Les cellules solaires à base de nanofils de silicium offrent une alternative intéressante pour la réalisation de panneaux photovoltaïques à haut rendement et à faible coût. Elles bénéficient notamment des excellentes propriétés optiques des nanofils qui forment une surface à très faible réflectivité tout en piégeant efficacement la lumière. Dans cette thèse, nous utilisons et améliorons une méthode de gravure chimique peu coûteuse et industrialisable pour la fabrication de forêts de nanofils de silicium. En adaptant la mouillabilité du substrat et des nanofils, nous avons remédié au problème d'agglomération inhérent à cette méthode lorsqu’on veut obtenir des forêts denses et désordonnées de nanofils. En combinant cette méthode de gravure chimique à la lithographie assistée par nanosphères, nous avons pu fabriquer des réseaux ordonnés de nanofils avec un contrôle précis des propriétés géométriques (diametre des nanofils et distance entre eux). Les propriétés optiques de ces réseaux ont été étudiées théoriquement et expérimentalement afin d'identifier les configurations optimales. Nous avons ensuite fabriqué des cellules solaires à partir de ces différents types de nanofils et deux types de structures. Le premier type, des cellules solaires HIT (Hétérojonction avec couche mince Intrinsèque) à base de nanofils de silicium, a été fabriqué par RF-PECVD. L'optimisation des conditions de dépôt plasma nous a permis d'obtenir des cellules solaires hautement performantes: rendements de 12,9% et facteurs de forme au-delà de 80%. Le second type, des cellules solaires hybrides, est basé sur la combinaison d'une couche organique et des nanofils de silicium. La caractérisation des cellules fabriquées montre des rendements prometteurs. Enfin, nous présentons des résultats préliminaires pour transférer ces concepts à une technologie couches minces. / Silicon Nanowire (SiNW) based solar cells offer an interesting choice towards low-cost and highly efficient solar cells. Indeed solar cells based on SiNWs benefit from their outstanding optical properties such as extreme light trapping and very low reflectance. In this research project, we have fabricated disordered SiNWs using a low-cost top-down approach named the Metal-Assisted-Chemical-Etching process (MACE). The MACE process was first optimized to reduce the strong agglomeration observed at the top-end of the SiNWs by tuning the wettability properties of both the initial substrate and the SiNWs surface. By combining the MACE process with the nanosphere lithography, we have also produced ordered SiNW arrays with an accurate control over the pitch, diameter and length. The optical properties of these SiNW arrays were then investigated both theoretically and experimentally in order to identify the geometrical configuration giving the best optical performance. Disordered and ordered SiNW arrays have been integrated into two types of solar cells: heterojunction with intrinsic thin layer (HIT) and hybrid devices. SiNW based HIT devices were fabricated by RF-PECVD and the optimization of the process conditions has allowed us to reach efficiency as high as 12.9% with excellent fill factor above 80%. Hybrid solar cells based on the combination of SiNWs with an organic layer have also been studied and characterized. The possible transfer of this concept to the thin film technology is finally explored.

De nos jours, il est crucial pour les industries de réduire leur consommation énergétique. Pour les industries du transport, cela peut se faire par le biais de l’allègement des pièces de structure. Dans ce contexte, les structures cellulaires représentent une des solutions les plus prometteuses. Grâce au développement de la fabrication additive, l’élaboration de telles géométries complexes n’est plus un frein à leur utilisation. Néanmoins, cette dernière restera limitée tant que les propriétés mécaniques – et plus particulièrement la résistance en fatigue pour les pièces aéronautiques – ne seront pas maîtrisées. Ce travail de thèse a pour objectif de déterminer les mécanismes qui gouvernent le comportement en fatigue de ces structures cellulaires. Pour cela, le travail s’est focalisé sur l’élement unitaire les constituant : la poutre. Des éprouvettes minces représentatives de la poutre ont été élaborées par Electron Beam Melting puis caractérisées à l’état brut de fabrication à l’aide de différentes techniques (tomographie aux rayons X, microscopie optique et électronique, …). Leurs propriétés statique et cyclique en traction ont ensuite été évaluées. L’état de surface et en particulier les défauts d’entaille ont été identifiés comme responsable de la perte de résistance. L’impact de ces défauts sur la résistance en fatigue a été prédit avec succès par le biais de diagrammes de Kitagawa. L’impact de l’orientation de fabrication a également été observé et prédit. Différents post-traitements ont ensuite été utilisés afin d’améliorer ces propriétés. Le polissage chimique et le grenaillage ultrasonique ont réduit de manière significative la criticité des défauts de surface ce qui a grandement amélioré les propriétés mécaniques des éprouvettes, jusqu’à se rapprocher de celles obtenues après usinage. Par ailleurs, la compression isostatique à chaud a provoqué la fermeture de l’entièreté des défauts internes ainsi qu’un grossissement de la microstructure. Ce dernier point permet une amélioration supplémentaire de la performance en fatigue une fois combiné avec un traitement de surface. Enfin, une méthode permettant de détecter automatiquement tous les défauts d’entailles et de déterminer leur criticité et leur influence sur la résistance en fatigue a été proposée et discutée. Elle a ensuite été appliquée avec succès aux échantillons attaqués chimiquement mais des modifications demeurent nécessaire pour l’appliquer à d’autres états de surface. / Nowadays, reducing the energy consumption is crucial for most of the industries. For transportation industries, it can be achieved through weight reduction. In this context, cellular structures turn out to be one of the most efficient solution. Thanks to the development of additive manufacturing, producing such complex geometries is no longer an issue. However, their use will remain limited as long as their fatigue performances are not known. This PhD work aimed at understanding the mechanisms that govern the fatigue behaviour of such cellular structures. It was first decided to focus on their unitary element, i.e. a single strut. Single struts samples were manufactured by Electron Beam Melting and then characterized in as-built conditions using different experimental techniques (X-ray tomography, optical and electron microscopy, etc.). Their static and cyclic tensile properties were then evaluated. The rough surface and in particular notch-like defects were found to be responsible for the knockdown of the mechanical properties. Regarding the fatigue resistance, their detrimental impact was predicted using Kitagawa diagrams. It also enabled to explain the impact of the build orientation. Different post-treatments were used in order to improve these mechanical properties. Chemical etching and ultrasonic shot peening (USP) significantly reduced the severity of surface defects of as-built thin struts and thus increased their mechanical properties. After USP, the fatigue properties of machined samples were almost matched. Hot Isostatic Pressing lead to the closure of all internal defects and to the coarsening of the microstructure. When combined with one of the surface treatments, the fatigue properties were further improved. Finally, a method enabling to systematically and automatically extract from the surface the most critical defects and quantitatively analyze their influence on fatigue life was proposed and discussed. It was successfully applied to chemical etched samples but improvements are mandatory for other surface conditions.

Ziel ist die räumliche Abbildung biologischer Materialien (Knochen, Kollagenfibrillen und Zähne) hinsichtlich deren Struktur auf der Nanometerskala mit Hilfe der Nanotomographie. Die Nanotomographie ist eine moderne dreidimensionale Volumenabbildungsmethode auf der Nanometerskala basierend auf der Rasterkraftmikroskopie. Für die Nanotomographie wurden Ätzprotokolle an Zähnen, Kollagenfibrillen und Knochen entwickelt, die einen gleichmäßigen Abtrag bewirken. Lineare Verschiebungen der aufgenommenen Schichten werden mit Hilfe der manuellen Registrierung korrigiert und zu einem Volumenbild rekonstruiert. Ein zentrales Ergebnis sind dabei erste hochaufgelöste Volumenbilder einzelner Kollagenfibrillen im nativen Knochen. Neben der konventionellen Nanotomographie wird ein Ansatz zur automatisierten Nanotomographie mit einer Auflösung von 10 nm am Beispiel des menschlichen Knochens und Zahnes demonstriert. Mit Hilfe von mikroskopischen und elektronenmikroskopischen Techniken wurden die verschiedenen Strukturebenen des humanen Zahn und Knochens abgebildet und die räumlichen Strukturen der TM-AFM-Bilder auf der Mikro- und Nanometerskala eingeordnet. Darüber hinaus konnte mit Hilfe analytischer Messmethoden die chemische Zusammensetzung des kortikalen nativen Knochens erfasst werden und Änderungen durch das Ätzen detektiert werden.

Orientadores: Sandro Guedes de Oliveira, Julio Cesar Hadler Neto / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Física Gleb Wataghin / Made available in DSpace on 2018-08-21T04:43:57Z (GMT). No. of bitstreams: 1 Vellame_IgorAlencar_D.pdf: 6307121 bytes, checksum: 509c7cc3c5c11f238463340fa191af50 (MD5) Previous issue date: 2012 / Resumo: O presente trabalho pode ser inserido na grande área de estudo da interação da radiação com sólidos. Ele tem como principal objetivo entender a cinética de reconstituição dos danos causados por irradiação com íons ( traço latente) na apatita e e realizado através do estudo de annealing em traços atacados. O que se denomina traço latente e a trilha de danos causada pela desaceleração do íon, enquanto este atravessa a matéria. Estes traços latentes são meta-estaveis em relação ao tratamento térmico e apresentam uma taxa de reação a dissolução muito mais elevada que o mineral não danificado. Assim, para compreender as alterações causadas pelos tratamentos térmicos e necessária entender como o processo de ataque químico ocorre. Um cristal natural de apatita foi cortado em algumas orientações cristalográficas (principalmente basal e prismática) e estas amostras foram montadas em resina para obtenção de uma superfície plana com técnicas de polimento. Grande parte destas amostras foi irradiada com nêutrons (para induzir a fissão do isótopo 235 U com fluências de nêutrons térmicos próximas a 3xl015 cm-2 ) ou com íons pesados (152Sm e 238 U com fluências pr6ximas a lx106 cm-2 e 5x 1011 cm-2). Utilizando a espectroscopia no infra-vermelho, foi possível estimar o valor do diâmetro do traço latente. Os valores encontrados (~8-9 nm) são coerentes com diversas medidas utilizando outras técnicas presentes na literatura. As taxas de dissolução da superfície do material pelo acido nítrico em diferentes condições (concentração e temperatura) foram medidas pelo método da máscara com êxito. Observou-se uma inversão na razão entre as taxas para as diferentes orientações conforme a concentração do reagente aumentada. A distribuição de comprimentos projetados também foi estudada para estimar a eficiência de observação e revelação do ataque químico (razão entre quantos traços são efetivamente contados e quantos traços são gerados). A metodologia presente na literatura para o calculo da distribuição de comprimentos projetados foi revista e novas estimativas foram feitas utilizando métodos numéricos com intuito de estimar os comprimentos e desvios dos fragmentos de fissão leve e pesado na apatita. Foi observada uma deficiência intrínseca na medida do comprimento projetado, mas esta sozinha não e capaz de explicar o deficit de alcance observado para as irradiações com íons. Duas metodologias para o ca1culo do conteúdo de urânio nas amostras são apresentadas e os resultados da comparação com valores obtidos par outras técnicas independentes são satisfatórios. Isto fortalece o método dos traços de fissão como uma técnica absoluta para a dosimetria de nêutrons. Par fim, para o estudo do tratamento térmico, dais conjuntos de dados pana traços de íons foram preparados: um a partir da diminuição do comprimento projetado; e outro com o estudo da variação na abertura superficial de traços de íons incidentes perpendicularmente. Foi possível correlacionar as reduções da abertura superficial e do comprimento através de uma lei de potencia. Aparentemente, a abertura superficial parece ser um indicador da quantidade de defeitos e isto possibilita vincular melhor a cinética do tratamento térmico. Algumas extrapolações geológicas também foram realizadas e o razoável acordo com os dados geológicos demonstra que o processo e universal e que traços de íons podem ser usados como ferramenta para o estudo do tratamento térmico em traços atacados / Abstract: This work can be inserted in the great study area of radiation interactions with solids. It has as the main goal the understanding of the reconstitution of damage caused by ion irradiation (latent track) in apatite and it is investigated through the annealing of chemically etched tracks. A latent track is the damage trail caused by the ion deceleration in matter. These tracks are thermally meta-stable and they present an enhanced dissolution rate when compared to the non-damaged bulk mineral. Thus, in order to understand t he alterations caused by a thermal treatment, it is necessary to understand how does the chemical etching occur. A natural apatite crystal was cut in some crystallographic orientations (mainly basal and prismatic) and these samples were mounted in epoxy resin in order to obtain a fiat surface with polishing techniques. Great part of these samples were irradiated with thermal neutrons (inducing the 235 U fission with fiuence close to 3x 1015 cm-2 ) or heavy ions e 52Sm and 238U with nominal fluences of lx106 cm-2 and 5x1011 cm-2 ). Applying infra-red spectroscopy, it was possible to estimate the values of ion latent track diameters. The founded values (~8-9 nm) are coherent with several measurements employing other techniques presented in the literature. The mineral surface dissolution rates by nitric acid were successfully measured in different conditions ( etchant concentration and temperature) with the mask method. As the etchant concentration increases, an inversion in the dissolution rates ratio between different orientations was observed. The projected length distribution was also studied to estimate the revelation/observation efficiency (ratio between how many tracks were effectively counted and how many are expected). The methodology presented in the literature for the calculation of the expected projected length distribution was revised and new estimates were made with numerical methods. These numerical methods were employed to estimate the length and standard deviation of light and heavy fission fragments in apatite. An intrinsic deficit in the projected length measurement was observed. However, it alone could not explain the huge range deficit observed for external source irradiation in apatite. Two methodologies for the calculation of uranium content in t he samples were proposed. The comparison of the results with other values found from independent techniques was satisfactory. This strengthen the fission track method as an absolute technique for neutron dosimeter. Finally, two data sets for ion track thermal annealing study were prepared:! one from the shortening of projected length; and the other from the variation of perpendicular ion track etch-pit aperture. It was possible to correlate the aperture and length reduction with a power law. Apparently, the etch-pit aperture seems to be an indicator of the amount of defects which remains in the latent track after the thermal treatment. This enables one to better constrain the thermal annealing kinetic. Some geological extrapolation were also predicted. The reasonable agreement with geological data demonstrates that the process is universal and that ion tracks can be used as proxies for the thermal annealing behavior study / Doutorado / Física / Doutor em Ciências

The use of pre-hardened mold steels has increased appreciably over the years; more than 80% of the plastic mold steels are used in pre-hardened condition. These steels are delivered to the customer in finished state i.e. there is no need of any post treatment. With hardness around ~40HRC, they have properties such as good polishability, good weldability, corrosion resistance and thermal conductivity. Machinability is a very important parameter in pre-hardened mold steels as it has a direct impact on the cost of the mold. In normal machining operations involving intricate or near net shapes, machining constitutes around 60% of the total mold cost. Efforts are underway to explore every possible way to reduce costs associated with machining and to make production more economical. All the possible parameters which are considered to affect the machinability are being investigated by the researchers. This thesis work focuses on the effect of prior austenite grain size on the machinability of pre-hardened mold steel (Uddeholm Nimax).  Austenitizing temperatures and holding times were varied to obtain varying grain sized microstructures in different samples of the same material. As it was difficult to delineate prior-austenite grain boundaries, experimental and empirical methods were employed to obtain reference values. These different grain sized samples were thereafter subjected to machining tests, using two sets of cutting parameters. Maximum flank wear depth=0.2mm was defined for one series of test which were more akin to rough machining, and machining length of 43200mm or maximum wear depth=0.2mm were defined for second series of tests which were similar to finishing machining. The results were obtained after careful quantative and qualitative analysis of cutting tools. The results obtained for Uddeholm Nimax seemed to indicate that larger grain sized material was easier to machine. However, factors such as retained austenite content and work hardening on machined surface, which lead to degradation of machining operations were also taken into consideration. Uddeholm Nimax showed better machinability in large grained samples as retained austenite(less than 2%) content was minimal in the large grained sample. Small grained sample in Uddeholm Nimax had a higher retained austenite (7+2%) which resulted in degradation of machining operation and a lesser cutting tool life.

Ziel ist die räumliche Abbildung biologischer Materialien (Knochen, Kollagenfibrillen und Zähne) hinsichtlich deren Struktur auf der Nanometerskala mit Hilfe der Nanotomographie. Die Nanotomographie ist eine moderne dreidimensionale Volumenabbildungsmethode auf der Nanometerskala basierend auf der Rasterkraftmikroskopie. Für die Nanotomographie wurden Ätzprotokolle an Zähnen, Kollagenfibrillen und Knochen entwickelt, die einen gleichmäßigen Abtrag bewirken. Lineare Verschiebungen der aufgenommenen Schichten werden mit Hilfe der manuellen Registrierung korrigiert und zu einem Volumenbild rekonstruiert. Ein zentrales Ergebnis sind dabei erste hochaufgelöste Volumenbilder einzelner Kollagenfibrillen im nativen Knochen. Neben der konventionellen Nanotomographie wird ein Ansatz zur automatisierten Nanotomographie mit einer Auflösung von 10 nm am Beispiel des menschlichen Knochens und Zahnes demonstriert. Mit Hilfe von mikroskopischen und elektronenmikroskopischen Techniken wurden die verschiedenen Strukturebenen des humanen Zahn und Knochens abgebildet und die räumlichen Strukturen der TM-AFM-Bilder auf der Mikro- und Nanometerskala eingeordnet. Darüber hinaus konnte mit Hilfe analytischer Messmethoden die chemische Zusammensetzung des kortikalen nativen Knochens erfasst werden und Änderungen durch das Ätzen detektiert werden.