X-ray computed tomography is a technique that has been successfully utilized to characterize internal microstructure of asphalt mixtures. The city of Linköping (Sweden) developed an action plan to reduce noise; accordingly KTH and VTI developed a method to determine air void content in porous asphalt using x-ray computed tomography and an image processing software called ImageJ. The present study is a continuation of the previously mentioned work and focuses on the investigation of aggregate structure in porous asphalt by x-ray computed tomography. First the previously proposed method to estimate air void content was validated. Then, the assessment of aggregate structure including qualitative and quantitative analysis was completed. Qualitative evaluation was performed to determine the quality of slices in regard to establishing challenging areas, and the extent of beam hardening present in the X-ray images. This evaluation produced quality slices for each sample in Y-direction to work as a reference to establish general threshold ranges and image enhancement procedures, as well as identifying the interface between the top and bottom layer of the porous asphalt. The quantitative analysis consisted of analysing aggregate structures in the porous asphalt and developing a method to estimate the aggregate size distribution in porous asphalt layers. The gradation curves from the quantification of aggregate size distribution in all directions (X, Y, Z) were compared to the gradation curves from laboratory sieving tests previously performed on the drilled asphalt cores. To determine the accuracy of the method a perimeter analysis was performed to evaluate the suggested method to measure the aggregates. The results obtained indicate that to quantify the aggregates in porous asphalt, enhancement of the images is needed, as well as morphological operations to deal with beam hardening and overlapping stones due to unsuccessful separation of aggregates when thresholding. This further indicates that ImageJ Fiji is more suitable for complex cases, such as cases where aggregates and mastic are hard to distinguish from each other, rather than the original ImageJ software. This is due to the extended plugins available in ImageJ Fiji, where more options of for example filtering and enhancing of images are available. The results also suggest that the proposed method is a suitable method to determine the aggregate size distribution in porous asphalt pavements, as it allows to quantify the aggregate distribution and produces realistic results with slight inaccuracies due to the analysis being performed in 2D. Future development will be focused on automizing the determination of air void structure and aggregate size distribution, but also on the development of procedures to determine other relevant parameters such as mastic and binder content to establish a complete methodology to investigate the internal structure of a porous asphalt pavement, as well as 3D analysis to determine these parameters.

Heard Island is a remote Australian territory which lies in the South-middle sector of the Indian Ocean.The island lies in the central province of the Kerguelen Plateau. On the north-western face of the islandlies the Laurens Peninsula, where modern volcanism has been periodic since approximately 10 ka, butno eruption has been recorded. The main volcanic feature of the peninsula is Mt Dixon of which noactivity has been observed but it is thought to have erupted within the past few hundred years. This thesis applied the crystal size distribution method to three thin sections from the LaurensPeninsula. The samples were collected from a phonolite from Jacka valley, a teprhiphonolite from thebase of the Red Island cone, and a tephrite east of Cape Cartwright. Crystal dimensions were calculatedusing ImageJ Fiji, these dimensions were corrected for 3D dimensions using CSDslice, and the datawas plotted using CSDcorrections. Microcrysts were traced using backscattered electron (BSE) images,and high resolutions scans of the thin section were used to trace phenocrysts. The results of the crystalsize distributions show concave-up shapes in all plots with steep slopes for smaller crystals, followedby shallow slopes for larger crystals. This suggests binary magma mixing by replenishment occurred inthe magmas associated with all three samples. The different slopes suggest two separate crystallisationconditions: Phenocrysts crystalized slowly in the chamber and microcrysts crystallized relativelyquickly during or after eruption. Textural differences in the three samples suggest that the tephrite hadthe longest residence time and underwent the most replenishment events, followed by thetephriphonolite and lastly the phonolite. Finally, since replenishment is the mechanism of mixingbeneath the Laurens Peninsula, then volcanism might still be active, and the chambers could currentlybe replenishing, which could trigger an eruption. / Heard Island är ett avlägset australiensiskt territorium som ligger i den södra delen av den Indiskaoceanen. Ön ligger i den centrala provinsen på Kerguelenplatån. På den nordvästra sidan av ön liggerLaurens-halvön, där modern vulkanism daterar sig till cirka 10 ka. Den främsta vulkaniska strukturenpå halvön är Mt Dixon där ingen aktivitet har registrerats, men som tros ha haft ett utbrott under desenaste hundra åren. Denna avhandling tillämpade metoden för kristallstorleksfördelning på tre tunnslipar frånLaurenshalvön. Proverna samlades in från en fonolit från Jacka valley, en tefrifonolit från basen av RedIsland cone och en tefrit öster om Cape Cartwright. Kristalldimensioner beräknades med ImageJ Fiji,dessa dimensioner korrigerades för 3D-dimensioner med CSDslice, och datat plottades medCSDcorrections. Mikrokristaller spårades med hjälp av backscattered electron images (BSE) ochhögupplösta skanningar av tunnslipen användes för att spåra fenokryster. Resultaten avkristallstorleksfördelningarna föreslog binär magmablandning via påfyllning i alla tre proverna. Dessavisade konkava former i alla plotter med branta sluttningar för mindre kristaller, följt av plattaresluttningar för större kristaller. De olika lutningarna på kurvorna föreslog två separatakristallisationsförhållanden: fenokryster kristalliserade långsamt i kammaren, och mikrokristallerkristalliserade relativt snabbt under eller efter utbrottet. Texturella skillnader i de tre proverna antyddeatt tefriten hade den längsta residenstiden och genomgick flest påfyllningshändelser, följt avtefrifonoliten och slutligen fonoliten. Slutligen, om påfyllning var mekanismen för att blandas underLaurenshalvön, så kan vulkanismen fortfarande vara aktiv, men för närvarande i ettpåfyllningsuppehåll.

No description available.

No description available.

Fatigue and ductility properties in various tool steels, produced by powder metallurgy, spray forming or conventionally ingot casting, have been analysed experimentally and successfully compared to developed models. The models are able to predict the fatigue limit and cause for fatigue fracture, and strain- and stress-development until fracture during the ductile fracture process respectively. Total fracture in a tool steel component, both in fatigue and ductility testing, is caused by a propagating crack initiated by particles, i.e. carbides or non-metallic inclusions. The models are based on experimentally observed size distributions. The axial fatigue strength at two million cycles was determined for various tool steels. The fracture surface of each test bar broken was examined in SEM to determine the cause for fatigue failure, i.e. a single carbide or inclusion particle or a cluster of carbides, and the size of the particle. The particles act as stress concentrators where a crack is easily initiated when the material is subjected to alternating stresses. The developed models calculate the probability that at least one particle will be present in the material which is larger than the threshold level for crack initiation at a certain stress range. The ductility testing was performed on various tool steels by four-point bending under static load. The load and displacement until total fracture were recorded and the maximum strain and stress acting in the material were calculated. The fracture surface of each broken test bar was examined in SEM, though the crack initiating area appears different compared to a fatigue failure. Ductile fracture is caused by a crack emanating from voids nucleated around many particles in a joint process and then linked together. By finite element modelling of void initiation and propagation in 2D of an experimentally observed carbide microstructure for each tool steel, successful comparisons with experiments were performed. Carbides were modelled as cracked when larger than a certain size, based on fracture surface observations, and the matrix cracked above a pre-defined plastic deformation level. The stresses and strains at total failure were in good agreement between model and experiments when evaluated. The use of these developed models could be a powerful tool for optimisation of fatigue and ductility properties for tool steels. With good fatigue and ductility properties normal failures appearing during operation of a tool steel product could be minimised. By theoretical tests in the developed models of various carbide microstructures the optimum mechanical properties could be achieved with a minimum of experiments performed. / QC 20101119

Yes / The tribological performance of the piston assembly of an automotive engine is highly influenced by the complex flow mechanisms that supply lubricant to the upper piston rings. As well as affecting friction and wear, the oil consumption and emissions of the engine are strongly influenced by these mechanisms. There is a significant body of work that seeks to model these flows effectively. However, these models are not able to fully describe the flow of lubricant through the piston assembly. Some experimental studies indicate that droplets of lubricant carried in the gas flows through the piston assembly may account for some of this. This work describes an investigation into the nature of lubricant misting in a fired gasoline engine. Previous work in a laboratory simulator showed that the tendency of a lubricant to form mist is dependent on the viscosity of the lubricant and the type and concentration of viscosity modifier. The higher surface area-to-volume ratio of the lubricant if more droplets are formed or if the droplets are smaller is hypothesised to increase the degradation rate of the lubricant. The key work in the investigation was to measure the size distribution of the droplets in the crankcase of a fired gasoline engine. Droplets were extracted from the crankcase and passed through a laser diffraction particle sizer. Three characteristic droplet size ranges were observed: Spray sized (250–1000 μm); Major mist (30–250 μm); and Minor mist (0.1–30 μm). Higher base oil viscosity tended to reduce the proportion of mist-sized droplets. The viscoelasticity contributed by a polymeric viscosity modifier reduced the proportion of mist droplets, especially at high load.

The collisions frequency of dispersed phases (particles, droplets, bubbles) in a turbulent carrier phase is a fundamental quantity that is needed for modeling multiphase flows with applications to chemical processes, minerals flotation, food science, and many other industries. In this dissertation, numerical simulations are performed to determine collisions frequency of bi-dispersed particles (solid particles and bubbles) in homogeneous isotropic turbulence. Both direct numerical simulations (DNS) and Large Eddy simulations (LES) are conducted to determine velocity fluctuations of the carrier phase. The DNS results are used to validate existing theoretical models as well as the LES results. The dissertation also presents a CFD-based flotation model for predicting the pulp recovery rate in froth flotation machines. In the direct numerical simulations work, particles and bubbles suspended in homogeneous isotropic turbulence are tracked and their collisions frequency is determined as a function of particle Stokes number. The effects of the dispersed phases on the carrier phase are neglected. Particles and bubbles of sizes on the order of Kolmogorov length scale are treated as point masses. Equations of motion of dispersed phases are integrated simultaneously with the equations of the carrier phase using the same time stepping scheme. In addition to Stokes drag, the pressure gradient in the carrier phase and added-mass forces are also included. The collision model used here allows overlap of particles and bubbles. Collisions kernel, radial relative velocity, and radial distribution function found by DNS are compared to theoretical models over a range of particle Stokes number. In general, good agreement between DNS and recent theoretical models is obtained for radial relative velocity for both particle-particle and particle-bubble collisions. The DNS results show that around Stokes number of unity particles of the same group undergo expected preferential concentration while particles and bubbles are segregated. The segregation behavior of particles and bubbles leads to a radial distribution function that is less than one. Existing theoretical models do not account for effects of this segregation behavior of particles and bubbles on the radial distribution function. In the large-eddy simulations efforts, the dissertation addresses the importance of the subgrid fluctuations on the collisions frequency and investigates techniques for predicting those fluctuations. The cases studied are of particles-particles and particles-bubbles collisions at Reynolds number Re_λ = 96. A study is conducted first by neglecting the effects of subgrid velocity fluctuations on particles and bubbles motions. It is found that around Stokes number of unity solid particles of the same group undergo the well known preferential concentration as observed in the DNS. Effects of pressure gradient on the particles are negligible due to their small sizes. Bubbles as a low inertia particles are very sensitive to subgrid velocity and acceleration fields where the effects of pressure gradient in the carrier phase are dominant. However, particle-bubble radial distribution functions from LES are not as low as that from DNS. To account for the effects of subgrid field on the dispersion of particles and bubbles, a new multifractal methodology has been developed to construct a subgrid vorticity field from the resolved vorticity field in frame work of LES. A Poisson's solver is used to obtain the subgrid velocity field from the subgrid vorticity field. Accounting for the subgrid velocity fluctuations (but neglecting pressure gradient) produced minor changes in the radial distribution function for particle-particle and particle-bubble collisions. We conclude from this study that for accurate particle tracking in LES the subgrid velocity fluctuations must be dynamically realizable field (temporally and spatially correlated with the large scale motion). Adding random SGS velocity fluctuations is not enough to capture the correct radial distribution functions of dispersed phases especially for bubbles-particles collisions where the pressure gradient term ( or acceleration Du_f′/Dt) is responsible for particle-bubble segregation around particle Stokes number near one. A CFD-based model for minerals flotation machines has been developed in this dissertation. The objective of flotation models is to predict the recovery rate of minerals from a flotation cell. The developed model advances the state-of-the-art of pulp recovery rate prediction by incorporating validated theoretical collisions frequency models and detailed hydrodynamics from two-phase flow simulations. Spatial distributions of dissipation rate and air volume fraction are determined by the two-phase hydrodynamic simulations. Knowing these parameters throughout the machine is essential in understanding the effectiveness of different components of flotation machine (rotor, stator or disperser, jets) on the flotation efficiency. The developed model not only predicts the average pulp recovery rate but also it indicates regions of high/low recovery rates. The CFD-based flotation model presented here can be used to determine the dependence of recovery rate constant at any locality within the pulp based on particle diameter, particle specfic gravity, contact angle, and surface tension. / Ph. D.

[ES] La comprensión de los fenómenos físicos que acontecen en la región densa (también conocida como campo cercano) durante la atomización de los sprays ha sido una de las mayores incógnitas a la hora de estudiar sus aplicaciones. En el sector industrial, el rango de interés abarca desde toberas en aplicaciones propulsivas a sprays en aplicaciones médicas, agrícolas o culinarias. Esta evidente falta de conocimiento obliga a realizar simplificaciones en la modelización, provocando resultados poco precisos y la necesidad de grandes caracterizaciones experimentales en la fase de diseño. De esta manera, los procesos de rotura del spray y atomización primaria se consideran problemas físicos fundamentales, cuya complejidad viene dada como resultado de un flujo multifásico en un régimen altamente turbulento, originando escenarios caóticos. El análisis de este problema es extremadamente complejo debido a la ausencia sustancial de teorías validadas referentes a los fenómenos físicos involucrados como son la turbulencia y la atomización. Además, la combinación de la naturaleza multifásica del flujo y su comportamiento turbulento resultan en una gran dificultad para afrontar el problema. Durante los últimos 10 años, las técnicas experimentales han sido finalmente capaces de visualizar la región densa, pero la confianza, análisis y efectividad de dichos experimentos en esta región del spray todavía requiere de mejoras sustanciales. En este contexto, esta tesis trata de contribuir al entendimiento de estos procesos físicos y de proporcionar herramientas de análisis para estos flujos tan complejos. Para ello, mediante Direct Numerical Simulations se ha afrontado el problema resolviendo las escalas de movimiento más pequeñas, y capturando todas las escalas de turbulencia y eventos de rotura. Uno de los objetivos de la tesis ha sido evaluar la influencia de las condiciones de contorno del flujo entrante en la atomización primaria y en el comportamiento turbulento del spray. Para ello, se han empleado dos condiciones de contorno diferentes. En primer lugar se ha empleado una condición de contorno sintética para producir turbulencia homogenea a la entrada, simulando el comporamiento de la tobera. Una de las características más interesantes de este método es la posibilidad de retocar los parámetros dentro del algoritmo. En particular, la escala de longitud integral se ha variado para evaluar la influencia de las estructuras mas grandes de la tobera en la atomización primaria. El análisis de la condición de contorno sintética también ha permitido el diseño óptimo de simulaciones de las cuales se han derivado estadísticas turbulentas significativas. En este escenario, se han llevado a cabo estudios más profundos sobre la influencia de propiedades de las estructuras turbulentas como la homogeneidad y la anisotropía tanto en el espectro de los flujos como en las estadísticas de las gotas. Para tal fin, se han desarrollado metodologías novedosas para computar el análisis espectral y la estadística de las gotas Entre los resultados de este análisis destaca la independencia de la condición de contorno de entrada en las estadísticas de las gotas, mientras que por otra parte, recalca que las características turbulentas desarrolladas en el interior de la tobera afectan a la cantidad total de masa atomizada. Estas consideraciones se encuentran respaldadas por el análisis espectral realizado, mediante el cuál se concluye que la turbulencia multifásica comparte el comportamiento universal descrito por las teorías de Kolmogorov. / [CA] La comprensió dels fenòmens físics que succeïxen en la regió densa (també coneguda com a camp pròxim) durant l'atomització dels sprays ha sigut una de les majors incògnites a l'hora d'estudiar les seues aplicacions. En el sector industrial, el rang d'interés comprén des de toveres en aplicacions propulsives a sprays en aplicacions mèdiques, agrícoles o culinàries. Esta evident falta de coneixement obliga a realitzar simplificacions en la modelització, provocant resultats poc precisos i la necessitat de grans caracteritzacions experimentals en la fase de disseny. D'esta manera, els processos de ruptura del spray i atomització primària es consideren problemes físics fonamentals, la complexitat dels quals ve donada com resultat d'un flux multifàsic en un règim altament turbulent, originant escenaris caòtics. L'anàlisi d'este problema és extremadament complex a causa de l'absència substancial de teories validades dels fenòmens físics involucrats com són la turbulència i l'atomització. A més, la combinació de la naturalesa multifàsica del flux i el seu comportament turbulent resulten en una gran dificultat per a afrontar el problema. Durant els últims 10 anys les tècniques experimentals han sigut finalment capaces de visualitzar la regió densa, però la confiança, anàlisi i efectivitat dels experiments en esta regió del spray encara requerix de millores substancials. En este context, esta tesi tracta de contribuir en l'enteniment d'estos processos físics i de proporcionar ferramentes d'anàlisi per a estos fluxos tan complexos. Per a això, per mitjà de Direct Numerical Simulations s'ha afrontat el problema resolent les escales de moviment més menudes, al mateix temps que es capturen totes les escales de turbulència i esdeveniments de ruptura. Un dels objectius de la tesi ha sigut avaluar la influència que les condicions de contorn del flux entrant tenen en l'atomització primària i en el comportament turbulent del spray. Per a això, s'han empleat dos condicions de contorn diferents. En primer lloc s'ha empleat una condició de contorn sintètica per a produir turbulència homogènia a l'entrada, simulant el comportament de la tovera. Una de les característiques més interessants d'este mètod és la possibilitat de retocar els paràmetres dins de l'algoritme. En particular, l'escala de longitud integral s'ha variat per a avaluar la influència de les estructures mes grans de la tovera en l'atomització primària. L'anàlisi de la condició de contorn sintètica també ha permés el disseny òptim de simulacions de les quals s'han derivat estadístiques turbulentes significatives. En este escenari, s'han dut a terme estudis més profunds sobre la influència de propietats de les estructures turbulentes com l'homogeneïtat i l'anisotropia tant en l'espectre dels fluxos com en les estadístiques de les gotes. Per a tal fi, s'han desenrotllat metodologies noves per a computar l'anàlisi espectral i l'estadística de les gotes. Entre els resultats d'esta anàlisi destaca la independència de la condició de contorn d'entrada en les estadístiques de les gotes, mentres que d'altra banda, es recalca que les característiques turbulentes desenrotllades en l'interior de la tovera afecten a la quantitat total de massa atomitzada. Estes consideracions es troben recolzades per l'anàlisi espectral realitzat, per mitjà del qual es conclou que la turbulència multifásica compartix el comportament universal descrit per les teories de Kolmogorov. / [EN] The understanding of the physical phenomena occurring in the dense region (also known as near field) of atomizing sprays has been long seen as one of the biggest unknown when studying sprays applications. The industrial range of interest goes from nozzles in combustion and propulsion applications to medical sprays, agricultural and food process applications. This substantial lack of knowledge is responsible for some important simplification in modeling, that often result to be inaccurate or simply partial, leading to the evident need of large experimental characterization during the design phase. In fact, the spray breakup and primary atomization processes are indeed fundamental problems of physics, which complexity results from the combination of a multiphase flow in a highly turbulent regime that leads to chaotic scenarios. The analysis of this problem is extremely problematic, due to a substantial lack of definitive theories about the physical phenomena involved, namely turbulence and atomization. Furthermore, the combination of the multiphase nature of the flow and its turbulent behavior makes substantially difficult to address the problem. Only within the last 10 years, experimental techniques have been capable of visualizing the dense region, but the experiments reliability, analysis and effectiveness in this region still requires vast improvements. In this scenario, this thesis aims to contribute in the understanding of these physical process and to provide analysis tools for these complex flows. In order to do so, Direct Numerical Simulations have been used for addressing the problem at its smallest scale of motion, while reliably capturing all turbulence scales and breakup events. The multiphase nature of the flow is accounted for by using the Volume of Fluid method. One of the goal of the thesis was to assess the influence of the inflow boundary conditions on the primary atomization and on the spray's turbulence behavior. In order to do so, two different boundary conditions were used. In a first place, a synthetic inflow boundary condition was used in order to produce a homogeneous turbulence inflow, simulating the nozzle behavior. One of the interesting features of this method was the possibility of tweaking the parameters within the algorithm. In particular, the integral length scale was varied in order to assess the influence of nozzle larger turbulent structures on the primary atomization. The analysis on the synthetic boundary condition also allowed to optimally design simulations from which derive meaningful turbulence statistics. On this framework, further studies were carried over on the influence of turbulent structures properties, namely homogeneity and anisotropy, on both the flows spectra and droplets statistics. In order to achieve this goal, novel procedures for both computing the flow spectra and analyzing droplets were developed and are carefully addressed in the thesis. The results of the analysis highlight the independence of droplets statistics from the inflow boundary condition, while, on the other hand, remarking how the total quantity of atomized mass is significantly affected by the turbulence features developed within the nozzle. This considerations are supported by the spectrum analysis performed, which also highlighted how multiphase turbulence shares the universal features described in Kolmogorov theories. / Crialesi Esposito, M. (2019). Analysis of primary atomization in sprays using Direct Numerical Simulation [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/133975

The efficiency of multicrystalline (mc) silicon solar cells depends strongly on the fraction of recombination active crystal defects. This work focuses on a systematic analysis of how the area fraction of recombination active crystal defects and thus the solar cell efficiency is af-fected by the grain structure of mc-silicon wafers, i.e. grain size, grain orientation and type of the grain boundaries between adjacent grains. For that purpose a new characterization method was developed which allows the measurement of the grain orientation and grain boundary type of full 156x156 mm² mc-silicon wafers. The results of the grain structure analysis were correlated with the etch pit density, the recombination active area fraction measured by photo-luminescence imaging, and the solar cell efficiency in order to quantify the most important features of the grain structure, which were relevant to obtain high quality mc-silicon wafer material. For the determination of the grain orientation and grain boundary type two metrology sys-tems were combined. The so-called grain detector determines the geometrical data of each grain (size and form) by a reflectivity measurement. Afterwards the wafer with the geomet-rical information of all grains is transferred into the so-called Laue Scanner. This system irra-diates each grain larger 3 mm² with white x-rays and creates a backscatter diffraction pattern (Laue pattern) for each grain. From this Laue pattern the grain orientation and the grain boundary type of neighboured grains is calculated and statistically analysed in combination with the geometrical data of the grain detector. In this work the grain structure of twelve industrially grown mc-silicon bricks, which were produced by different manufacturers, and two laboratory grown bricks were investigated. Seven of these bricks show a fine grain structure. This material named class F is considered to be typical for so-called High Performance Multi (HPM) silicon. The other bricks show a coarse-grained structure. This grain structure was called class G and corresponds to the con-ventional mc-silicon material. The results show that the grain structures of the start of the crystallization process differ sig-nificantly between class F and class G. The class F mc-silicon wafers have a uniform initial grain size (characterized by coefficient of variation CV¬KG < 2.5) and grain orientation (charac-terized by coefficient of variation CVKO < 1.5) distribution with a small mean grain size (< 4 mm²) and a high length fraction of random grain boundaries (> 60 %) in comparison to the class G wafers. Despite the totally different initial grain structure for the class F and class G bricks, the grain structure of the wafers which represent the end of the crystallization process is more or less comparable. It can be concluded that the development of the grain structure along the crystal height of the class F bricks is driven by an energy minimization due to the surface energy and the grain boundary energy, that means that the share of (111) oriented grains having the lowest surface energy and the share of ∑3 grain boundaries having the lowest interface energy increase from the start of crystallization to the end. This phenomenon could not be observed for the class G bricks, which show a decreasing ∑3 length fraction and a decreasing area fraction of {111} oriented grains. This energetically unfavourable grain structure development is not clear so far but it means another kind of energy minimization effect must exist within class G. This could be for instance the formation of dislocations. The grain structure investigations show clearly that especially the initially fine-grained struc-ture of the class F bricks, i.e. at the start of crystallization, influences beneficially the area fraction of recombination active defects and the solar cell efficiency subsequently. This ob-servation can be explained as follows. Reduced dislocation cluster formation: • The small grain sizes in combination with the low length fraction of ∑3 grain bounda-ries capture the dislocations within a grain. Dislocations are not able to move across the grain boundaries which have not the ∑3-type within moderate stress and tempera-ture fields. This prohibits the formation and expansion of large dislocation cluster. • The previously described energetically driven grain selection and the continuously in-creasing grain size from bottom to top leads to an overgrowth of grains. This means that also dislocated grains will disappear which also prohibits the formation of large dislocation cluster. Reduced possibility of dislocation formation: • Compared to the class G bricks the area fraction of {111} oriented grains is reduced. Therefore, the possibility of the formation of dislocations is reduced, because they would be activated first in {111} oriented grains taking the Schmidt factor in account which is lowest for {111} oriented grains. After the dislocation generation within a {111} oriented grain, the dislocation can move forward on 3 of 4 possible {111} slip planes which have an angle of 19.5° with regard to the growth direction. No other ori-entation has more slip planes for the dislocation movement which have an angle smaller 20° with regard to the growth direction. These arguments in combination with the high reproducibility of the characteristic initial class F structure can explain the observed low recombination active area fraction from start to end of crystallization which was smaller 5 % and especially the low variation of 2 % of the electrical active wafer area in between the class F bricks. One can also easily explain the higher recombination active area fraction up to 14 % and the large variation of 10 % between the class G bricks due to the obtained grain structure data. These differences in the recombination active area fractions are reflected in the solar cell efficiency which is 0.4 % higher for the class F bricks compared to the class G bricks. In consideration of the above mentioned reasons it is not beneficial for the industrial ingot production technology to increase the ingot height further, due to the fact that the advanta-geous initial grain structure properties of class F bricks disappear with increasing crystal height.

Cette étude porte sur le broyage en voie humide (nanobroyage) de produits organiques à usage pharmaceutique dans un broyeur à billes agité. L'objectif des travaux réalisés était d'analyser la faisabilité de l'opération de nanobroyage et d'améliorer la compréhension des processus de réduction de taille dans le cas de produits organiques cristallins. Dans un premier temps, des expériences préliminaires ont été menées pour le choix d'agents mouillants et dispersants adéquats pour les matériaux choisis (ciclopirox, ibuprofène) et pour la mise au point du mode de fonctionnement du procédé de broyage. Nous avons également testé différentes techniques comme la spectroscopie acoustique et la diffusion dynamique de la lumière pour caractériser la distribution de taille des particules broyées, en se basant sur une étude expérimentale conduite sur la calcite, utilisée dans cette étude comme matériau de référence. La seconde partie a été consacrée au broyage par microbilles appliqué aux différents matériaux choisis. Nous avons étudié l'influence des paramètres opératoires tels que le débit de suspension, la vitesse de rotation de l'agitateur, la taille des billes de broyage et la concentration en solide sur l'efficacité énergétique du procédé et la qualité des produits broyés. Les critères de qualité pris en compte dans cette étude sont la distribution de taille des particules, la stabilité et le comportement rhéologique des suspensions broyées ainsi que les propriétés structurales du produit. L'effet du broyage sur les changements microstructuraux des différents produits a enfin été analysé. Une attention particulière a également été portée sur l'effet de la température sur le procédé de réduction de taille et les propriétés de l'ibuprofène broyé. / This work focuses on wet grinding (nanogrinding) of organic materials for pharmaceuticals using a stirred media mill. The aim of the work was to examine the feasibility of nanogrinding process and to improve the understanding of size reduction processes applied on crystalline organic products. Firstly, preliminary investigations were conducted to make a choice of appropriate wetting agents and dispersants for the selected materials (ciclopirox, ibuprofen), and for the development of the operation mode of the grinding process. We also tested different techniques such as acoustic attenuation spectroscopy and dynamic light scattering to characterize the ground particle size distribution, based on an experimental study conducted on calcite, used in this study as reference material. The second part was devoted to the milling process by grinding beads applied to the selected materials. The influence of operating parameters such as suspension flow rate, stirrer tip speed, grinding media diameter and solid mass concentration on grinding process efficiency and ground products quality were investigated. The quality criteria considered in this study are particle size distribution, stability and rheological behaviour of the products, as well as their structural properties. The effect of grinding process on the microstructural change of different materials was finally analysed. Particular attention was also focused on the effect of temperature on size reduction process and ground ibuprofen properties.