Cette étude fait partie du projet ANR DEFISURF, avec pour objectif d'identifier et de modéliser les divers effets de la surface sur la tenue en fatigue de composants forgés. Deux composants sont étudiés: une éprouvette extrudée à froid et une bielle estampée à chaud et nettoyée de sa calamine par grenaillage (shot-blasting). Pour chaque composant, différents lots sont étudiés afin de quantifier l'effet des procédés sur les caractéristiques mécaniques et sur le comportement en fatigue. Deux taux de corroyage différents sont utilisés pour l'extrusion à froid. Pour les bielles, différents grenaillages sont réalisés pour obtenir divers états de surface.Les différents lots sont caractérisés de façon approfondie et des essais de fatigue sont effectués. Des essais de fatigue en traction, torsion et flexion plane sont réalisés sur les éprouvettes extrudées. Des éprouvettes de fatigue sont prélevées dans l'âme des bielles et sollicitées en flexion plane.En extrusion à froid, les aspects les plus influents en fatigue sont la prédéformation subie lors de la mise en forme (taux de corroyage) et les contraintes résiduelles. En forgeage à chaud, ce sont les défauts de forgeage en surface et les contraintes résiduelles introduites par le grenaillage qui ont le plus d'influence.Une modélisation en fatigue est proposée pour chaque composant. Pour l'extrusion, un critère de fatigue multiaxial permet de prendre en compte les différents types de chargement ainsi que l'effet des contraintes résiduelles. Pour les bielles deux approches sont utilisées. La première est une analyse de la géométrie des défauts qui utilise un demi-ellipsoïde pour approximer leur forme. La deuxième approche est une simulation numérique par éléments finis des défauts critiques. Les contraintes résiduelles sont intégrées dans les simulations avec un critère multiaxial. Les simulations permettent de retrouver les résultats expérimentaux avec une erreur d'environ 15%. / This study is part of the DEFISURF project, with the goal of analysing and modelling the various effects of the surface on the fatigue strength of forged components. Two components are studied: a cold-extruded specimen and a connecting rod which is hot-forged and then cleaned by shot-blasting. For each component, different batches are studied in order to quantify the effects of the process on the mechanical characteristics and the fatigue behaviour. Two different reduction of sections are used for the cold-extruded specimens and shot-peening is used to obtain various surface states for the connecting rods.The various batches are thoroughly characterised and fatigue tests are performed. Traction, torsion and plane-bending tests are conducted on the cold-extruded specimens. Fatigue specimens are machined from the central part of the connecting rods and loaded in plane-bending.For cold-extrusion, the parameters with the most influence in fatigue are the prestrain induced during forging and the residual stresses. In hot-forging, the surface defects produced during forging and the residual stresses induced by the shot-blasting have the most influence.For each component, a fatigue model is suggested. For the cold-extruded specimens, a multiaxial fatigue criterion is used to take into account the various fatigue loadings and the effect of the residual stresses. Two approaches are used for the connecting rods. The first is a geometrical analysis of the defect which approximates them with an ellipsoid. The second approach uses finite element simulations of the critical defects. The shot-peening residual stresses are integrated in the simulations with a multiaxial criterion. These simulations predict the fatigue limit of the specimens with an error of around 15%.

The goal of this thesis is to create overall, automatic and non-contact quality control of a pellet. The issue is divided into two separate parts. The first part deals with precise dimensional measuring of pellet - its length and head diameter so that it is precise and reasonably fast. Precise measuring is achieved with help of algorithms which achieve the sub-pixel precision by polynomial approximation of the edges extracted from the image gradients. The second part deals with the defects of a pellet. Detecting defects like longitudinal furrows or skirt cuts is achieved with convolutional neural networks. The measurement modules work with the resulting precision up to 0.025 mm in case of length measuring and up to 0.01 mm in case of head diameter measuring. In case of defect detections, neural network shows very high classification success rate. The contribution of this thesis is a presentation of innovative approaches in automatic quality control of pellets with use of neural networks and a demonstration of its usage in real manufacturing process.

Cette thèse contribue à l’étude des effets géants et anormaux de piézo-résistance (PZR) observés dans le nano-silicium. La PZR du silicium massif est devenue la clé de voûte de nombreuses technologies dont l’industrie micro-électronique vise des dispositifs de dimensions nanométriques. Il est donc logique d’investiguer la PZR du silicium à ces échelles spatiales où ont été révélé l’existence d’une PZR géante et d’une PZR d’amplitude « normale » mais de signe anormale. Cependant l’origine de ces effets reste peu claire et dans certains cas, leur véracité a été remise en cause. L’ensemble de ces effets semble corrélé à un appauvrissement en porteurs libres où le courant devient limité par la charge d’espace (en anglais SCLC). Pour mettre en lumière la dépendance en contrainte mécanique des taux de capture et d’émission de porteurs libres sur des pièges liés aux défauts cristallins, nous utilisons la technique de spectroscopie d’impédance qui, alliée à la spectroscopie de photoémission, suggère que les pièges en question sont ceux liés aux défauts intrinsèques de surface. La PZR géante n’est observée qu’en dehors du régime stationnaire. Dans le régime stationnaire dans laquelle se situe l’ensemble des études précédentes, bien qu’une PZR géante ne soit pas observée, une PZR de signe anormale est mesurée dans le silicium où une densité de défauts bien choisis a été introduite. Nous démontrons que cette dernière est due à un changement de type de porteur majoritaire induit par la tension appliquée en régime SCLC. Le chapitre 1 aborde l’historique de la PZR jusqu’aux observations de la PZR géante et anomale dans le nano-silicium. Le chapitre 2 présente les modèles physiques de la PZR en régime ohmique. La théorie des SCLCs est ensuite introduite. Le chapitre 3 présente les dispositifs expérimentaux, les procédures de mesure ainsi que les échantillons étudiés. Le chapitre 4 contient les principaux résultats obtenus par la spectroscopie d’impédance. Une PZR géante et nouvel effet de piézo-capacitance sont observés. Une comparaison avec la théorie indique que les dispositifs opèrent dans une régime SCLC en présence de pièges électroniques rapides, et que la PZR géante résulte de la dépendance en contrainte des taux de capture et d’émission de ces pièges. Ceci donne lieu à des changements importants de densités de porteurs hors du régime stationnaire. Ce chapitre se termine sur une discussion, revisitée à la lumière de nos résultats, des effets controversés de PZR géante publiés dans la littérature. Le chapitre 5 traite la mesure de la dépendance en contrainte du « pinning » du niveau de Fermi de surface, réalisée en combinant cartographie Raman et photoémission sur des leviers en silicium statiquement fléchis dont les surfaces sont terminées par une oxyde native. L’observation d’un déplacement du niveau de Fermi de surface pair en contrainte tend à montrer que les défauts intrinsèques de surface (type Pb0) sont à l’origine des effets géants présentés dans le chapitre 4.Le chapitre 6 aborde les mesures en régime stationnaire de PZR du silicium n.i.d. de type n pour laquelle une densité de bi-lacunes de silicium a été introduite. La caractéristique courant-tension montre trois régimes : à basse tension une loi ohmique dominé par les électrons majoritaires ; à des tensions intermédiaires une loi de Mott-Gurney modifiée des trous injectés depuis les contacts p++ ; à haute tension un régime plasma électron-trou. La PZR est déterminée par le porteur majoritaire. A basse tension un comportement du silicium type n est observé (i.e. de signe négatif) tandis qu’aux tensions intermédiaires une PZR similaire à celle du silicium type p est observée (i.e. de signe positive). A haute tension la PZR correspond à la somme de ces, conséquence directe de la présence d’électrons et de trous dans le régime plasma. Le chapitre 7, tout en résumant les conclusions principales de cette thèse développe également les directions futures à explorer. / This thesis presents a study of giant, anomalous piezo-resistance (PZR) in depleted nano-silicon. PZR in bulk silicon is a technologically important phenomenon in which mechanical stress changes the electrical resistivity via a change in the charge carrier effective masses. With continued reductions in device dimensions, it is of interest to explore the PZR of silicon micro- and nano-objects in which giant PZR and PZR of anomalous sign have been reported in recent years. The physical origin of these effects remains unclear and in some cases, even the veracity of the claimed results has been questioned. Some basic elements of the claimed effects are agreed upon, for example they occur in surface depleted nanostructures where transport is described by space charge limited currents (SCLC). In this thesis the details of the stress-dependence of the charge trapping and emission rates at fast electronic traps during SCLC transport in fully depleted silicon-on-insulator is probed using impedance spectroscopy. This, combined with an X-ray photo-electron spectroscopy study of statically deflected silicon cantilevers, strongly suggests that giant, non-steady-state PZR is due to stress-induced changes to hole trapping dynamics at intrinsic interface states. In contrast, under steady-state conditions like those used in all previous studies, giant PZR is not observed even in the presence of interface traps. On the other hand, anomalous, steady-state PZR is observed in defect engineered SCLC devices, and is shown to be the result of a voltage bias induced type change of the majority carrier. In chapter 1 the history of PZR is introduced. Prior reports of giant and anomalous PZR are then discussed. Chapter 2 presents the physical description of the PZR in silicon when transport occurs in the Ohmic regime. Both large-signal and small-signal SCLC transport are then introduced. Chapter 3 introduces the experimental details and the samples used throughout this work. Chapter 4 contains the principal impedance spectroscopy results. Giant, anomalous PZR and a novel piezo-capacitance are observed under non-steady-state conditions in fully-depleted silicon-on-insulator. Comparison of theory and data indicate that the devices operate in the SCLC regime in the presence of fast traps, and that the giant, anomalous PZR results from the stress dependence of the charge capture and emission rates of these traps. This in turn yields large changes of the non-equilibrium charge carrier concentrations. The importance of these observations in clarifying the physical origin, and the veracity of previous reports of steady-state, giant PZR, is discussed. Chapter 5 reports a comparison of Raman and XPS maps on statically deflected silicon cantilevers, providing a spectroscopic measurement of the stress-dependence of the pinned surface Fermi level at natively oxidized (001) silicon surfaces. A simplified analysis of the observed even symmetry of the stress-induced Fermi level shifts suggests that intrinsic interface defects (Pb0) are likely responsible for the giant, anomalous PZR reported in Chapter 4. Chapter 6 reports the DC bias dependence of the PZR in n.i.d. n-type, defect engineered silicon devices. The device characteristic exhibits three regimes; an Ohmic regime at low biases dominated by equilibrium electrons, a modified Mott-Gurney regime at intermediate biases dominated by holes injected from p++ contacts, and an electron-hole plasma regime at high biases. In each case the PZR depends on the majority carrier type; at low biases the usual n-type PZR is observed (i.e. the sign is negative); at intermediate biases it switches to the bulk p-type (i.e. positive) PZR; in the plasma regime, the PZR is a combination of the bulk electron and hole values. The results help shed light on observations of anomalous (i.e. sign reversed) PZR in depleted nano-silicon. Finally, chapter 7 summarizes the conclusions and introduces possible future research directions.

This master thesis studies the behaviour of two aluminium alloys in ultrasonic cleaning at two different intensities, as well as the effect of a cleaning solution, Formula 815 GD-NF on the same surface have been studied with respect to surface roughness and material composition. Methods like Light Optical Microscopy (LOM), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and 3D topography using white light interferometry (VSI) was used to study the surface and material composition. It was found that both the ultrasonic cleaning, as well as the solution itself both increase surface roughness of the samples. When crossing a threshold in ultrasonic intensity micro jet cavitation dislodge precipitates, or areas weakened by precipitate to form a large pit. And the following heat from the jet causes the surface to oxidise, becoming more brittle, and be broken up by other cavitation phenomena to cause rapid acceleration of surface roughness in an area originating from the pit.

No description available.

In der vorliegenden Arbeit wurden facettierte Nanolegierungen aus Gold und Palladium in der Größenordnung von 1 – 3 nm synthetisiert und charakterisiert. Die Synthese erfolgte in sphärischen Polyelektrolytbürsten (SPB), welche als Stabilisatorsystem fungierten. Die Strukturaufklärung erfolgte mittels hochauflösender Transmissionselektronenmikroskopie (HR-TEM) und Extended X-ray Absorption Fine Structure (EXAFS) Spektroskopie. Die Nanolegierungen wurden als Katalysatoren zur Reduktion von 4-Nitrophenol verwendet, wobei eine gesteigerte katalytische Aktivität, im Vergleich zu monometallischen Nanopartikeln, beobachtet wurde. Im HR-TEM wurden auf den Kanten der Metallkristalle Oberflächendefekte in Form von Stufen sichtbar, wobei eine Korrelation der Oberflächendefekte zur katalytischen Aktivität hergestellt wurde. Durch EXAFS-Analysen konnte nachgewiesen werden, dass eine Zusammensetzung von 75 mol-% Gold und 25 mol-% Palladium annähernd eine statistische Mischung aufweist. Mit steigendem Palladiumgehalt wurde eine leichte Anreicherung von Palladium an der Oberfläche der Partikel, sowie nichtmetallisches Palladium der Oxidationsstufe 2+ gefunden. Diese unterschiedliche Anordnung der Elemente für verschiedene Zusammensetzungen korreliert ebenfalls mit der katalytischen Aktivität. Ferner konnte eine Kontraktion des Netzebenenabstands für kleine Partikel mittels EXAFS nachgewiesen werden. Bei der Verwendung als Katalysatoren wurde eine zeitliche Reaktionsverzögerung festgestellt, welche auf die Oberflächenrestrukturierung der Metallnanopartikel hinweist. Zusätzlich konnte durch den Vergleich von SPB stabilisierten und stabilisatorfreien Goldnanopartikeln festgestellt werden, dass das SPB System die katalytische Aktivität nicht signifikant beeinträchtigt. / In this work facetted gold-palladium nanoalloys have been synthesized and characterized in the range of 1 – 3 nm. The spherical polyelectrolyte brushes (SPB) have been used during synthesis and for stabilization of the nanoparticles. Structural analyses have been done by high resolution transmission electron microscopy (HR-TEM) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The nanoalloys have been used as catalysts for the reaction of 4-nitrophenol, where an enhanced catalytic activity has been found compared to monometallic nanoparticles. Surface defects are visible by steps at the edge of the metallic crystal where a correlation of these surface defects and the catalytic activity has been found. By EXAFS spectroscopy an almost statistic mixture for a composition of 75 mol-% gold and 25 mol-% palladium, slight enrichment of palladium at the surface of the particle, and the presence of nonmetallic palladium with an oxidation number of 2+ has been observed. This different atomistic arrangement correlates with the catalytic activity as well. In addition, a contraction of the lattice parameter has been observed for small particles by EXAFS measurements. Using the nanoalloys as catalyst, a delay time for the reaction has been found which indicates a restructuring of the surface of the metal nanoparticles. By comparison of SPB stabilized and support-free gold nanoparticles no significant influence of the SPB system on the catalytic activity has been observed.

In industrial use of paint systems a swift processing is crucial. Another very important issue is to improve the quality of the final coating. This report investigates the film formation process of powder coatings, specially the spreading of individual powder particles. The obtained results can be used to understand and control the film formation process. In this way the desired levelling can be achieved and thus the desired gloss or other surface characteristics that may be required. This means that the method could be used when evaluating different polymer and additive combinations that could be used to change film formation behaviour or curing time for powder coating systems to suit various substrates. It makes it possible to avoid and minimize different surface defects as orange peel or cratering in the powder coated film. We used a reflection optical microscope to better understand the film formation process and especially the spreading of a powder melt on surfaces with various surface energies. The obtained data were: the particle diameter, the area, area ratio and the contact angle of the powder particle as a function of time and temperature. This information can be used to derive the surface tension of any powder melt. In this report we evaluate the dependencies of temperature, heat rate and surface energy for powder coatings on different substrates. The method provides information that can be used to optimize the film formation of a specific powder coating/substrate combination. This method can be used to evaluate the powder spreading and levelling on different substrates from a surface tension point of view. We found, as expected, that the powder flows out on a hydrophilic surface and is inhibited by a hydrophobic. The increase of the area ratio on a hydrophilic surface was about five times as the initial area coverage and on a hydrophobic surface only two times the initial area coverage. The contact angle between the melted powder particle on the different surface types could be calculated. The melt surface tension could be calculated since three substrates surfaces with various surface energies were used. The melt surface tension was found to be about 18.5 mN/m. / Sammanfattning Vid industriell användning av ett färgsystem är det viktigt med en snabb och smidig målningsprocess. En viktig del är att förbättra kvaliteten på den färdiga ytan. Denna rapport undersöker filmbildningsprocessen för pulverfärg, närmare bestämt spridningen av individuella pulverpartiklar. Resultaten från utvärderingen av denna metod kan användas för att bättre förstå och få kontroll över filmbildningsprocessen. Med denna undersökningsmetod kan den önskade utslätningen uppnås och därmed den önskade glansen eller annan yteffekt som kan vara önskvärd. Metoden kan användas för att utvärdera olika polymer- och additivkombinationer som kan användas för att ändra filmbildningens uppförande eller bestämma härdningstiden för en pulverfärg att passa ett visst substrat. Metoden gör det möjligt att förhindra och minska olika ytdefekter såsom apelsinskals- eller kratereffekter i pulverfärgens yta. Ett optiskt reflectionsmikroskop användes för att bättre kunna förstå filmbildningsprocessen och särskilt spridningen av smält pulver på substrat med olika ytenergier. De mätdata vi fick var partikeldiameter, area, areaförändring och kontaktvinkeln för pulverpartiklar som funktion av tid och temperatur. Ur denna information kunde pulversmältans ytenergier härledas. I denna rapport utvärderas pulvrets beroende av temperatur, uppvärmning och ytenergi på olika substrat. Denna metod ger information som kan användas för att optimera filmbildningen av en specifik kombination av pulverfärg och substrat. Denna metod kan också användas för att utvärdera pulverspridning och utjämning av färgfilmen på olika substrat med avseende på ytenergierna. Som förväntat flyter pulvret ut på hydrofila ytor och utflytningen ändras på en hydrofob yta. På en hydrofil yta sprider sig partikeln till fem gånger den ursprungliga arean över substratet och motsvarande två gånger för en hydrofob yta. Kontaktvinkeln mellan en smält pulverpartikel på olika sorters substrat från utförda mätningar beräknas utifrån utförda mätningar. Kontaktvinklar mellan pulver och olika substrat kan användas för att beräkna smältans ytspänning. Smältans ytspänning kan beräknas då experiment gjorts på tre sorters ytor med olika kända ytenergier. Smältans ytspänning var 18,5 mN/m. Slutsatsen är att det går att observera och utvärdera resultaten av utsmältningsförloppet för pulverfärg med denna metod.

[pt] O presente trabalho se baseia na teoria dos defeitos equivalentes, também conhecida como teoria de Murakami, que permite a predição da vida-fadiga de materiais estruturais adotando o parâmetro (raiz quadrada de area), responsável por uma equivalência quantitativa entre heterogeneidades microestruturais (inclusões metalúrgicas) existentes na região de análise do material e descontinuidades mecânicas (furos) usinados nos corpos de prova. Neste contexto, a tese propõe novas equações, a partir da teoria de Murakami, para prever falhas por fadiga em carregamentos ultralongos (fadiga de altíssimo ciclo, VHCF) do aço DIN42CrMo4, de larga aplicação na fabricação de eixos virabrequins para unidades geradoras de usinas termoelétricas. Corpos de prova do aço DIN42CrMo4 foram usinados com furos de diâmetros variando entre 0,18 mm e 0,70 mm e ensaiados num regime de fadiga de altíssimo ciclo, variando o valor da amplitude de tensão do ensaio, para assim determinar em quais condições o material falha e obter a curva experimental S-N do aço DIN42CrMo4 na presença de diferentes tamanhos de defeitos (furos). Os resultados experimentais permitiram o desenvolvimento de equações em função do parâmetro e curvas de Wohler do material, em conformidade com diferentes descontinuidades mecânicas nos corpos de prova e resistências à fadiga do material. Consequentemente, se estabeleceu uma metodologia que permite uma correlação entre inclusões metalúrgicas, tensão aplicada e vida superlonga em fadiga de eixos virabrequins em serviço em usinas termoelétricas. / [en] The present work is based on the theory of equivalent defects, also known as Murakami s theory, which allows the prediction of the fatigue life of structural materials by adopting the parameter (square root of area), responsible for a quantitative equivalence between microstructural heterogeneities (metallurgical inclusions) existing in the region analysis of the material and mechanical discontinuities (holes) machined in the specimens. In this context, the thesis proposes new equations, based on Murakami s theory, to predict fatigue failures in ultralong loads (very high cycle fatigue, VHCF) of DIN42CrMo4 steel, widely used in the manufacture of crankshafts for generating units of thermoelectric power plants. DIN42CrMo4 steel specimens were machined with holes with diameters varying between 018 mm and 0.70 mm and tested in a very high cycle fatigue regime, varying the value of the test stress amplitude, to determine under what conditions the material failure and obtain the experimental S-N curve of DIN42CrMo4 steel in the presence of different sizes of defects (holes). The experimental results allowed the development of equations as a function of the parameter and Wohler curves of the material, in accordance with different mechanical discontinuities in the test specimens and resistance to fatigue of the material. Consequently, a methodology was established that allows a correlation between metallurgical inclusions, applied stress and super-long fatigue life of crankshafts in service in thermoelectric power plants.