axial resolution of the inline coherent imaging (ICI) system is 7–8 microns and the acquisition rate is up to 230 kHz. The capture time is as low as 1.5 microseconds. 3D laser machining usually requires ultrafast lasers and homogeneous materials. With ICI, a feedback system is developed for 3D sculpture suitable even for heterogeneous materials without any sophisticated material characterization. 3D patterns with sizes up to 1 mm × 1 mm × 0.2 mm are sculpted in bone and wood with a ps UV laser. 3D patterns with sizes up to 6 mm × 6 mm × 2 mm are sculpted in bone with a CW IR laser. Many laser applications require high scan speed facilitated by scanning optics. The versatility of ICI is also demonstrated in a galvo-telecentric beam delivery system. ICI is used in a process of trench (as long as 10 mm) etching of steel to monitor the intrapulse and interpulse morphology changes as well as the sweep-to-sweep (up to 36 sweeps) depth changes. High scan speed (up to 375 mm/s) trench etching of silicon are also monitored and the parameter space is explored without destructive post-processing. Motion during imaging capture time (>1.5 microseconds) may cause contrast degradation. To reduce the motion artifacts, preliminary experiments on stroboscopic ICI based on a kHz pulse repetition rate femtosecond laser are described. By “sampling” the motion of the machining front discretely with a “sampling time” as short as the imaging pulse duration, our results demonstrate that stroboscopic ICI is a promising way to improve the ICI contrast against motion artifacts. / Thesis (Master, Physics, Engineering Physics and Astronomy) -- Queen's University, 2014-04-30 13:56:35.793

Possessing a wide band gap and large break down field, gallium nitride (GaN) is of interest for a host of high power, high frequency applications including next generation cellular base stations, advanced military radar, and WiMAX networks. Much of this interest stems from the continued development of the AlGaN/GaN high electron mobility transistor (HEMT) that is capable of operating at sizable power densities and switching speeds. The same fields responsible for this performance, however, also elicit acute device heating and elastic loads. These induced thermomechanical loads limit both performance and reliability thus necessitating continued improvement in the management and characterization of the coupled environments. In response, this study establishes a new implementation of Raman spectroscopy capable of simultaneously measuring the operational temperature and stress in a HEMT using only the Stokes response. First, the linewidth (FWHM) of the Stokes signal is utilized to quantify the operating temperature of a HEMT independent to the influences of stress. Second, a new method, incorporating the use of the linewidth and peak position in tandem, is developed to estimate the biaxial thermoelastic stress that arises during device operation. With this capability, the HEMT's resultant load is assessed, highlighting the large role of the residual stress on the total mechanical state of the device. Subsequently, this same linewidth is leveraged to identify the distinct effect that electrical carriers have on the thermally relevant decay of longitudinal optical phonon modes. Further investigation of the lattice transport then concludes the study by way of an analytical treatment describing the significant influence of interfacial disorder on the energy transport at GaN/substrate boundaries.

Machines operating in dusty environments, such as mining and civil works, are prone to premature failure, leading to production losses. To address this problem, this research project examines the interaction between solid contaminants and the bearing micro-geometry, in lubricated surface contacts. In particular, it seeks to identify anti-wear additives that are effective in reducing wear under abrasive conditions, making machine elements more dirt tolerant. In general, the influence of antiwear additive is so small that it is difficult to isolate it. Manufactures often make claims about their antiwear products, which are difficult to verify. Hence, there is a need to characterising the antiwear additives available with a well-defined parameter, making it easier for consumers to compare the efficacy of various additives, and be able to select the most suitable additive for a given environment. Effect of micro-geometry parameters such as radial clearance, out-of-roughness and surface roughness was examined and a Film Shape Factor (FSF) – also termed gamma ratio – has been proposed for ensuring adequate separation of journal bearings operating in hydrodynamic lubrication regime, where the out-of-roundness values are higher than the surface roughness values. In this research, an experimental study has been conducted on journal bearings, to examine the influence of five antiwear additives on the bearing wear and micro-geometry. The test additives were provided by the industry partner without revealing their chemical identity or composition; however, these included some of the most commonly used antiwear additives. The tests were performed under three conditions: pure base oil, base oil containing contaminants, and base oil containing contaminants treated with five different additives. The experiments were aimed at choosing one wear measuring technique that evaluates the performance of an individual additive reliably, and based on this technique the additives were characterised. To achieve these objectives, a multi-wear parameter approach (MWPA) was developed, which employed three main wear measurement methodologies, i.e. weight loss, micro-geometry and particle counts –to examine the effect of the antiwear additives. Minimum oil film thickness was also measured to study the lubrication status in the bearing contacts. The MWPA helped in comparing different wear measuring methods, and in selecting the most reliable one. This approach also helped in developing short duration wear tests, thereby saving time, while still getting reliable results without repeating these. Wear experiments were performed on seven sets of bronze bearings and steel sleeve shafts. The test contaminant was 16 micron Aluminium oxide Al2O3 powder mixed in oil with 4% concentration by weight. These solid contaminants were treated with five different antiwear additives to study their influence on the bearings. Bearings were operated such that the minimum oil film thickness in the bearing was equal to the size of the contaminants. These tests were run for a constant sliding distance of 7536m. The results showed that most of the wear measuring techniques do not suit heavily contaminated test conditions. However, the out-of-roundness technique proved to be the most reliable and practical. Based on this technique a methodology was developed which gave a wear characteristic number (N). A unique value of N can be derived for each additive, thereby ranking the additives for their efficacy. The finding of this research provides a better understanding of the methodologies used for measuring wear in journal bearings subjected to dusty environments, and examines the efficacy of each one of these. The wear characteristic number (N) can be used by manufacturers with support from international standards organisations, so that the users can confidently choose the most appropriate antiwear additive for their application. Machines operating in a dusty environment, such as mining industry and civil works are prone to premature failure with subsequent production losses. In response to this problem, this research project examines the interaction between solid contaminant particles and the lubricant film micro-geometry in lubricated surface contacts. In particular, it seeks to identify lubricant anti-wear additives, which are effective in reducing wear under abrasive conditions and thus making machine elements more dirt tolerant.