For the commercial success of polymer - multiwalled carbon nanotube (MWNT) composites the production of these materials on industrial scale by melt processing is of significant importance. The complete dispersion of primary MWNT agglomerates in a polymer melt is difficult to achieve, making it an important and challenging technological problem. Hence, it is necessary to understand the process of MWNT agglomerate dispersion in a polymer melt. Based on an intensive literature research on mechanisms and influencing factors on dispersion of other agglomerated nanostructured fillers (e.g. carbon black), the main dispersion steps were evaluated and investigated concerning the agglomerated MWNT.Consequently, systematic investigations were performed to study the effect of the melt infiltration on MWNT agglomerate dispersion and to analyse the corresponding main dispersion mechanisms, namely rupture and erosion. The states of MWNT agglomerate dispersion were assessed by quantifying the agglomerate area ratio and particle size distribution using image analysis of optical transmission micrographs. Additionally, the composite’s electrical resistivity was determined. In the prevailing study, polycarbonates (PC) varying in molecular weight were used to produce composites containing 1 wt% MWNT (Baytubes C150HP) as model systems and a discontinuous microcompounder was applied as melt mixing device. The agglomerate structure of the used MWNT material made them especially suitable for the reported investigations. The step of melt infiltration into the primary nanotube agglomerates plays a crucial role for their dispersion in the PC melt. During melt mixing when low shear rates were applied, better state of MWNT dispersion was obtained in high viscosity matrices because applied shear stresses were high. On the contrary, if high shear rates were applied, similar states of MWNT dispersion were obtained in low and high viscosity matrices although significantly lower shear stresses were applied in the low viscosity matrix as compared to the high viscosity matrix. The results indicate that if the applied shear stress values are compared, with increasing matrix viscosity the agglomerate dispersion gets worsen. This is attributed to the fact that low viscosity matrices can infiltrate relatively faster than high viscosity matrices into the agglomerate making them weaker and reducing the agglomerate strength. Thus, at sufficient shear rates MWNT agglomerates disperse relatively faster in low viscosity matrix. This illustrates a balance between the counteracting effects of viscosity on agglomerate infiltration and agglomerate dispersion. Additionally, the effect of matrix molecular weight on the size of un-dispersed MWNT agglomerates was investigated. Under similar conditions of applied shear stress, the composites based on low molecular weight matrix showed smaller sized un-dispersed primary agglomerates as compared to composites with higher molecular weight matrices. This again highlights the role of matrix infiltration as the first step of dispersion. Following the step of melt infiltration, agglomerate size gets reduced due to the dispersion mechanisms. To analyse the corresponding contributions of different dispersion mechanisms (rupture and erosion), the kinetics of MWNT agglomerate dispersion was investigated. If high mixing speeds are employed dispersion is quite fast and needs less time as compared to low mixing speed. A model is proposed to estimate the fractions of rupture and erosion mechanisms during agglomerate dispersion based on the kinetic study in the discontinuous mixer. Under the employed experimental conditions, at high mixing speeds, the dispersion was found to be governed by rupture dominant mechanism, whereas at low mixing speeds the dispersion was controlled by both mechanisms. As far as electrical resistivity is concerned, for a given content of MWNT as the state of dispersion improves, the resistivity values decrease significantly but only up to a plateau value. The composites produced using low viscosity matrices have lower resistivity values as compared to high viscosity matrices. Additionally, composites were prepared using additives, whereas the additives were found to be useful for improving filler dispersion and electrical conductivity.

The diploma thesis aims to analyze bent FRP reinforcements. It describes the method of production of bent FRP reinforcement, examples of application of FRR reinforcement in structures and mentions aggressive influences influencing the durability of FRP reinforcement. Furthermore, an experiment is proposed to monitor changes in straight and bent FRP reinforcement stored in an aqueous environment at 20 °C and an alkaline environment at 20 °C and 40 °C. The output of the diploma thesis is the evaluation of changes in mechanical properties and durability. The condition of the FRP reinforcement is documented using optical and electron mocroscopy.

A fairly new technology used to produce metallic components is powder metallurgy (PM). Among the advantages with this technique are decreased cost of production for complex-shaped parts, new alloys are made possible, reduced end processing, less material loss, and vibrational damping effects. The downside is the number of pores created which can alter the tribological properties of the material. The focus of this report is to investigate how lean PM steel behaves under tribological contacts.  Friction and wear will be investigated using a pin-on-disc setup to mimic the sliding part of a gear tooth mesh. Previous studies show that the amount of wear, and if the wear increases or decreases with increased density is dependent on the degree of porosity and the pore size. This means that the wear might be minimized by optimizing the number of pores in the material and their shape and size. The result of this study shows that the friction coefficient decreases with increasing density. The wear coefficient show signs of the same correlations but further tests are needed. The main wear comes from adhesive wear, with signs of abrasive wear. The amount of abrasive wear seems to increase with an increase in density, supporting previous studies claiming that pores can trap wear debris and decrease the number of abrasive particles in the contact.

Cellulose is the most abundant biopolymer on Earth as it is found in every plant cell wall; therefore, it represents one of the most promising natural resources for the fabrication of sustainable materials. In plants, cellulose is mainly used for structural integrity, however, some species organise cellulose in helicoidal nano-architectures generating strong iridescent colours. Recent research has shown that cellulose nanocrystals, CNCs, isolated from natural fibres, can spontaneously self-assemble into architectures that resemble the one producing colouration in plants. Therefore, CNCs are an ideal candidate for the development of new photonic materials that can find use to substitute conventional pigments, which are often harmful to humans and to the environment. However, various obstacles still prevent a widespread use of cellulose-based photonic structures. For instance, while the CNC films can display a wide range of colours, a precise control of the optical appearance is still difficult to achieve. The intrinsic low thermal stability and brittleness of cellulose-based films strongly limit their use as photonic pigments at the industrial scale. Moreover, it is challenging to integrate them into composites to obtain further functionality while preserving their optical response. In this thesis, I present a series of research contributions that make progress towards addressing these challenges. First, I use an external magnetic field to tune the CNC films scattering response. Then, I demonstrate how it is possible to tailor the optical appearance and the mechanical properties of the films as well as to enhance their functionality, by combining CNCs with other polymers. Finally, I study the thermal properties of CNC films to improve the retention of the helicoidal arrangement at high temperatures and to explore the potential use of this material in industrial fabrication processes, such as hot-melt extrusion.

Die vorliegende Arbeit befasst sich mit der Synthese und der Untersuchung von Struktur-Eigenschaftsbeziehungen neuartiger V-förmiger, formstabiler Mesogene zur Realisierung biaxial nematischer Mesophasen (Nb). Alle synthetisierten Verbindungen besitzen ein formtreues Oligo(phenylenethinylen)-Grundgerüst, an welches laterale Alkyloxyketten und verschiedene terminale Substituenten (z. B. -CN, O(CH2)nCOOEt, Pyridyle) angebunden wurden. Durch dieses spezielle Design erhält man ausschließlich nematische und keine höher geordneten flüssigkristallinen Phasen. Durch den Einsatz verschiedener zentraler heterozyklischer Kernbausteine konnten erfolgreich Öffnungswinkel zwischen 108.9° und 160° realisiert werden. Dabei zeigen Thiadiazolderivate stets enantiotrope Mesophasen, wobei im Hochtemperaturbereich eine uniaxiale Phase mit biaxialen Aggregaten vorliegt. Beim Abkühlen konnte bei etwa 50 °C mittels Polarisationsmikroskopie und dielektrischer Spektroskopie ein Übergang in die Nb-Phase nachgewiesen werden. Die erstmalige Beobachtung eines direkten Übergangs von der isotropen Phase in die Nb-Phase gelang durch den Einsatz von Benzo[1,2-b:4,3-b]dithiophen als Kernbaustein.

Die vorliegende Arbeit befasst sich mit der Synthese und der Untersuchung von Struktur-Eigenschaftsbeziehungen neuartiger V-förmiger, formstabiler Mesogene zur Realisierung biaxial nematischer Mesophasen (Nb). Alle synthetisierten Verbindungen besitzen ein formtreues Oligo(phenylenethinylen)-Grundgerüst, an welches laterale Alkyloxyketten und verschiedene terminale Substituenten (z. B. -CN, O(CH2)nCOOEt, Pyridyle) angebunden wurden. Durch dieses spezielle Design erhält man ausschließlich nematische und keine höher geordneten flüssigkristallinen Phasen. Durch den Einsatz verschiedener zentraler heterozyklischer Kernbausteine konnten erfolgreich Öffnungswinkel zwischen 108.9° und 160° realisiert werden. Dabei zeigen Thiadiazolderivate stets enantiotrope Mesophasen, wobei im Hochtemperaturbereich eine uniaxiale Phase mit biaxialen Aggregaten vorliegt. Beim Abkühlen konnte bei etwa 50 °C mittels Polarisationsmikroskopie und dielektrischer Spektroskopie ein Übergang in die Nb-Phase nachgewiesen werden. Die erstmalige Beobachtung eines direkten Übergangs von der isotropen Phase in die Nb-Phase gelang durch den Einsatz von Benzo[1,2-b:4,3-b]dithiophen als Kernbaustein.

This thesis work was conducted at Luleå University of Technology in collaboration with Sandvik Rock Tools. The aim of the work was to determine the influence of carbon content on the wear performance in carburized steel in the dry contact interface of threaded connections between drill rods. In order to investigate this, samples of drill rod steel were carburized to three different carbon concentrations and shot peened to replicate the production process of a drill rod. The samples were wear tested by utilizing a twin-disc wear tester with one disc rotating at 100 RPM and the other at 3000 RPM to mimic the operating conditions in the threaded connection between drill rods. The results was evaluated by wear rate, surface topography, hardness as well as optical analysis by light optical microscopy and scanning electron microscopy. The results show that an increased surface carbon content provide a decrease in wear rate and an increase in hardness in the surface layer that undergo microstructural changes due to the frictional heat and contact pressure during wear testing. The primary wear mechanisms were identified as plastic deformation, adhesive scratching and material removal through delamination.

[ES] La tomografía por difracción surge para mejorar las técnicas de imagen al considerar la naturaleza ondulatoria de la luz. Mientras que los primeros sistemas de imagen médica se basaban únicamente en fuentes sin difracción, este enfoque consigue mejorar la reconstrucción del índice de refracción de los objetos, lo que permite, por ejemplo, el estudio de estructuras subcelulares. Del mismo modo, la demanda de redes de telecomunicaciones cada vez más rápidas y seguras ha propiciado la aparición de la fotónica. Hace dos décadas, la combinación de estos dos campos dio lugar a los primeros sistemas de tomografía por difracción óptica (ODT), los cuáles han evolucionado rápidamente durante este siglo. En esta tesis, presentamos dos nuevas aplicaciones de la ODT. La primera está relacionada con el concepto del microscopio tomográfico de fase (TPM), una versión de la ODT que permite el estudio de células aisladas, con muchas aplicaciones biomédicas, como el diagnóstico y la prognosis del cáncer. Sin embargo, los sistemas TPM actuales son caros, pesados y complejos. Para resolver estos problemas, proponemos el concepto de TPM en chip. Con este fin, diseñamos una hoja de ruta hacia el primer dispositivo tomográfico integrado en el marco de la tecnología lab-on-a-chip (LoC), y desarrollamos los primeros pasos para ello: 1) Hasta ahora, sólo se han utilizado detectores planos para obtener los mapas de índice de refracción de los objetos estudiados en TPM, basados en la detección del campo difractado hacia delante. Sin embargo, los principios físicos fundamentales indican que medir también el campo difractado hacia detrás debería mejorar la resolución de las imágenes. Además, un detector plano no es la configuración óptima para el TPM en chip. En esta línea, hemos explorado la posibilidad de usar detectores circulares en este escenario, como una técnica más adecuada para las configuraciones en chip, demostrando al mismo tiempo que este enfoque proporciona una mejor resolución que el lineal. 2) Proponemos un esquema de TPM en chip basado en el uso de nanoantenas dieléctricas como fuente de luz y píxeles detectores ODT, y caracterizamos experimentalmente su comportamiento mediante microscopía óptica de campo cercano. En cuanto a la segunda aplicación, estudiamos el potencial de la ODT como nuevo paradigma en la detección de capas de invisibilidad realistas, una de las aplicaciones más importantes de los metamateriales. Hasta ahora, el scattering cross section (SCS) se ha utilizado como modelo de referencia para diseñar y observar la eficacia de estos dispositivos para ocultar objetos. En nuestro estudio, demostramos que la ODT puede detectar las capas de invisibilidad prácticas con una sensibilidad superior a la que ofrece el SCS, incluso a las frecuencias de trabajo óptimas. Además, es posible obtener una imagen representativa del tamaño y la forma de la capa, revelando claramente su existencia. Finalmente, se discuten las conclusiones extraídas de los resultados obtenidos. Además, se detallan las futuras líneas de trabajo para abordar los retos que no se han completado en esta tesis doctoral. / [CA] La tomografia per difracció sorgeix per millorar les tècniques d'imatge anteriors en considerar la naturalesa ondulatòria de la llum. Mentre que els primers sistemes d'imatge mèdica es basaven únicament en fonts sense difracció, aquest enfocament aconsegueix millorar la reconstrucció de l'índex de refracció dels objectes, la qual cosa permet, per exemple, l'estudi d'estructures subcelulars. De la mateixa manera, la demanda de xarxes de telecomunicacions cada vegada més ràpides i segures ha propiciat l'aparició de la fotònica. Fa dues dècades, la combinació d'aquests dos camps va portar als primers sistemes de tomografia per difracció òptica (ODT), els quals han evolucionat ràpidament durant aquest segle. En aquesta tesi, presentem dues noves aplicacions de la ODT. La primera està relacionada amb el concepte del microscopi tomogràfic de fase (TPM), una versió de la ODT que permet l'estudi de cèl·lules aïllades, amb moltes aplicacions en biomedicina, com el diagnòstic i prognosi del càncer. No obstant això, els sistemes TPM actuals són cars, pesats i complexos. Per resoldre aquests problemes, proposem el concepte de TPM en xip. Per fer-ho, dissenyem un full de ruta cap al primer dispositiu tomogràfic integrat en el marc de la tecnologia lab-on-a-chip (LoC), i desenvolupem els primers passos a aquest efecte: 1) Fins ara, només s'han utilitzat detectors plans per a obtindre els mapes d'índex de refracció dels objectes estudiats en TPM, basats en la detecció del camp difractat cap avant. No obstant això, els principis físics fonamentals indiquen que mesurar també el camp difractat cap endarrere hauria de millorar la resolució de les imatges. A més, un detector pla no és la configuració òptima per al TPM en xip. En aquesta línia, hem explorat la possibilitat d'usar detectors circulars en aquest escenari, com una tècnica més adequada per a les configuracions en xip, demostrant al mateix temps que aquest enfocament proporciona una millor resolució que el lineal. 2) Proposem un esquema de TPM en xip basat en l'ús de nanoantenes dielèctriques com a font de llum i píxels detectors ODT, i caracteritzem experimentalment el seu comportament en camp pròxim mitjançant microscòpia òptica de camp pròxim. Pel que fa a la segona aplicació, estudiem el potencial de la ODT com a nou paradigma en la detecció de capes d'invisibilitat realistes, una de les aplicacions més importants dels metamaterials. Fins ara, el scattering cross section (SCS) s'ha utilitzat com a model de referència per a dissenyar i observar l'eficàcia d'aquests dispositius per a ocultar objectes. En el nostre estudi, vam demostrar que la ODT pot detectar les capes d'invisibilitat pràctiques amb una sensibilitat superior a la que ofereix el SCS, fins i tot a les freqüències de treball òptimes. A més, és possible obtindre una imatge representativa de la grandària i la forma de la capa, revelant clarament la seua existència. Finalment, es discuteixen les conclusions extretes dels resultats obtinguts i es detallen les futures línies de treball per a abordar els reptes que no s'han completat en aquesta tesi doctoral. / [EN] Diffraction Tomography arises to improve previous imaging techniques by considering the wave nature of light. Whereas the first medical imaging systems relied only on non-diffracting sources, this approach results in an enhanced reconstruction of the object's refractive index distribution, allowing, for example, the study of subcellular structures. Likewise, the demand for increasingly faster and secure telecommunication networks led to the advent of photonics. Two decades ago, the combination of these two fields gave rise to the first optical diffraction tomography (ODT) systems, which have rapidly evolved during this century. In this thesis, we present two novel applications of ODT. The first one is related to the concept of tomographic phase microscopy (TPM), a version of ODT that enables the study of isolated cells, with many applications in biomedicine, such as the diagnosis and prognosis of cancer. Nevertheless, current TPM systems are expensive, heavy, and cumbersome. To solve these issues we propose the concept of on-chip TPM. For this purpose, we design a roadmap towards the first integrated tomographic device in the frame of lab-on-a-chip (LoC) technology and develop the first steps to this end: 1) Until now, only flat detectors have been used to obtain the refractive index maps of the objects studied in TPM, based on the detection of the forward scattering. However, fundamental physical principles indicate that measuring also the backscattered field should improve the resolution of the images. Moreover, a flat detector is not the optimal configuration for on-chip TPM. In this vein, we have explored the possibility of using circular detectors in this scenario as a more suitable technique for on-chip configurations, demonstrating at the same time that this approach provides a better resolution than the linear one. 2) We propose a TPM on-chip scheme based on the use of dielectric nanoantennas as the ODT light source and detector pixels, and experimentally characterize their near-field behavior via scanning near-field optical microscopy. As for the second application, we study the potential of ODT as a new paradigm in the detection of realistic invisibility cloaks, one of the most important applications of metamaterials. Up to now, the scattering cross section (SCS) has been used as the gold standard to design and observe the effectiveness of these devices in hiding objects. In our study, we show that ODT can detect practical invisibility cloaks with a higher sensitivity than that offered by the SCS, even at the optimal working frequencies. Moreover, it is possible to obtain an image depicting the size and shape of the cloak, clearly revealing their existence. Finally, the conclusions drawn from the obtained results are discussed. In addition, future lines of action to address the challenges that have not been completed in this doctoral thesis are detailed. / Díaz Fernández, FJ. (2021). Novel Applications of Optical Diffraction Tomography: On-chip Microscopy and Detection of Invisibility Cloaks [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/180125

An effective procedure and parameter window was developed for underwater friction stir welding (UWFSW) 304L stainless steel with a PCBN tool. UWFSW produced statistically significant: increases in yield strengths, decreases in percent elongation. The ultimate tensile strength was found to be significantly higher at certain parameters. Although sigma was identified in the UWFSWs, a significant reduction of sigma was found in UWFSWs compared to ambient FSWs. The degree of sensitization in UWFSWs was evaluated using double loop EPR testing and oxalic acid electro-etched metallography. Results were compared to base metal, ambient FSW, and arc welds. Upper and lower sensitization localization bands were identified in the UWFSWs. Although higher sensitization levels were present in UWFSWs compared to the arc weld, ambient FSW, and heat treated base metals, the UWFSWs were found less susceptible to corrosion than arc welds due to the subsurface location of the sensitization bands. A SCC analysis of UWFSWs relative to base metal and arc weldments was performed. U-bends were exposed to two 3.5% NaCl cyclic immersion experiments at 21 °C and 63 °C for 1000 hours each. A tertiary test was conducted in a 25% NaCl boiling solution. The UWFSW u-bends were no more susceptible to SCC than base metal in the cyclic immersion tests. In the boiling NaCl test, the SCC of the UWFSWs showed significant improvement over the SCC of arc welds. Arc u-bends cracked entirely within the weld bead and HAZ, while SCC in the UWFSWs showed no cracking localization.

Jádrem této disertační práce bylo studovat optické a elektrické charakteristiky tenkovrstvých elektroluminiscenčních součástek řízených střídavým proudem (ACTFEL) a zejména vliv procesu stárnutí luminiforů na jejich optické a elektrické vlastnosti. Cílem této studie měl být příspěvek ke zvýšení celkové účinnosti luminoforů, vyjádřené pomocí jasu, účinnosti a stability. Vzhledem k tomu, že současnou dominantní technologií plochých obrazovek je LCD, musí se další alternativní technologie plošných displejů porovnávat s LCD. Výhodou ACTFEL displejů proti LCD je lepší rozlišení, větší teplotní rozsah činnosti, větší čtecí úhel, či možnost čtení při mnohem vyšší intenzitě pozadí. Na druhou stranu je jejich nevýhodou vyšší energetická náročnost, problém s odpovídající barevností tří základních barev a podstatně vyšší napětí nutné pro činnost displeje. K dosažení tohoto cíle jsme provedli optická, elektrická a optoelektrická měření ACTFEL struktur a ZnS:Mn luminoforů. Navíc jsme studovali vliv dotování vrstvy pomocí KCl na chování mikrostruktury a na elektroluminiscenční vlastnosti (zejména na jas a světelnou účinnost) ZnS:Mn luminoforů. Provedli jsme i některá, ne zcela obvyklá, měření ACTFEL součástek. Vypočítali jsme i rozptylový poměr nabitých barevných center a simulovali transportní charakteristiky v ACTFEL součástkách. Studovali jsme vliv stárnutí dvou typů ZnS:Mn luminoforů (s vrstvou napařenou či získanou pomocí epitaxe atomových vrstev) monitorováním závislostí svítivost-napětí (L-V), velikost vnitřního náboje - elektrické pole luminoforu (Q-Fp) a kapacitance-napětí (C-V) ve zvolených časových intervalech v průběhu stárnutí. Provedli jsme krátkodobá i dlouhodobá měření a pokusili jsme se i o vizualizaci struktury luminoforu se subvlnovým rozlišením pomocí optického rastrovacího mikroskopu pracujícího v blízkém poli (SNOM). Na praktickém případu zeleného Zn2GeO4:Mn (2% Mn) ACTFEL displeje, pracujícího při 50 Hz, jsme také studovali stabilitu svítivosti pomocí měření závislosti svítivosti na napětí (L-V) a světelné účinnosti na napětí (eta-V). Přitom byl zhodnocen význam těchto charakteristik. Nezanedbatelnou a neoddělitelnou součástí této práce je i její pedagogický aspekt. Předložený text by mohl být využit i jako učebnice pro studenty na mé univerzitě v Lybii.