The objective of this thesis is to develop improved reliability-based structural design methods for stiffened aluminium. panels in high-speed vessels. In recent years aluminium high-speed vessels have grown larger and are venturing into increasingly hostile operating environments. Designing such vessels requires structural prediction techniques capable of producing a light structure with high confidence in its strength and safety. However, current aluminium marine structural design methods are largely simple modifications of steel methods that do not account for all of the differences between aluminium and steel. TTds thesis presents new reliability-based design techniques for the ultimate strength and fatigue strength of aluminium stiffened panels. A review of recent aluminium high-speed vessels is made, along with their structural configuration and hydrodynamic loading. Structural reliability techniques are discussed. Existing prediction methods, including marine approaches and civil engineering design codes are compared to experimental results for the compressive collapse of aluminium plates and stiffened panels. A modified technique is proposed to model the compressive collapse of such panels. The tensile response of welded aluminium, structures is investigated, including the influence of strain concentration in the reduced-strength region around welds. Reliability formulations are presented and discussed for ultimate strength predictions. A reliability based hot-spot S-N fatigue prediction method is developed for welded connections, including an analysis of the material and prediction uncertainty values and a comparison with existing design codes. Discussion of extending the fatigue prediction techniques to include through-life initiationpropagation fatigue models are presented, along with a simple trial application to butt welds. Conclusions from the techniques investigated are presented, and potential future developments are discussed.

Adhesive bonding of aluminium alloys is a widely used joining technology across many industrial sectors including aerospace, automotive, marine, defence and construction. One of the key attractions of adhesive bonding is the superior fatigue performance and joint stress distribution. The applications are not without limitations and adhesive joints often suffer from premature failure when put into service in harsh environments such as those containing high degrees of moisture.

La métallurgie des poudres permet d’élaborer des pièces à des températures inférieures à la température de fusion et d’obtenir des composites ayant des propriétés remarquables. Ainsi, la faible densité de l’aluminium associée à l’excellente résistance mécanique des nanotubes de carbone (NTC) font des composites Al/NTC des matériaux prometteurs pour divers domaines tels que l’aéronautique ou l’automobile. Cependant, l’obtention de propriétés mécaniques améliorées passe par le contrôle de la microstructure et en particulier des joints de grains. Ainsi, l’absence de porosité et la répartition uniforme des nanotubes de carbone entre les grains sont des conditions nécessaires au renforcement. Un protocole permettant la désagglomération des nanotubes puis leur dispersion an sein d’une poudre d’aluminium a été établi. Sa remarquable efficacité a été caractérisée par microscopie et son impact sur les propriétés mécaniques des matériaux élaborés vérifié. Le frittage des poudres a été effectué par deux méthodes : pressage à chaud et frittage flash. L’étude approfondie des joints de grains a permis de mettre en évidence l’influence des paramètres de frittage (temps, température, technique) sur la réactivité du système Al-NTC. Ainsi, un mécanisme de formation des cristaux de carbure d’aluminium faisant intervenir la cristallisation puis la rupture de la couche d’oxyde en surface des grains d’aluminium est proposé. Enfin, différents paramètres tels que la teneur en NTC, la technique et les conditions de frittage utilisées et l’emploi du broyage comme prétraitement des poudres composites ont été mis en relation avec l’amélioration de la résistance mécanique de l’aluminium constatée. / Powder metallurgy routes allow the synthesis below the melting temperature of composites with notable properties. Due to the combination of the aluminum (Al) low density and the excellent mechanical properties of carbon nanotubes (CNT), Al/CNT composites might be promising materials for various fields such as aerospace and automotive. However, the improvement of mechanical properties requires the control of the microstructure and especially of grain boundaries. Indeed, high density and uniform distribution of carbon nanotubes in the matrix are necessary conditions for mechanical strengthening. A protocol was developed in order to ensure the nanotubes disentanglement and dispersion within the aluminum powder. Its high efficiency was characterized by microscopy technics and its impact on the composites mechanical properties was highlighted. The powders are sintered by two methods: hot pressing and spark plasma sintering. The study of grain boundaries highlights the influence of sintering parameters (time, temperature, technique) on the Al-CNT system reactivity. Thus, an aluminum carbides formation mechanism involving crystallization and cracking of the oxide layer at the aluminum grains surface is proposed. Finally, various parameters such as the CNT content, sintering conditions and techniques used and the prior ball milling of the composite powders are related to the improvement of the aluminum mechanical strength.

Cette étude porte sur la faisabilité de l’élaboration de matériaux multicouches à grains ultrafins par un procédé original de métallurgie douce : le laminage cumulé contrôlé. Les multicouches à base d’aluminium sont renforcés par des alliages de compositions Al-Ni-Sm pris dans des états amorphe ou cristallisés. Cette combinaison à ce jour inédite est originale compte tenu de la différence marquée de comportement mécanique et de mécanisme de déformation des constituants. Les paramètres du procédé sont d’abord définis à partir de la caractérisation de la stabilité microstructurale des constituants et de leur comportement mécanique. Plusieurs types de traitement thermique et mécanique, ainsi que différents nombres de couches ont été testés afin d’optimiser la microstructure et par tant l’aptitude à la mise en forme. Les transformations de phases (recristallisation dynamique ou non de l’aluminium, changements de phases au sein des alliages Al-Ni-Sm…) ont été analysées par diffractométrie X, microscopies et calorimétrie différentielle. Parmi les principaux résultats, la cristallisation du verre métallique induite par déformation est démontrée. En relation avec la modification de propriétés mécaniques induite par le changement de microstructure des renforts, les multicouches élaborées à partir de renforts à l’état cristallin sont plus malléables que celles obtenues au moyen d’alliages à l’état amorphe. La différence est reliée à la fois à la morphologie des débris et à l’accommodation des déformations au niveau des interfaces matrice/renfort. Au stade actuel du travail, un multimatériau a été synthétisé à partir de 216 couches d’aluminium et de 180 feuilles de renfort à l’état cristallin. Ce matériau à grains ultrafins présente encore une distribution non uniforme de fragments de renforts. / This study of feasibility deals with the development of ultrafine grained (UFG) multilayers by an original process i.e. controlled accumulative roll bonding. Aluminium based multilayers are reinforced by Al-Ni-Sm alloys taken either in the amorphous or crystallized state. This association of materials is particularly interesting according to the significant difference of mechanical behavior and mechanism of deformation of both constituents. The definition of the process parameters arises from the study of both the stability and the mechanical behaviour of the constituents. Numerous thermal and mechanical treatments as well as various numbers of stacked layers have been considered in order to optimize the microstructure and therefore workability of the multilayers. The phase transformations (dynamical or static recrystallization of Al, crystallization of amorphous alloys…) have been investigated by X-ray diffractometry, various kinds of microscopy and differential scanning calorimetry. Among the main results, the crystallization of the metallic glass due to deformation has been proved. Due to the modification of the mechanical properties induced by the change of microstructure of the reinforcements, the multilayers bearing crystalline reinforcements are more deformable than those containing amorphous alloys. The difference is explained by the morphology of the fragments of reinforcements as well as by the accommodation of deformation at their interfaces. Finally, a multimaterial has been prepared from 216 Al layers and 180 layers of crystalline reinforcements. This UFG material presents a heterogeneous distribution of reinforcements.

Aluminium alloy castings are being used increasingly in safety-critical applications in the automotive and aerospace industries. To produce castings of sufficient quality, it is, therefore, important to understand the mechanisms of the formation of defects in aluminium melts, and important to have a reliable and simple means of detection. During the production of aluminium ingots and castings, the surface oxide on the liquid is folded in to produce crack-like defects (bifilms) that are extremely thin, but can be extremely extensive, and so constitute seriously detrimental defects. However, the presence of bifilms has not been widely accepted, because there has been no single metal quality test that has been able to resolve features that are only nanometres, or sometimes micrometres, in thickness. In the past, porosity has usually been held solely responsible for most failures in aluminium alloys, and hydrogen has been blamed as the actual cause. In this work it has been found that bifilms are the initiator and hydrogen is only a contributor in the porosity formation process. For the first time, evidence is presented for the contribution of air (or perhaps more strictly, residual nitrogen from air) as an additional gas, adding to hydrogen in pores in cast Al alloys. The Reduced Pressure Test (RPT) is used which is a simple and widely known test, is cost effective and involves no complicated equipment or consumables, thus recommending it for implementation on the foundry floor. On this basis, several Al-Si based alloys were studied. A quality index -Bifilm Index- is introduced to quantify the results of the reduced pressure test. In addition, mechanical tests were carried out to correlate bifilm index with mechanical properties.

Extruded Al-Mn alloy are used in heat exchanger applications due to their light weight and good thermal conductivity. Depending on the application, the units may be subjected to external corrosion, which can lead to perforation of the tube. The industrial test most commonly used to assess heat exchanger alloys is the seawater acetic acid test (SWAAT). This is a cyclic fog at 40°C and pH 2.9. In the present study, it was found that pits developing in extruded Al-Mn tubes during the SWAAT test are purely crystallographic. Furthermore, a mechanistic understanding for crystallographic pitting has been developed. The SWAAT test can be of relatively long duration and, typically, does not yield information on the underlying corrosion initiation and propagation mechanisms. In the present study, alternate methods to assess pitting corrosion were elaborated. A drop testing procedure has been successfully implemented to study the mechanism of pit initiation. It was revealed that pits initiated within the aluminium matrix in the vicinity of grain boundaries. A close link between large second-phase particles and pit initiation was established. No preferred grain orientation for pit initiation was evident. Scanning electron microscopy and associated tomography were undertaken for the first time to clarify the mechanism of pit propagation. The pit walls were oriented {100}, while the fast-dissolving planes were {110} and {111}. The findings were in accordance with previous literature. Corrosion penetrated deeper into the alloy when the corrosion front was close to a grain boundary. Pit walls were cathodic to the aluminium matrix, possibly due to enrichment of alloying elements at pit walls. The effect of alloy additions on the corrosion behaviour of extruded aluminium alloys was investigated. Alloys with varying copper, iron and manganese contents were compared. Shot noise analysis and post-mortem analyses were undertaken. The increased amount of manganese in solid solution delayed the transition from micropits to stable pitting. This delay is attributable to second-phase particles that are less cathodic to the aluminium matrix in alloys with increased manganese content. Increasing copper decreased the size of the dissolved polyhedra during stable pitting. Furthermore, pits propagated faster in alloys rich in copper. This could be attributed to an increased level of copper enrichment at the pit walls. Finally, more second-phase particles were present in alloys with increased iron levels. Additionally, pits located in those alloys propagated deeper than pits located in alloys with low levels of iron. A competition between two different types of cathodes, enrichment layer and second-phase particles, is suggested. In conclusion, the effect of microstructure and alloy additions on the corrosion mechanism for crystallographic pitting developed during the project was clarified.

This thesis addresses the development, evaluation and modelling of an anti-segregation system ("AS-System") for.use in larger silos handling alumina in the aluminium smelting industry. This work is unlike much of what has gone before because it is much more grounded in the technical and economic consequences of segregation for a particular manufacturing process. Segregation of particulates, i.e. separation of components due to differences in properties such as size, density etc., has an extensive literature going back as far as 1915, but this focuses mainly on the segregation process itself and largely ignores the context and the consequences. The consequence of segregation is loss of homogeneity; the impact that has on any given process, is generally not addressed very deeply. Surveying the literature on segregation, and studying the total processes of aluminium production, creates a basis for understanding the importance of segregation for aluminium production, as well as the importance of powder technology in general for this industry. A method for quantification of segregation in this production process, based on sampling, has been established. This was intended to give the fundamental information necessary for measuring the extent of the problem and the degree of improvement achieved. By placing sampling points along the logistic chain for the alumina, and by sampling these points for a long enough period, information about the influence of the various handling steps on the bulk solids can be identified. Segregation by particle size is the main type of influence, although the work has shown that attrition is another. Standardised statistical expressions have been used for analysing the bottlenecks of the logistic loops, and study of the results has led to a useful way of expressing the level of segregation, the change of segregation level in a handling step (silo filling and discharge), and improvements in this change. The degree of segregation when handling alumina has proven to be quite considerable in terms of effects on the production process. The effects on the efficiency of the aluminium smelting process, and the environment, have both been evaluated. Variations in the alumina due to segregation have been found to correlate with both dust concentration in the smelter pot room, and anode effects (an unwanted upset in the smelting process). An economical evaluation of an investment in anti segregation systems has been made. This evaluation has shown significant economic consequences, clearly justifying both the investigations of segregation, and the implementation of anti segregation measures. To remedy the effects of air current segregation in the aluminium industry, a complete Anti Segregation System (AS-System) based around Anti Segregation Tubes (AST) utilising a special inlet configuration has been developed. In a number of full size installations, this solution has proved itself capable of handling the variations and transients of process conditions which occur in the industry, with a large operational capacity range, due to the special inlet configuration. The effect of the full scale installed anti segregation systems have been measured, and compared to other systems. The AS-System clearly demonstrated a homogenising effect no matter how low the ingoing variations in particle size were. Other commercial systems which have been evaluated have turned out to be no more than Segregation Effect Damping Systems, since they only seem to reduce the segregation effect after it has happened, instead of trying to eliminate the problem by directly attacking the segregation mechanism itself which is what the AS-System does. A new scaled down test rig for the AS-System was developed, consisting of three ASTs fed from a central distributor. To test the potential effect of the AS-System, to determine its efficiency in countering segregation, tests with repeated filling and emptying of a scale silo were carried out. The results clearly showed that the AS-System very much reduced segregation, compared to conventional filling, even in a small-scale silo. Improved models have been developed for the function of the AST and these have been verified against measurements from the new test rig. The early version of the test rig for the AST used only one centre-mounted tube, with one pressure measurement in the top of the tube. The first models were based on the assumption of the pressure being linear, and assumed full dispersion of the falling material inside the tube; and calibrated from the single pressure measurement inside at the top of the tube. Although this simple model calculated very conservative values of the negative pressure, the model was used for the initial development and design of the AST, and later the ASSystem (Anti Segregation System). A second model was derived, where the material velocity was calculated based on free fall. This model was also based on the idea of full dispersion, but was in better agreement with measured values during further tests, which showed a considerable deviation from the original assumption of a linear pressure distribution once intermediate pressure measurements were available. When using the multi-phase-flow-simulation-program-code FLUENT to simulate the pressure distribution of the AST, the results were quite disappointing, however the FLUENT program was able to identify an initial positive pressure generated by the flow from the inlet box to the tube. Implementing this initial pressure into the simple non-linear model above, both the trend and values correspond quite well with the measured values. A single particle drag model was tried, but dismissed after calculating the maximum possible capacity for known tubes and finding the predictions to be unrealistically low. A new approach was introduced, modelling the fall of the powder in a continuous layer along the inner wall of the tube on one side, creating skin drag along the surface between the falling solid powder and the air. The length of the tube and the width of the chosen AST profile define this surface. This approach assumes that the powder falls like a layer along the tube wall. Previous theory for pressure drop in pneumatic conveying inspired this approach, but it had not previously been used for gravity flow in vertical tubes, and as a result the novel Solid Surface Body Drag Model (SSBDM) was developed. This analytical model gives very good correspondence with the measured data for the pressure distribution inside the AST, yet is extremely simple to use. When comparing the model with measured data, the SSBDM was able to predict the pressure distribution within the error boundaries of the test measurements. A method for design of the AST was derived from the SSBDM, using a dimensionless parameter function determined for the pressure drop model. The models giving the design indicate that the capacity is more than proportional to the cross sectional area of a chosen tube profile, which is in agreement with observations. The model suggests that the capacity is proportional to the cross sectional area in the power of 1.25. This model allowed the study of the effect of tube shape, which revealed that a square profile for the AST does not seem to be the optimum design; rather, a rectangular profile should be chosen for maximum capacity. The model suggests that the capacity is proportional to the width of the side of the tube along which the powder layer is falling, but proportional to the perpendicular side in a rectangular profile in the power of 1.5. The model gives an equation for pressure drop which can also be utilised to place the first valve on the tube. It also shows that for high capacities, and large silos, a system consisting of several ASTs should be chosen (AS-System). Predictions from the model have been tested against the measured capacities of full scale installed systems and give good agreement. Overall, the AS-System has been shown to be cost-effective in reducing segregation; results measured from the full scale installations show a homogenising factor (reduction in variation of the material being handled) of 1-1.5. As a result of these verifications and the simplicity of the model presented in this thesis, the plant engineer can confidently design a system which will function correctly and make a positive, predictable improvement in the homogeneity of the alumina in his plant.

Les procédés de mise en forme de tôles minces sont très largement répandus dans l’industrie. Néanmoins, l’utilisation de ces procédés est limitée par le niveau de formabilité du matériau formé, notamment dans le cas des alliages d’aluminium. Afin d’améliorer ces limites de formabilité, des procédés de mise en forme à chaud peuvent être envisagés. L’objectif de cette thèse est d’étudier à l’aide d’approches expérimentale et numérique l’effet de la température et de la vitesse de déformation sur la formabilité des tôles en alliage d’aluminium AA5086 et de proposer une modélisation capable de prédire ces effets. Une campagne d’essais a été réalisée sur ce matériau à partir d’un essai d’emboutissage de type Marciniak. Des courbes limites de formage (CLF) ont été établies sur une plage de température allant de l’ambiant jusqu’à 200°C et pour des vitesses de déformation allant du quasi-statique à 2s-1. Des effets, positif de la température et négatif de la vitesse de déformation sur la formabilité ont été mis en évidence. La prise en compte des effets de la température et de la vitesse de déformation dans les modèles prédictifs des CLF, qu’ils soient analytiques ou numériques, est à ce jour très limitée. Dans ce travail, un modèle numérique prédictif basé sur la simulation par éléments finis du modèle géométrique de Marciniak et Kuczynski (M-K) est proposé. Les déformations limites obtenues avec de ce modèle sont très sensibles à la description du comportement thermo-viscoplastique du matériau et à la calibration du défaut géométrique pilotant l’apparition de la striction dans le modèle M-K. Des essais de traction uniaxiale réalisés dans les mêmes conditions opératoires que les essais de mise en forme de Marciniak ont permis d’identifier des lois d’écrouissage de nature très différentes (rigidifiante, saturante ou mixte). Ces lois conduisent à des prédictions très différentes de la formabilité du matériau pour une valeur donnée du défaut géométrique du modèle EF M-K. Différentes stratégies de calibration de la taille de ce défaut initial ont été envisagées. L’utilisation du point expérimental de la CLF correspondant à des conditions de déformation plane permet de calibrer de manière satisfaisante la valeur de ce défaut. Cette procédure de calibration a été appliquée pour l’ensemble des lois identifiées. Les lois de nature rigidifiante de type Ludwick se sont montrées les plus effficaces alors que les lois saturante de type Voce se sont avérées incapables de prédire la formabilité du matériau pour certaines conditions opératoires. Finalement, il est démontré qu’une valeur constante du défaut géométrique ne peut être retenue pour l’ensemble des conditions opératoires étudiées même si le modèle M-K s’est avéré assez efficace pour représenter l’effet de la température plutôt que celui de la vitesse de déformation. / Sheet metal forming processes are widely used in industry. Nevertheless, the use of these processes is limited by the formability of the considered material, in particular in the case of the aluminium alloys. To improve the formability, warm forming processes can be considered. The objective of this work is to study by means of both experimental and numerical approaches, the effects of temperature and strain rate on the formability of AA5086 aluminium alloy sheets and to propose a modeling suitable to predict these effects. Experimental tests have been carried out on this material by means of the Marciniak stamping experimental device. Forming limit curves (FLCs) have been established on a temperature range going from ambient temperature to 200°C and on a strain rate range going from quasi-static up to 2s-1. A positive effect of the temperature and a negative effect of the strain rate on the formability limits were highlighted. To date, very few predictive models of the FLCs taking into account temperature and strain rate effects are proposed in the literature. In this work, in order to predict the experimental temperature and strain rate sensitivities, a predictive model based on the finite element simulation of the Marciniak and Kuczynski (M-K) geometrical model is proposed. The limit strains obtained with this model are very sensitive to the description of the thermo-viscoplastic behaviour modeling and to the calibration of the initial geometrical imperfection controlling the onset of the necking. Thanks to tensile tests carried out for the same operating conditions that those of Marciniak forming tests, several types (power law, saturation and mixed) of hardening laws have been identified. These hardening laws have been implemented in theFE M-K model to obtain numerical limit strains. Very different formability limits have been observed for a given value of the geometrical defect. Several strategies for the calibration of this initial imperfection size have been tested. The use of the experimental point of the FLC0 corresponding to plane strain condition allows a good calibration of the initial imperfection value. This calibration procedure was carried out for all hardening laws. It is shown that the power law type models such as Ludwick law are more efficient while saturation laws such as Voce law are unable to predict the material formability for some conditions. Finally, it is shown that a constant value of the geometrical defect cannot be used to the whole operating conditions studied even if FE M-K model is shown to be efficient to represent the temperature effect rather than strain rate one.

The aluminium AA1050 alloy, known as commercially pure aluminium, contains 99.5% Al, together with Fe and Si as major alloying elements. During fabrication of aluminium substrates for lithographic printing plates in Bridgnorth Aluminium Ltd, the AA 1050 aluminium alloy proceeds through various stages of thermomechanical processing, with the conditions at each processing stage influencing the microstructure of the final coil. Because of its specific gravity, tensile strength, surface performance and coating adhesion behaviour, the AA 1050 aluminium alloy is one of the preferred materials for offset printing, which has been the dominant printing process for years. During manufacturing of the offset plate, the AA 1050 alloy is subjected to alkaline etching, electrograining and anodizing. Reactivity of the material to those chemical and electrochemical processes depends on various alloy properties, the thickness and composition of oxide film over the macroscopic alloy surface, cold work applied and the presence of second phase particles, which influence properties and quality of the final product.During the project, the main objectives were to understand the process in the production of the final product from slab to coil as well as to investigate some microstructural changes during the following stages of the production process and, finally, the performance behaviour of the final product.The set of experiments, including microstructural observation and electrochemical tests, has been developed to investigate the AA 1050 aluminium sheet in accordance with the objective of this study. Four homogenisation trials in the industry environment were performed to enable sample collection from the real production line; also, samples from each processing stage were examined with the special attention paid to those collected during the plant experimental homogenisation trials. It was found that the microstructure of the aluminium changed throughout the different production stages and influences the material response in the alkaline solution used for etching. Furthermore, the conditions of homogenisation (time and temperature) have impact on the properties like the electrochemical behaviour in alkaline and acid solutions, as well as the microstructure of the final aluminium sheet. Differentiation between the behaviour of final gauge samples was possible in terms of characterisation of the second phase particles characterisation (distribution and composition) present in the resultant alloy product.

Στην παρούσα διδακτορική διατριβή μελετάται η ανάπτυξη λεπτών υμενίων πορωδών ανοδικών οξειδίων του αλουμινίου (αναφέρονται και ως πορώδης ανοδική αλουμίνα) σε υπόστρωμα πυριτίου. Επιπλέον, εξετάζεται η ανάπτυξη εφαρμογών που αφορούν τη χρήση της πορώδους αλουμίνας ως μάσκα και ως μήτρα για την δημιουργία νανονημάτων ή κβαντικών τελειών (νανονησίδων) στο Si. Το πρώτο κεφάλαιο πραγματεύεται τη θεωρία και τους μηχανισμούς που διέπουν την ανάπτυξη πορωδών υμενίων, που προέρχονται από ανοδική οξείδωση (ανοδίωση) τόσο φύλλων αλουμινίου, όσο και υμενίων αλουμινίου σε υπόστρωμα πυριτίου. Επιπροσθέτως, παρατίθεται ο ρόλος που διαδραματίζουν οι ηλεκτροχημικές συνθήκες ανοδίωσης, όπως το pH, η θερμοκρασία και η εφαρμοζόμενη τάση, στα τελικά δομικά χαρακτηριστικά των πορωδών υμενίων. Στο δεύτερο κεφάλαιο παρουσιάζονται τα τεχνολογικά βήματα διεργασιών που αφορούν την προετοιμασία των δειγμάτων τα οποία πρόκειται να ανοδιωθούν, και δίνονται λεπτομέρειες για την πειραματική διάταξη η οποία χρησιμοποιείται κατά την ανοδίωση. Στο τρίτο κεφάλαιο μελετώνται εκτενώς, τρεις παράγοντες που έχουν σημαντική επίδραση στα τελικά δομικά χαρακτηριστικά των πορωδών υμενίων. Κατά τους δύο πρώτους, εξετάζεται η επίδραση του πάχους του προς ανοδίωση υμενίου αλουμινίου πάνω στο Si, καθώς και ο περιορισμός του σε επιφάνειες μερικών τετραγωνικών μικρομέτρων πάνω στο Si, στο μέγεθος και την πυκνότητα των πόρων. Ο τρίτος παράγοντας αφορά το ρόλο της ανοδίωσης του υμενίου του αλουμινίου σε δύο και τρία στάδια σε συνδυασμό με τη χημική εγχάραξή του μετά από κάθε στάδιο ανοδίωσης, στην ανάπτυξη εξαγωνικής συμμετρίας στην κατανομή των πόρων. Το τέταρτο κεφάλαιο, πραγματεύεται την ανάπτυξη εφαρμογών που συνδέονται με τη χρήση της πορώδους αλουμίνας ως μάσκα και ως μήτρα για τη δημιουργία νανοδομών επάνω στο πυρίτιο. Ως εκ τούτου παρουσιάζεται η δημιουργία νανονησίδων Cr, Ti, νανοστηλών Si, και νανονημάτων Au, πάνω στο Si, εφαρμογές στις οποίες τα πορώδη ανοδικά υμένια χρησιμοποιήθηκαν ως ενδιάμεσο στάδιο. Στο πέμπτο κεφάλαιο παρατίθεται η ανάπτυξη διαμέσου της πορώδους αλουμίνας, εξαγωνικά διατεταγμένων νανονησίδων SiO2 στο Si. Επίσης, παρουσιάζεται ο ηλεκτρικός χαρακτηρισμός διατάξεων οι οποίες αποτελούνται από την εν λόγω δομή. Σε ένα επιπλέον βήμα, οι νανονησίδες SiO2 χρησιμοποιούνται για την ανάπτυξη νανοκρυσταλλιτών Si στο εσωτερικό τους μέσω της τεχνικής της ιοντικής σύνθεσης. Τα σημαντικότερα αποτελέσματα και συμπεράσματα που προέκυψαν από την εκπόνηση της παρούσας διδακτορικής διατριβής συνοψίζονται στα εξής: • Βελτίωση της εξαγωνικής συμμετρίας στην κατανομή των πόρων, μέσω ανοδίωσης σε δύο ή τρία στάδια σε συνδυασμό με χημική εγχάραξη του προς ανοδίωση αλουμινίου έπειτα από κάθε στάδιο ανοδίωσης. • Αύξηση της πυκνότητας των πόρων των ανοδικών υμενίων κατά μία τάξη μεγέθους, με περιορισμό του προς ανοδίωση αλουμινίου σε προεπιλεγμένες περιοχές στο Si, επιφάνειας μερικών τετραγωνικών μικρομέτρων. • Ανάπτυξη διατεταγμένων νανοδομών Ti και Cr σε υπόστρωμα Si χρησιμοποιώντας λεπτά υμένια πορώδους αλουμίνας πάνω σε Si. Ιδιαίτερα οι δομές Cr, μπορούν να χρησιμοποιηθούν ως μεταλλική νανοδομημένη μάσκα για την εγχάραξη με ενεργά ιόντα του υποστρώματος Si και τη δημιουργία νανοστηλών Si πάνω σε αυτό. Η δημιουργία νανοστηλών Si, βρίσκει πληθώρα εφαρμογών στη Νανοηλεκτρονική, σε αισθητήρες, Nανοφωτονική, μνήμες κ.τ.λ. • Οι πυκνότητες διεπιφανειακών καταστάσεων που προέκυψαν από τον ηλεκτρικό χαρακτηρισμό της διεπιφάνειας υμενίων πορώδους αλουμίνας με το πυρίτιο, και της διεπιφάνειας πορώδους αλουμίνας – νανονησίδων SiO2 με το πυρίτιο. Οι τιμές που υπολογίστηκαν είναι ενθαρρυντικές, αν ληφθεί υπόψη ο ηλεκτροχημικός τρόπος παρασκευής των εν λόγω σύνθετων υμενίων πάνω στο πυρίτιο. • Ανάπτυξη μεμονωμένων νανοκρυσταλλιτών Si ενσωματωμένων σε νανονησίδες SiO2. Για το σκοπό αυτό συνδυάστηκαν δύο διαφορετικές τεχνολογίες, εκείνη της ιοντικής σύνθεσης και εκείνη της ανάπτυξης νανονησίδων SiO2 διαμέσου λεπτών υμενίων πορώδους αλουμίνας απευθείας σε υπόστρωμα Si. Τέτοιες δομές νανοκρυσταλλιτών έχουν εφαρμογές σε διατάξεις μη πτητικών μνημών, όπου η κατανεμημένη αποθήκευση φορτίου στους νανοκρυσταλλίτες ευνοεί τη χρήση λεπτότερων οξειδίων πύλης και τη δυνατότητα σμίκρυνσης του πάχους των οξειδίων αυτών χωρίς να μειώνεται ο χρόνος αποθήκευσης φορτίου. / In the present thesis, the growth of porous anodic alumina films on Si substrate was studied extensively. Potential applications of porous anodic alumina films formed directly on Si, regarding the use of porous membranes as mask or template for various nanostructures growth directly on Si, are discussed. Chapter one deals with the theory and mechanisms governing porous anodic alumina film growth, either on porous anodic films formed by anodization of aluminum foils, or on porous anodic films developed on Si substrates. Additionally, the effect of different factors (pH, temperature, applied voltage) on the final structural characteristics is presented. In chapter two, the preliminary processing steps regarding sample preparation before the anodization procedure are quoted. Moreover, details about the experimental set-up and the electrochemical conditions used during the sample anodization in the current work are given. In chapter three, the influence of three different factors, in the final structural characteristics, is investigated. Primarily, the impact of the initial aluminum thickness deposited on Si substrate, and secondly the confinement of the aluminum film in areas of a few μm2, in the pore size and pore density are studied. Finally, the influence of the third factor is associated with a three-step instead of a two-step anodization, in combination with an in-between step of aluminum chemical etching, on the ordering and the uniformity of the pores. The deposition of Ti and Cr nanodots arrays on Si, using the porous alumina membrane as a masking layer, is investigated in chapter four. Furthermore, the Ti nanodots are used for the electrodeposition of Au nanodots and nanowires inside the porous alumina films. Additionally, the Cr dots are used as metallic nanostructured mask for the Si etching by reactive ion etching process, that leads to the formation of Si nanopillars on Si substrate. In chapter five the growth of hexagonally ordered SiO2 dots on Si through porous anodic alumina membranes, in various acidic electrolytes, is studied. Moreover, the electrical characterization of the interface of porous alumina film/Si and porous alumina film with SiO2 dots in pore bottoms/ Si is presented. Finally, in the present thesis the technology of fabrication of Si nanocrystals embedded in SiO2 dots arrays through porous alumina membranes on Si substrate is developed for the first time. This was achieved by the combination of ion beam synthesis with the already existing technology of porous anodic alumina growth on Si substrates. The nanocrystals are electrically isolated from the substrate. This technique is promising as an application in non-volatile memory devices. The main achievements accomplished through this study are summarized as follows: • The optimization of pores ordering by developing the porous alumina membrane in two or three processing steps in combination with the chemical etching of Al film, lying above the porous membrane, following each anodization cycle. • The increase of porous density by the confinement of porous alumina film in areas of a few μm2 on Si. • The development of Ti, Cr and nanodots arrays, directly on Si, through porous alumina membranes. The use of Cr nanodots as nanostructured masking layer for the formation of Si nanopillars, formed by etching of Si substrate with RIE, on Si. • The density of interface stages results from the electrical characterization of porous alumina with or without SiO2 dots at each pore bottom, with the Si substrate. The results are encouraging, keeping in mind that the pore membranes and SiO2 dots were electrochemically grown directly on Si substrate. • The development of distinct Si nanocrystalls, embedded in SiO2 dots, combining for the first time two different technologies, that is the fabrication of porous anodic alumina films directly on Si substrate, as well as the ion beam synthesis technique. The proposed technique is promising for the fabrication of non-volatile memory devices.