A new class of treatment processes called Advanced Reduction Processes (ARP) has been proposed. The ARPs combine activation methods and reducing agents to form highly reactive reducing radicals that degrade oxidized contaminants. Batch screening experiments were conducted to identify effective ARP by applying several combinations of activation methods (ultraviolet light, ultrasound, electron beam, microwaves) and reducing agents (dithionite, sulfite, ferrous iron, sulfide) to degradation of five target contaminants (perchlorate, nitrate, perfluorooctanoic acid, 2,4 dichlorophenol, 1,2 dichloroethane) at 3 pH levels (2.4, 7.0, 11.2). These experiments identified the combination of sulfite activated by ultraviolet light produced by a low pressure mercury vapor lamp as an effective ARP. More detailed kinetic experiments were conducted with nitrate and perchlorate as target compounds and nitrate was found to degrade more rapidly than perchlorate. The effects of pH, sulfite concentration, and light intensity on perchlorate and nitrate degradation were investigated. The effectiveness of the sulfite/UV-L treatment process improved with increasing pH for both perchlorate and nitrate.

Les nanostructures à base de nitrures d’éléments III suscitent un intérêt croissant, en raison de leurs propriétés singulières et de leurs applications technologiques potentielles, dans les diodes électroluminescentes (LED) notamment. La maîtrise et le contrôle du dopage de ces nanostructures est un enjeu crucial, mais difficile. A ce sujet, cette thèse apporte une contribution nouvelle, en explorant le processus de dopage de type n et p des nanofils (NFs) de GaN crus par épitaxie par jets moléculaires (EJM). En particulier, les propriétés électriques de ces structures ont été caractérisées par une approche multi-technique, à l’échelle du NF unique.Tout d'abord, les propriétés structurales et électriques d'une série de NFs de GaN dopés au Si (type n) ont été étudiées. Des mesures de spectroscopie de rayons X à haute résolution sur des NFs individuels ont mis en évidence une incorporation de Si plus élevée dans les NFs que dans les couches minces épitaxiées, ainsi qu’une migration du Si à la surface du NF pour le fil ayant le niveau de dopage le plus élevé. Des mesures de transport sur des NFs uniques (quatre contacts avec une température allant de 300 K jusqu’à 5 K) ont démontré un contrôle du dopage, avec une résistivité allant de 10^2 à 10^-3 Ω.cm et une concentration de porteurs comprise entre 10^17 et 10^20 cm-3. Des mesures réalisées sur des transistors à effet de champ à NFs uniques non intentionnellement dopés ont démontré qu’ils sont de type n avec une mobilité de porteurs élevée.Parallèlement à cela, les conditions de croissance de NFs de GaN dopés au Mg (p-type) et de jonctions p-n ont été déterminées afin d’obtenir une incorporation significative en Mg. Les propriétés électriques de jonctions p-n axiale à base de NFs de GaN posées sur un substrat de SiO2 et contactés avec de l’oxyde d’indium-étain (ITO) ont été étudiées en utilisant la technique du courant induit par faisceau électronique (EBIC). L’analyse EBIC a permis de localiser la jonction p-n le long du fil et de clairement montrer son bon fonctionnement en polarisation directe ou inverse. L'analyse EBIC a démontré que le GaN de type p est hautement résistif, confirmant ainsi les difficultés à réaliser des mesures de transport sur ce matériau.Cette étude originale a permis de décrire les propriétés électriques et de dopage de ces NFs de GaN à une échelle nanoscopique, facilitant ainsi la fabrication des futurs dispositifs incorporant des nanostructures à base de GaN. / III-nitride nanostructures have been attracting increasing attention due to their peculiar properties and potential device applications as lighting LEDs. The control and evaluation of the doping in the nanostructures is a crucial, yet a challenging issue. This thesis advances the field by exploring the n and p type doping process of GaN nanowires (NWs) grown by molecular beam epitaxy (MBE). In particular, their electrical properties have been revealed through a multi-technique approach at the single NW level.Firstly, the structural and electrical properties of a series of Si-doped (n-type) GaN NWs have been studied. High resolution energy dispersive X-ray spectroscopy measurements on single NWs have illustrated the achievement of a higher Si incorporation in NWs than in epilayers, and Si segregation at the edge of the NW with the highest doping. Furthermore, direct transport measurements (four probes measurements from 300 K down to 5 K) on single NWs have shown a controlled doping with resistivity from 10^2 to 10^-3 Ω.cm, and a carrier concentration from 10^17 to 10^20 cm-3. Field effect transistor measurements have evidenced the n-type nature and a high electron mobility of the non-intentionally doped NWs.Secondly, the growth conditions of Mg-doped (p-type) and axial GaN p-n junction NWs have been determined to achieve significant Mg incorporation. Furthermore, the electrical properties of the axial GaN p-n junction NWs, dispersed on SiO2 and contacted by ITO, have been studied using electron beam induced current (EBIC) technique. EBIC technique revealed the location of the p-n junction and clearly demonstrated its operation under reverse and forward polarization. Moreover, EBIC showed highly resistive p-GaN in accordance with the difficulties to perform direct transport measurements on p-GaN NWs.This original study provides a nanoscale description of the electrical and doping properties of the GaN NWs, facilitating the fabrication of the future GaN nanostructures based devices.

Dans leurs usages courants comme isolants électriques, les matériaux solides organiques sont constitutifs aussi bien des câbles de transport d'énergie électrique, des circuits de commande et de conversion de puissance que des composants (micro)électroniques ou des systèmes embarqués (revêtement thermique des satellites, batteries d'accumulateurs...). La diversité des contraintes d'utilisation auxquelles ils sont soumis (champ électrique, rayonnement, température, humidité...) les prédisposent à emmagasiner des charges en leur sein, susceptibles d'affecter la fiabilité des systèmes qui en dépendent. L'un des moyens communément mis en œuvre pour étudier le comportement électrique de ces charges est la mesure de la distribution spatio-temporelle des charges d'espace, en soumettant le diélectrique à une différence de potentiel continue à travers deux électrodes. Cette méthode ne permet cependant pas toujours de distinguer clairement la contribution des charges dues à la génération, d'une part, et celles dues aux phénomènes de transport, d'autre part. Cette étude propose une approche alternative, consistant à déposer sous vide des charges (électrons) au sein de l'isolant par le biais d'un faisceau d'électrons, à une position connue et en quantité maîtrisée, en prenant en compte d'autres processus physiques liés à l'implantation d'électrons afin de prévoir et modéliser le comportement de ces matériaux irradiés. Des films de PolyEthylène basse densité (PEbd), préparés par thermomoulage, ont été irradiés par un faisceau d'électrons de 80 keV avec un flux de 1 nA/cm2. Les mesures de charge d'espace par la méthode Electro-Acoustique Pulsée (PEA), réalisées d'abord in-situ, puis ex-situ sous polarisation électrique DC, confirment une localisation effective de charges au sein du matériau. Les résultats sous polarisation électrique après irradiation mettent en évidence une importante présence de charges positives dans la zone irradiée du diélectrique. Les caractérisations électriques des films PEbd irradiés montrent un comportement complètement différent de celui d'un même matériau non-irradié, laissant penser à une modification de la structure chimique du matériau. Des mesures physico-chimiques (spectroscopie infra-rouge, Photoluminescence et Analyse Enthalpique Différentielle-DSC) sur ces films PEbd irradiés, ne montrent pas une dégradation significative de la structure chimique du diélectrique qui expliquerait le comportement électrique observé sous polarisation post-irradiation. Des mesures complémentaires montrent le comportement réversible du PEbd irradié puis polarisé, qui serait uniquement lié à la présence des charges générées par le faisceau. Les données expérimentales de cette étude ont parallèlement alimenté un modèle numérique de transport de charges, développé pour tenir compte des contraintes sous irradiation. Ce modèle a permis de reproduire les résultats d'implantation de charge par faisceau d'électrons in-situ ainsi que la majorité des processus électriques observés sur du PEbd irradié puis polarisé. Il confirme l'impact de la charge déposée par faisceau d'électrons sur le comportement sous polarisation et permet de conclure quant à l'origine des charges positives observées post-irradiation, qui seraient dues aussi bien aux phénomènes d'injection aux électrodes qu'à la création de paires électrons/trous par le faisceau d'électrons pendant l'irradiation. / In their common uses as electrical insulators, organic solid materials are constitutive of electric power transmission cables, power control and conversion circuits as well as (micro) electronic components or embedded systems (thermal coating of satellites, batteries of accumulators, etc.). Under various constraints of use (electric field, radiation, temperature, humidity ...) they can accumulate charges in their bulk which could affect the reliability of the systems in which they are employed. One of the commonly used means to study the electrical behavior of these charges is to measure the spatiotemporal distribution of charges by subjecting the dielectrics to a continuous potential difference between two electrodes. However, this method does not always allow clearly distinguishing the contribution of charges due to generation on the one hand and the one due to transport phenomena on the other hand. This study proposes an alternative approach, consisting in generating charges (electrons) within the electrical insulation using an electron-beam under vacuum. The charges are hence deposited at a known position and in a controlled quantity. Other physical processes related to the implantation of electrons must then be taken into account in order to predict and model the behavior of these irradiated materials. Low-density polyethylene (LDPE) films, prepared by thermal molding, were irradiated by a 80 keV electron-beam with a current flux of 1 nA/cm2. Space charge measurements using the Pulsed Electro-Acoustic (PEA) method, performed first in-situ and then ex-situ under DC electrical polarization, confirm an effective localization of charges within the material. The results under electrical polarization after irradiation show an important amount of positive charges in the irradiated zone of the dielectric. The electrical characterizations of irradiated LDPE films show a completely different behavior compared to the same non-irradiated material, suggesting a modification of the chemical structure of the material. Physico-chemical measurements (infrared spectroscopy, Photoluminescence and Differential Scanning Calorimetry-DSC) on these irradiated PEbd films do not show a significant degradation of the chemical structure of the dielectric which would explain the observed electrical behavior under post-irradiation polarization. Additional measurements show the reversible behavior of the irradiated then polarized PEbd, which would be only related to the presence of the charges generated by the beam. The experimental data of this study have simultaneously fed a numerical model of charge transport, developed to take into account the irradiation constraints. This model allows reproducing the in-situ results of charge implantation by the electron beam as well as the majority of the electrical processes observed on irradiated and polarized LDPE. It confirms the impact of the electron-beam deposited charge on the behavior under polarization and allows concluding on the origin of the positive charges observed after irradiation, which would be due to injection at the electrodes as well as to the creation of electron-hole pairs by the electron-beam during irradiation.

Additive manufacturing (AM) is the name given to the technology of building 3D parts by adding layer-by-layer of materials, including metals, plastics, concrete, etc. Of the different types of AM techniques, electron beam melting (EBM), as a powder bed fusion technology, has been used in this study. EBM is used to build parts by melting metallic powders by using a highly intense electron beam as the energy source. Compared to a conventional process, EBM offers enhanced efficiency for the production of customized and specific parts in aerospace, space, and medical fields. In addition, the EBM process is used to produce complex parts for which other technologies would be either expensive or difficult to apply. This thesis has been divided into three sections, starting from a wider window and proceeding to a smaller one. The first section reveals how the position-related parameters (distance between samples, height from build plate, and sample location on build plate) can affect the microstructural characteristics. It has been found that the gap between the samples and the height from the build plate can have significant effects on the defect content and niobium-rich phase fraction. In the second section, through a deeper investigation, the behavior of Alloy 718 during the EBM process as a function of different geometry-related parameters is examined by building single tracks adjacent to each other (track-by-track) andsingle-wall samples (single tracks on top of each other). In this section, the main focus is to understand the effect of successive thermal cycling on microstructural evolution. In the final section, the correlations between the main machine-related parameters (scanning speed, beam current, and focus offset) and the geometrical (melt pool width, track height, re-melted depth, and contact angle) and microstructural (grain structure, niobium-rich phase fraction, and primary dendrite arm spacing) characteristics of a single track of Alloy 718 have been investigated. It has been found that the most influential machine-related parameters are scanning speed and beam current, which have significant effects on the geometry and the microstructure of the single-melted tracks.

Comprendre et modéliser le comportement des matériaux sous irradiation électronique est un enjeu important pour l’industrie spatiale. La fiabilité des satellites nécessite de maîtriser et prédire les potentiels de surface s'établissant sur les diélectriques. Ce travail de doctorat a donc pour objectif de caractériser et de modéliser les différents mécanismes physiques (en surface et en volume) gouvernant le potentiel de charges dans les matériaux polymères spatiaux tels que le Téflon® FEP et le Kapton® HN. La mise au point d'un nouveau dispositif et d'un protocole expérimental a permis de corroborer l'existence d’une conductivité latérale des charges, souvent négligée dans les modèles physiques et numériques. Les études paramétriques, révélant l’influence de l’énergie et le flux des électrons incidents, ont permis de brosser un portrait des processus mis en jeu pour le transport (par saut ou par piégeage/dépiégeage) de charges en surface. A la lumière de cette étude, une conductivité équivalente est extraite, assimilant le matériau à un système prenant en compte les mécanismes de transport volumique et surfacique. L'analyse des évolutions non-monotones de potentiel mesurées sur les polymères spatiaux en condition spatiale a permis de révéler une dépendance de la conductivité volumique induite sous irradiation avec la dose reçue. L'étude paramétrique réalisée sur les mécanismes de transport en volume révèle une influence minoritaire du déplacement du barycentre de charges et du vieillissement physicochimique. Un modèle «0D» à un seul niveau de pièges, prenant en compte les mécanismes de piégeage/dépiégeage et recombinaison entre les porteurs de charges, a été développé. Ce modèle simplifié permet de reproduire qualitativement les évolutions de potentiel expérimentales en fonction du débit de dose et lors d'irradiations successives. / Charging behaviours of space dielectric materials, under electron beam irradiation, is of special interest for future spacecraft needs, since this mechanism could induce electrostatic discharges and consequently damages on the sensitive systems on board. In order to assess the risks of charging and discharging, this work aims at understanding the overall charge transport mechanisms and predicting the electrical behaviour of the insulator materials, especially Teflon® FEP and Kapton® HN. For an optimized prediction, the first part of our work is thus to check whether lateral conduction process can take place in the overall charge transport mechanism. Through the definition of a new experimental set-up and protocol, we have been able to discriminate between lateral and bulk conductivity and to reveal the presence of lateral conductivity that is enhanced by radiation ionization processes. We have been able to demonstrate as well that lateral intrinsic conductivity is enhanced with the increase current density and when approaching the sample surface. The second part of our work deals with the characterization of the electrical charging behaviour of Teflon® FEP under multi-energetic electron beam irradiation and the modelling of the overall bulk charge transport mechanisms. An experimental study on charge potential evolution as a function of electron spectrum, electric field, relaxation time, dose and dose rate, was performed. A numerical model has been developed to describe the effect of the different abovementioned mechanisms on the evolution of the surface potential. This model agrees correctly with the experimental phenomenology at qualitative level and therefore allows understanding the physical mechanisms steering charge transport in Teflon® and Kapton®.

O interesse na utilização de fibras naturais com matrizes poliméricas para a preparação de compósitos espalhou-se rapidamente ao longo dos últimos anos. No entanto, a adesão interfacial entre a fibra e a matriz tem ainda de ser aperfeiçoada. Para melhorar a adesão entre os constituintes e, consequentemente as propriedades mecânicas e térmicas dos materiais, duas abordagens foram investigadas: a irradiação por feixe de elétrons e a mercerização. Este trabalho descreve a fabricação e caracterização de biocompósitos de polietileno de alta densidade e fibra do ouriço da castanha do Brasil que foram preparadas por duas metodologias diferentes: a primeira foi irradiar o compósito com 150 kGy e a segunda foi irradiar a matriz com 15 kGy e então produzir o compósito. Para ambas as metodologias foram utilizadas fibras naturais mercerizadas e não mercerizadas. O efeito dos tratamentos estudados para melhorar a adesão entre a fibra e a matriz polimérica foi avaliado através de caracterizações mecânica, química, térmica e morfológica. Com base neste estudo, observou-se que a fibra do ouriço da castanha do Brasil é um material tecnicamente viável para uso como reforço em compósitos poliméricos. Observou-se que o processo de irradiação da matriz seguida da produção dos compósitos é um método eficaz para melhorar as propriedades térmicas e mecânicas dos compósitos biopoliméricos e que, quando comparado com o processo de mercerização, esse método pode ser considerado mais ambientalmente correto (sem produtos químicos e sem geração de resíduo), mais barato e mais simples. / The interest in the use of natural fibres with polymeric matrix for the preparation of composite spread rapidly over the last years. However, the interfacial adhesion between the fiber and the matrix has to be improved. To improve the adhesion between the constituents and consequently the mechanical and thermal properties of materials, two approaches were investigated: electron beam irradiation and mercerization. This paper describes the fabrication and characterization of biocomposites compounds with high density polyethylene and fibre from Brazil nut pod that were prepared by two different methods: the first irradiating the composite with 150 kGy and the second was radiating matrix with 15 kGy and then produce the composite. For both methodologies, natural fibers, mercerized and non-mercerized were used. The effect of the treatments to improve adhesion between the fiber and the polymer matrix was evaluated through mechanical, chemical, thermal and morphology charcterization. Based on this study, it was observed that fibre from Brazil nut pod is a technically viable material for use as reinforcement in polymer composites. It was observed that the process of matrix irradiation followed by the composite fabrication is an effective method for improving the thermal and mechanical properties of the composites, when compared with mercerization process, this method can be considered more environmentally friendly (no chemicals, and without generating waste), cheaper and simpler.

O presente trabalho tem como objetivo desenvolver um processo de fabricação de elementos micro-ópticos utilizando-se litografia por feixe de elétrons, empregando o resiste SU-8, negativo e amplificado quimicamente, sobre substrato de Si. Para tanto, é realizado o estudo dos parâmetros do efeito de proximidade a, b e h para se modelar e controlar os efeitos do espalhamento dos elétrons no resiste e no substrato, e se altera o processamento convencional do SU-8 para se obter um processo com baixo contraste. A determinação dos parâmetros do efeito de proximidade para o sistema de escrita direta e amostra SU-8 / Si é feita experimentalmente e por simulação de Monte Carlo. Particularmente, verifica-se a dependência dos mesmos com a profundidade do resiste. Primeiramente utilizando o software PROXY, obtêm-se a, b e h da observação de padrões de teste revelados. Chega-se a 4m para o parâmetro () que mede o retroespalhamento dos elétrons pelo substrato e 0,7 para a relação (h) entre a intensidade destes com aquela dos elétrons diretamente espalhados pelo resiste (alcance dado por a). Ainda, com esses dados, estima-se o diâmetro do feixe do microscópio eletrônico de varredura a partir da equação de aproximação de espalhamento direto para pequenos ângulos (a = 128nm na superfície do resiste) e se determina a resolução lateral do processo (a = 800nm na interface resiste/ substrato, para um filme de 2,4m). Em seguida, usa-se o software CASINO para se calcular os parâmetros de proximidade a partir da curva de densidade de energia dissipada no resiste obtida pela simulação da trajetória de espalhamento dos elétrons. Confrontam-se, finalmente, os valores obtidos pelos dois métodos. Em relação ao processamento do resiste SU-8, são determinadas as condições experimentais para a fabricação de estruturas tridimensionais por litografia de feixe de elétrons. Especificamente, busca-se desenvolver um processo com características (espessura, contraste, sensibilidade e rugosidade) adequadas para a fabricação de micro-dispositivos ópticos. Inicia-se com o levantamento das curvas de contraste e da sensibilidade do SU-8 para determinadas temperaturas de aquecimento pós-exposição. Obtém-se contraste abaixo de 1 para aquecimento pós-exposição abaixo da temperatura de transição vítrea do resiste, mantendo-se sensibilidade elevada (2C/cm2). Em seguida, mede-se a rugosidade da superfície do filme revelado para diferentes doses de exposição. Para finalizar, submete-se a amostra a um processo de cura e escoamento térmico, para melhorar a dureza e a rugosidade do resiste a ser utilizado como dispositivo final Consegue-se um valor de rugosidade (40nm) inferior a 20 vezes o comprimento de onda de diodo laser de eletrônica de consumo. Por fim, é produzido um dispositivo com perfil discretizado em 16 níveis como prova de conceito. / This work aims at developing an electron-beam lithography process for the fabrication of microoptical elements using the negative tone chemically amplified resist SU-8 on Si substrate. A study of the proximity effect parameters a, b and h is carried out to model and control the electron scattering both in the resist and in the substrate, and the SU-8 standard processing conditions are changed to achieve a low contrast process. The determination of the SU-8 / Si proximity effect parameters and its dependence with resist depth is done employing an experimental method and through Monte Carlo simulations. First, a, b and h are obtained comparing exposed patterns calculated by the software PROXY. b, the parameter which measures the backscattering of the electrons by the substrate, is equal to 4m and the value of h, the ratio of the dose contribution of backscattered electrons to that of the forward scattered (related to a), is 0.7. The extrapolation of exposed patterns data is used to estimate the scanning electron microscope beam diameter through the equation for low angle scattering (a = 128nm at the resist surface) and the lateral resolution of the process is determined (a = 800nm at the resist/ substrate interface, for a 2.4m film). With aid of the software CASINO, Monte Carlo simulations of the scattering trajectories of electrons in substrate and resist materials are calculated, recording the energy that they dissipate through collisions along their path. The results obtained representing the profile of the energy dissipated in the resist are used to determine the proximity effect parameters. The experimental method results are compared to that obtained by simulation. Regarding the SU-8 processing, the process parameters for the fabrication of three-dimensional structures by electron-beam lithography are determined. The process is designed to have specifications (thickness, contrast, sensitivity and surface roughness) suitable for microoptical elements fabrication. It begins with the determination of the SU-8 contrast curve and its sensitivity for specific post-exposure bake temperatures. A below the unit contrast process with high sensitivity (2C/cm2) is achieved postannealing the sample below the resist glass transition temperature. The film surface roughness is measured after resist development for different exposure doses, and a controlled hardbake (cure) and reflow is carried to enhance both the mechanical properties and the surface roughness of the structures that will remain as part of the final device. A RMS roughness of 40nm, lower than 20 times the wavelength of consumer electronics laser diode, is obtained. The electron-beam process designed is applied to the fabrication of a microelement with a 16-level profile discretization.

Nous avons étudié l'influence de la fabrication de guides d'ondes optiques par échange protonique doux(SPE) sur les cristaux de niobate de lithium (LN) polarisé périodiquement et nous avons montré que,dans certains cas, ce processus conduit à la création de nanodomaines en surface. Ces nanodomaines enforme d'aiguille peuvent être responsables de la réduction de l'efficacité de conversion non linéaireobservée dans les guides qui sont affectés. Nous avons également étudié l'influence de différents typesd'échange protonique sur la formation, par application d'un champ électrique, de domaines dans le LNcongruent. Cette étude montre que le seuil de nucléation peut être fortement réduit par la présence duguide d'onde et que l'apparition et le développement des domaines en forme de traits est fortementmodifiée. Elle montre également que la fusion des nanodomaines existants au voisinage des parois dedomaine aboutit à la formation de parois élargies et de domaines en forme de dendrites. En irradiantavec un faisceau d'électrons la surface Z- d'un échantillon de LN préalablement soumis à un échangeprotonique doux et recouvert d'une couche de résine électronique, nous avons réussi à former desdomaines avec des formes arbitraires. Par cette technique, nous avons fabriqué des domainespériodiques d'excellente qualité dans des cristaux présentant des guides canaux SPE. Des expériences degénération de deuxième harmonique dans ces guides nous ont permis d'obtenir des efficacités deconversion de 48%/W.cm2 ce qui est conforme aux prédictions ainsi que la forme des spectres d'accordde phase que nous avons observés. Ceci démontre tout l'intérêt de ce processus / The investigation of influence of the soft proton exchange (SPE) optical waveguide (WG) creation onperiodically poled lithium niobate (PPLN) has been done. It has been shown that the WG fabricationprocess can induce the formation of needle like nanodomains, which can be responsible for thedegradation of the nonlinear response of the WG created in PPLN crystals. The domain structure (DS)evolution has been studied in congruent lithium niobate (LN) crystals with surface layers modified bythree different proton exchange techniques. The significant decrease of the nucleation threshold fieldand qualitative change of domain rays nucleation and growth have been revealed. The formation of abroad domain boundary and dendrite domain structure as a result of nanodomains merging in front ofthe moving rays has been demonstrated. The formation of DS in LN with SPE by irradiation of coveredby electron resist polar surface of LN has been investigated. Formation of domains with arbitrary shapesas a result of discrete switching has been revealed. Finally, it has been demonstrated that electron beamirradiation of lithium niobate crystals with surface resist layer can produce high quality periodical domainpatterns after channel waveguide fabrication. Nonlinear characterizations show that the conversionefficiencies and the phase matching spectra conform to theoretical predictions, indicating that thiscombination presents a great interest for device fabrication. Second harmonic generation withnormalized nonlinear conversion efficiency up to 48%/(W cm2) has been achieved in such waveguides

To investigate quantum confinement effects on silicon (Si) light source electroluminescence (EL) properties like quantum efficiency, external power efficiency and spectral emission, thin Si finger junctions with nanometre-scale dimensions were designed and manufactured in a fully customized silicon-on-insulator (SOI) semiconductor production technology. Since commonly available photolithography is unusable to consistently define and align nanometre-scale line-widths accurately and electron-beam lithography (EBL) by itself is too time-expensive to expose complete wafers, the wafer manufacturing process employed a selective combination of photolithography and EBL. The SOI wafers were manufactured in the clean-rooms of both the Carl and Emily Fuchs Institute for Microelectronics (CEFIM) at the University of Pretoria (UP) and the Georgia Institute of Technology’s Microelectronic Research Centre (MiRC), which made a JEOL JBX-9300FS electron-beam pattern generator (EPG) available. As far as is known this was the first project in South Africa (and possibly at the MiRC) that employed EBL to define functional nanometre-scale semiconductor devices. Since no standard process recipe could be employed, the complete design and manufacturing process was based on self-obtained equipment characterization data and material properties. The manufacturing process was unprecedented in both the CEFIM and MiRC clean-rooms. The manufacture of nanometre-scale Si finger junctions not only approached the manufacturing limits of the employed processing machinery, but also had to overcome undesirable physical effects that in larger-scale semiconductor manufacture usually are negligible. The device design, mask layout and manufacturing process therefore had to incorporate various material, equipment limitation and physical phenomena like impurity redistribution occurring during the physical manufacturing process. Although the complicated manufacturing process allowed many unexpected problems to occur, it was expected that at least the simple junction breakdown devices be functional and capable of delivering data regarding quantum confinement effects. Although due to design and processing oversights only 29 out of 505 measured SOI light sources were useful light emitters, the design and manufacture of the SOI light sources was successful in the sense that enough SOI light sources were available to conduct useful optical characterization measurements. In spite of the fact that the functional light sources did not achieve the desired horizontal (width) confinement, measured optical spectra of certain devices indicate that vertical (thickness) confinement had been achieved. All spectrometer-measured thickness-confined SOI light sources displayed a pronounced optical power for 600 nm < λ < 1 μm. The SOI light source with the highest optical power output emitted about 8 times more optical power around λ = 850 nm than a 0.35 μm bulk-CMOS avalanche light-source operating at the same current. Possible explanations for this effect are given. It was shown that the buried oxide (BOX) layer in a SOI process could be used to reflect about 25 % of the light that would usually be lost to downward radiation back up, thereby increasing the external power efficiency of SOI light sources. This document elaborates on the technical objectives, approach, chip and process design, physical wafer manufacture, production process control and measurement of the nanometre-scale SOI light sources. Copyright / Dissertation (MEng)--University of Pretoria, 2010. / Electrical, Electronic and Computer Engineering / unrestricted

The aerospace industry is constantly striving to becoming more economical and environmentally friendly. One of many efforts to achieve this is the Lightcam project which in this case is evaluating the use of additive manufacturing in the form of electron beam melting in conjunction with the nickel-based superalloy, Alloy 718. This combination is not fully explored and examined. For this purpose, a demonstrator vane was produced and it was subsequently evaluated in this thesis. The evaluation was performed in as-built condition and was divided in non-destructive testing, evaluation of these methods and metallographic review to confirm the results, and potentially revealing more properties. The non-destructive testing was performed using conventional radiography and computed tomography. Both methods struggled to deliver complete and reliable results, for varying reasons. Radiography could deliver results of the whole vane, but these were impossible to evaluate due to the rough surface created by the electron beam melting process. The computed tomography on the other hand was not affected by the rough surface and produced usable, though not complete, results of the vane. The reason for the computed tomography’s inability to deliver complete results was the material, varying thickness and complex geometry of the vane. As a complement and to verify the results from the non-destructive testing, a metallographic examination was conducted. These tests were conducted with the aim of answering the following three questions:  What non-destructive testing methods are suitable to evaluate Alloy 718 components manufactured with electron beam melting? - Neither radiography nor computed tomography are suitable as a sole evaluation method, for various reasons. All surface dependent methods were deemed unsuitable without testing due to the rough surface. What types of defects and in what quantity can they be found in the produced vane? - Defects found are: Porosity and lack of fusion, both found as internal and partially external and in varying sizes. Where are the defects located? - Pores are mainly found in the center of sections modeled to a 3mm thickness. Lack of fusion was found between build layers in all thicknesses. Apart from these results, hardness was found to vary depending on build height, increasing from the bottom towards the top. Microstructure was also found to vary with the build height, but always consisting of either equiaxed or columnar grains. / Lightcam