Τα κριτήρια σχεδιασμού στις σύγχρονες κατασκευές και κυρίως στην αεροναυπηγική και ναυπηγική βιομηχανία, στοχεύουν στην παραγωγή δομικών στοιχείων με μειωμένο βάρος και χαμηλότερο κόστος, ενώ ταυτόχρονα, απαιτείται να παρουσιάζουν υψηλότερες επιδόσεις και ικανοποιητική δομική ασφάλεια. Οι στόχοι αυτοί έχουν διαμορφώσει μια σχεδιαστική τάση η οποία οδηγεί στην αντικατάσταση των ‘παραδοσιακών’ διαφορικών δομών (differential structures) με ‘σύγχρονες’ ολοκληρωμένες δομές (integral structures). Η τάση αυτή βρίσκει εφαρμογή κατά κύριο λόγο στην αεροναυπηγική, όπου η μείωση του βάρους χωρίς υποβάθμιση της ασφαλούς λειτουργίας αποτελεί βασικό και μόνιμο στόχο. Η αυξημένη παραγωγή δομικών στοιχείων ολοκληρωμένων δομών έχει οδηγήσει σε συνεχή αύξηση της εφαρμογής διεργασιών συνένωσης με έμφαση στις προηγμένες διεργασίες συγκόλλησης. Οι διεργασίας συγκόλλησης οι οποίες, λόγω των πλεονεκτημάτων τους, βρίσκονται στην αιχμή της τεχνολογίας είναι η Συγκόλληση με Τριβή και Ανάμιξη (Friction Stir Welding – FSW) και η Συγκόλληση με Ακτίνα Λέιζερ (Laser Beam Welding – LBW). Η εφαρμογή συγκολλήσεων στην παραγωγή ολοκληρωμένων δομών έχει πολλά τεχνολογικά πλεονεκτήματα έναντι των άλλων τύπων σύνδεσης, ωστόσο, συνοδεύονται από την ανάπτυξη Παραμενουσών Τάσεων και στρεβλώσεων στο τελικό προϊόν, κάτι το οποίο, ανάλογα με την εφαρμογή, μπορεί να προκαλέσει σημαντικά προβλήματα. Συγκεκριμένα, οι στρεβλώσεις επηρεάζουν τη λειτουργικότητα του δομικού στοιχείου, αφού μεταβάλλουν την γεωμετρία του, ενώ οι παραμένουσες τάσεις, αναπροσαρμόζοντας το εσωτερικό εντατικό πεδίο, επιδρούν στη δομική τους ακεραιότητα. Όπως είναι γνωστό με κατάλληλη επιλογή των παραμέτρων της διεργασίας (π.χ. ταχύτητα συγκόλλησης, ισχύς κτλ) μπορεί να επιτευχθεί μείωση των αναπτυσσόμενων παραμενουσών τάσεων και στρεβλώσεων. Επίσης, τα τελευταία χρόνια έχει αποδειχθεί ότι η προσομοίωση μιας διεργασίας συγκόλλησης μπορεί να βοηθήσει σημαντικά στην επιλογή του βέλτιστου συνδυασμού των παραμέτρων της. Για το λόγο αυτό, μεγάλο μέρος της ερευνητικής δραστηριότητας στην περιοχή των προηγμένων διεργασιών συγκόλλησης έχει στραφεί προς την ανάπτυξη αξιόπιστων μεθοδολογιών προσομοίωσης, οι οποίες με δεδομένο (input data) τις παραμέτρους της διεργασίας μπορούν να δώσουν σαν αποτέλεσμα (output data) κρίσιμες απαντήσεις όσον αφορά στις τεχνολογικές ιδιότητες της συγκόλλησης. Βάσει των ανωτέρω, σκοπός της παρούσης διατριβής είναι η ανάπτυξη ολοκληρωμένων μεθόδων θερμομηχανικής προσομοίωσης των προηγμένων διεργασιών συγκόλλησης FSW και LBW με κύριο στόχο την πρόβλεψη των παραμενουσών τάσεων και των στρεβλώσεων καθώς και τη μελέτη της επίδρασης τους στη δομική ακεραιότητα των παραγόμενων δομικών στοιχείων. Ένα από τα σημαντικότερα και ίσως το κρισιμότερο στάδιο κατά την προσομοίωση μιας θερμομηχανικής διεργασίας είναι η εξομοίωση της θερμικής πηγής και ο υπολογισμός του θερμικού φορτίου, γιατί μια εσφαλμένη εκτίμηση του θερμικού φορτίου προκαλεί λανθασμένη πρόβλεψη της θερμοκρασιακής κατανομής και κατά συνέπεια εισάγει σφάλματα στον υπολογισμό των παραμενουσών τάσεων και των στρεβλώσεων. Στη βάση αυτή, τόσο για την περίπτωση της FSW όσο και για την LBW αναπτύχθηκαν μεθοδολογίες για τον προσδιορισμό των θερμικών πηγών τους και συνοδεύτηκαν από θερμικά μοντέλα για την πρόβλεψη του θερμοκρασιακού ιστορικού. Ακολούθως, το θερμοκρασιακό ιστορικό ασκείται υπό τη μορφή εξωτερικού φορτίου σε ένα θερμομηχανικό μοντέλο από όπου υπολογίζονται οι παραμένουσες τάσεις και οι στρεβλώσεις της διεργασίας. Τέλος, η εσωτερική εντατική κατάσταση του συγκολλημένου δομικού στοιχείου συνυπολογίζεται στο εντατικό πεδίο λόγω της φόρτισης λειτουργίας της κατασκευής και γίνεται πρόβλεψη των συντελεστών έντασης τάσης (Stress Intensity Factors - SIFs ) έτσι ώστε να εκτιμηθεί η επίδρασης της συγκόλλησης στη δομική ακεραιότητα. Τόσο το θερμομηχανικό όσο και το θραυστομηχανικό μοντέλο μπορούν να προσαρμοσθούν σε πολλούς διαφορετικούς τύπους σύνδεσης και ρηγμάτωσης, αντίστοιχα. / The design criteria in modern structures aim to the production of components with reduced weight and low cost, as well as, with higher performance and increased safety. The above goals lead to a tendency of replacing traditional differential structures with more modern integral structure, mainly in aeronautic sector where the weight and cost reduction, without decrease of safety, comprises the main target of the current research effort. The production of integral structures requires the adaptation of existing forming processes as well as the development and optimization of advanced welding processes. The most promising welding processes in aeronautics and maritime industries currently are the Friction Stir Welding–FSW and Laser Beam Welding-LBW. Despite of the many technological advantages of FSW and LBW process, their application in the production of integral structures leads to the development of Residual Stress (RS) and distortion fields which can cause significant problems. Specifically, distortions can effect on the components assembly, while, RS affect the structural integrity. However, an appropriate selection of process parameters can significantly reduce the RS and distortions levels. The usual way to optimize process parameters is experimental trial and error approach; recently, process simulation has been proven efficient, too. The present work aims to the development of efficient methodologies for the thermomechanical simulation of FSW and LBW processes in order to predict temperature history, as wells as RS and distortion fields. Consequently, the RS field is used for the determination of the welding effects on the structural integrity of the welded component. Generally, the reliability of a simulation methodology of any thermo-mechanical process, such as welding, is seriously affected by many parameters; two of them are very base, namely, the accurate determination of the heat input introduced to the material (thermal load) and the accurate representation of thermal and mechanical boundary conditions. As the boundary conditions determined by the welder and it is usually easy to transfer in a numerical model, one of the most difficult simulation issues is the appropriate determination of the heat input which will lead to an accurate prediction of the material temperature history. For this reason, one of the main objectives of the present work is to develop methodologies for the accurate thermal load calculation in both FSW and LBW processes. After the validation of the developed methodologies with respect to experimental measurements, the defined heat sources are used in global thermal models in order to predict the temperature histories which, thereinafter, are introduced in the thermo-mechanical models to predict the developed RS and distortion fields. Finally, the structural integrity of the welded component, under the effect of both RS field and service loading is studied; different possible ‘fracture scenarios’ are investigated based on the Stress Intensity Factor concept and the Elastic Fracture Mechanics principles.

O desenvolvimento e utilização de novos materiais, mais leves e com propriedades mecânicas superiores aos atuais, se mostram extremamente importantes devido à redução de peso e consequentemente redução na emissão de gases poluentes que poderiam gerar. As ligas de Fe-Mn-C com elevados teores de Mn (20-30%) representam um desenvolvimento muito recente de aços austeníticos, que, através dos seus mecanismos diferenciados de deformação reúnem elevada resistência mecânica com grande ductilidade. Essa nova classe de materiais estruturais possibilita uma efetiva redução de custos na produção através do reduzido tempo de processamento (sem a necessidade de tratamentos térmicos especiais e de processamentos termomecânicos controlados). A soldagem é, atualmente, o mais importante processo de união de metais usado no setor industrial. Dentro da variada gama de processos de soldagem existentes, a soldagem por fricção e mistura mecânica (SFMM, em inglês: Friction Stir Welding - FSW) se destaca por ser um processo de união no estado sólido que apresenta uma série de vantagens sobre as tecnologias convencionais de soldagem por fusão. Do ponto de vista metalúrgico, uma das suas principais vantagens se manifesta justamente na junção de materiais dissimilares, visto que o grau de mistura de composições e as transformações de fases entre materiais incompatíveis podem ser minimizados. Outra vantagem é que há um refino de grão no cordão de solda comparado com a microestrutura fundida que se forma nos processos convencionais. Este trabalho teve como objetivo produzir em escala laboratorial os aços de alta liga ao manganês com efeito TRIP, avaliar o impacto da velocidade de rotação da ferramenta na soldagem por fricção e mistura mecânica e avaliar a microestrutura e propriedades mecânicas das juntas soldadas. A microestrutura das juntas soldadas caracterizou-se pela presença apenas da zona de mistura e do metal base, além da formação de \'anéis de cebola\' na zona de mistura, esta não mostrou sinais de transformação martensítica induzida por deformação e sofreu recristalização dinâmica para todas as velocidades de rotação investigadas com a formação de grãos refinados e com morfologia equiaxial. Os corpos de tração fraturaram todos nos metais de base, mostrando que as propriedades mecânicas da zona de mistura foram superiores à do metal base e que a variação de aporte térmico alcançada com a velocidade de rotação da ferramenta não comprometeu a qualidade das juntas soldadas. / The development and application of new light materials with superior mechanical properties is extremely important to weight reduction in vehicles and consequently reduction of greenhouse gases emission. The Fe-Mn-C steels with high Mn (20-30%) are a recent development of austenitic steels, which, due to their different mechanisms of deformation, possesses high strength and high ductility as well. In addition, this new type of structural steel allows an effective reduction of manufacturing costs due to its reduced processing time (it does not require special heat treatments and controlled thermo mechanical processing). Welding has been one of the most important processes for joining metals. Among the available welding processes, friction stir welding (FSW) is notable for being a solid state process with great advantages over the conventional welding methods. In the mettalurgical point of view, welding dissimilar materials is a significant advantage of FSW over the other process. The main reason is the reduction of mixture of material and phase transformations between the incompatible materials in the weld. Moreover, grain refinement is another advantage from the process. The present study aimed to produce laboratorial scale high Mn steels with TRIP effect, investigate the impact of tool speed ont the microstructure and mechanical properties of friction stir welded joints. The microstructure of the welded joints exhibited only the stirred zone (SZ) and the base material (BM), besides the presence of ´onion rings´ within the stirred zone. The SZ exhibited no signs of martensite suggesting that dynamic recrystallization have occurred for all the speed tested. Moreover, the grains in the SZ had equiaxial morphology and were significantly refined. The fracture of the tensile specimens occurred in the base material, bringing to light that the welding process was beneficial to the mechanical properties. Furthermore, the variation of heat input achieved with the speed did not compromise the quality of welded joints.

Composite materials are multifunctional materials having unique mechanical and physical properties that can be tailored to meet the requirements of a particular application. Aluminium based Metal Matrix Composites (MMC) always draw the attention of researchers due to its unique characteristics such as better strength to weight ratio, low wear rate and lower thermal expansion coefficient. There are various methods for manufacturing of MMC that can be grouped into two major categories: (a) Solid sate method such as powder metallurgy, co-extrusion and (b) Liquid state method such as stir casting. All of these methods for production of composites have their own advantages and disadvantages. Porosity, and poor wettabilty of dispersoids with matrix are few common problems in solid state route. Formations of undesirable phases, and segregation of dispersoids are common problems in liquid state processing route. Friction Stir Processing (FSP) technique, a derivative technique of Friction Stir Welding (FSW) has emerged as a major solid state technique to produce composites. However, there are several challenges associated with it. Most of the past work has been on limited volume of material. Researchers have tried to combine FSP technique with powder metallurgy technique to overcome aforementioned challenges associated with these techniques. Where on one hand, powder metallurgy ensures the uniform dispersion of dispersoids in the matrix, on the other hand FSP on sintered billet removes the pores and other defects. The combination of these two techniques leads to a more controlled and uniform properties. However, at the same time, it can be noted that the combination of these processes is tedious and time consuming. In this study, an attempt is made to achieve bulk dispersion of a second phase into an aluminium matrix using FSP technique. A 5 mm thickness composite is attempted in this work. To achieve this objective proper and uniform mixing of the particles is required. To achieve this, new tools and processing steps are to be designed and analyzed for a better understanding of material flow around the tool pin and the effect of different tool pin geometries on the material flow. Keeping this objective, a detailed study is carried out on material flow during FSW process using aluminium as base metal. A marker material technique is employed to understand the material flow. A strip of copper is selected as the marker material. Material flow can be qualitatively predicted during the process by observing the distribution of marker material in the weld nugget. Three different kinds of tools, each with an additional feature are designed for this purpose (a) Plain frustum shape pin (b) threaded frustum shape pin and, (c) Triflute pin . The material flow due to the plain pin tool can be considered as primary flow during the FSP. Three different kinds of flow zones are observed in the weld nugget in the case of plain tool. It is found that higher numbers of geometrical features (threads and flutes) not only enhance the material flow but also lead to the additional flow currents and more thorough and uniform mixing. A closer study of the weld nugget revealed that the copper marker particles and the matrix were diffusion bonded. Based on the reaction time available and temperature in the weld nugget a diffusion layer thickness of 4 nm is expected between copper and aluminium. However, the diffusion layer thickness was found to be 3.5 μm, which is nearly three orders of magnitude higher. This can be attributed to the enhancement of diffusion due to simultaneous application of strain and temperature. As copper is soluble in the aluminium, an insoluble marker material tin was used for study of flow in the weld nugget. However, the effect of insolubility and lower melting point had some unexpected effect on the processing loads. The normal load during steady state tool traverse in conventional butt-welding is found to be around 2.7 KN while it attains an average value of 14.7 KN when a thin strip of tin is sandwiched between these plates. However, a drop in the torque of around 13.12 NM is observed when tin was sandwiched between the plates as compared to the case when no insert was present. On closer examination of the flow behavior, it is seen that the tin melted, squeezed out and formed a lubricious layer between the tool and the work piece. This reduced the torque significantly and a concomitant drop in temperature was observed. The interaction between the tool and the colder aluminium work piece would thus result in much larger normal and transverse load Based on the expected and unexpected results of flow pattern in the weld nugget, a new FSP tool and processing steps were developed to manufacture MMC. Tungsten, which is the highest melting point metal is chosen as the dispersing phase. Further, as tungsten has high melting point, the kinetics of intermetallics formation would be low for the given FSP processing time at the processing temperature. This would lead to tungsten acting as a more ductile strengthening particle, which is expected to should give some unique characteristics to the MMC. Tungsten powder with an average diameter of 414 nm was dispersed in aluminum matrix with three different proportions after optimizing all the process parameters. It is noted that the mechanical properties are significantly influenced as the tungsten content in the matrix increases. In practice, MMC shows relatively low ductility compared to the parent metal. However in this case the composite exhibited even better ductility than the as received aluminium plates (rolled sheets). The composite showed around 129 MPa of yield strength along with 21% ductility when tungsten content is 3.8 at.%. It is also found that the reaction between aluminum and tungsten occurs during the processing and form the Al12W intermetallic phase. Though the formation of this intermetallic phase was unlikely due to the low temperature and short time available during the process, the reaction kinetics between aluminium and tungsten would have been enhanced due to the simultaneous application of strain and temperature. Given that the metal-metal, tungsten-aluminium composite produced by FSP had unique properties and also formed intermetallics, a study on incorporation of a highly insoluble material, graphite was carried out. Further graphite with its own unique properties and very low wettability with aluminium could possibly impart completely different properties to the system. Past work on graphite aluminium composites produced by other methods did not show promise. As FSP imposes high strains at relatively high flow stresses on the processed material, it was seen that the graphite got sheared to form multi-layer graphene composites with the aluminium. The graphene sheets are formed by mechanical exfoliation of graphite particles during its incorporation in the matrix. The formation of graphene was confirmed after separating the graphite from the processed zone and TEM studies of the composite. It is seen that most of the graphite got converted into multilayer graphene. This aluminium-graphene composite exhibited enhanced ductility and UTS. As received aluminium plates exhibited only 11% ductility and around 100 MPa of UTS while this composite exhibited around 26 % ductility and 147 MPa of UTS. However, there is only a slight improvement in yield strength of this composite.

The Al-Zn-Mg-Cu (7XXX series) alloys are amongst the strongest aluminum available. However, they are considered unweldable with conventional fusion techniques due to the negative effects that arise with conventional welding, including hydrogen porosity, hot cracking, and stress corrosion cracking. For this reason, friction stir welding has emerged as the preferred technique to weld 7XXX series alloys. Aluminum 7449 is one of the highest strength 7XXX series aluminum alloy. This is due to its higher zinc content, which leads to a higher volume fraction of eta' precipitates. It is typically used in a slight overaged condition since it exhibits better corrosion resistance. In this work, the welds of friction stir welded aluminum 7449 were studied extensively. Specific focus was placed in the heat affected zone (HAZ) and nugget. Thermocouples were used in the heat affected zone for three different depths to obtain thermal profiles as well as cooling/heating profiles. Vicker microhardness testing, transmission electron microscope (TEM), and differential scanning calorimeter (DSC) were used to characterize the welds. Two different tempers of the alloy were used, a low overaged temper and a high overaged temper. A thorough comparison of the two different tempers was done. It was found that highly overaged aluminum 7449 tempers show better properties for friction stir welding. A heat gradient along with a high conducting plate (Cu) used at the bottom of the run, resulted in welds with two separate microstructures in the nugget. Due to the microstructure at the bottom of the nugget, higher strength than the base metal is observed. Furthermore, the effects of natural aging and artificial aging were studied to understand re-precipitation. Large improvements in strength are observed after natural aging throughout the welds, including improvements in the HAZ.

The recent emphasis on magnesium alloys can be appreciated by following the research push from several agencies, universities and editorial efforts. With a density equal to two-thirds of Al and one-thirds of steel, Mg provides the best opportunity for lightweighting of metallic components. However, one key bottleneck restricting its insertion into industrial applications is low strength values. In this respect, Mg-Y-Nd alloys have been promising due to their ability to form strengthening precipitates on the prismatic plane. However, if the strength is compared to Al alloys, these alloys are not attractive. The primary reason for low structural performance in Mg is related to low alloying and microstructural efficiency. In this dissertation, these terminologies are discussed in detail. A simple calculation showed that the microstructural efficiency in Mg-4Y-3Nd alloy is 30% of its maximum potential. Guided by the definitions of alloying and microstructural efficiency, the two prime objectives of this thesis were to: (i) to use thermomechanical processing routes to tailor the microstructure and achieve high strength in an Mg-4Y-3Nd alloy, and (ii) optimize the alloy chemistry of the Mg-rare earth alloy and design a novel rare—earth free Mg alloy by Calphad approach to achieve a strength of 500 MPa. Experimental, theoretical and computational approaches have been used to establish the process-structure-property relationships in an Mg-4Y-3Nd alloy. For example, increase in strength was observed after post aging of the friction stir processed/additive manufactured microstructure. This was attributed to the dissolution of Mg2Y particles which increased the alloying and microstructural efficiency. Further quantification by numerical modeling showed that the effective diffusivity during friction stir processing and friction stir welding is 60 times faster than in the absence of concurrent deformation leading to the dissolution of thermally stable particles. In addition, the investigation on the interaction between dislocations and strengthening precipitate revealed that, specific defects like the I1 fault aid in the accelerated precipitation of the strengthening precipitate in an Mg-4Y-3Nd alloy. Also, the effect of external field (ultrasonic waves) was studied in detail and showed accelerated age hardening response in Mg-4Y-3Nd alloy by a factor of 24. As the bottleneck of low strength is addressed, the answers to the following questions are discussed in this dissertation: What are the fundamental micro-mechanisms governing second phase evolution in an Mg-4Y-3Nd alloy? What is the mechanical response of different microstructural states obtained by hot rolling, friction stir processing and friction stir additive manufacturing? Is defect engineering critical to achieve high strength Mg alloys? Can application of an external field influence the age hardening response in an Mg-4Y-3Nd alloy? Can a combination of innovative processing for tailoring microstructures and computational alloy design lead to new and effective paths for application of magnesium alloys?

Metal fatigue is a recurring problem for metallurgists and materials engineers, especially in structural applications. It has been responsible for many disastrous accidents and tragedies in history. Understanding the micro-mechanisms during cyclic deformation and combating fatigue failure has remained a grand challenge. Environmental effects, like temperature or a corrosive medium, further worsen and complicate the problem. Ultimate design against fatigue must come from a materials perspective with a fundamental understanding of the interaction of microstructural features with dislocations, under the influence of stress, temperature, and other factors. This research endeavors to contribute to the current understanding of the fatigue failure mechanisms. Cast aluminum alloys are susceptible to fatigue failure due to the presence of defects in the microstructure like casting porosities, non-metallic inclusions, non-uniform distribution of secondary phases, etc. Friction stir processing (FSP), an emerging solid state processing technique, is an effective tool to refine and homogenize the cast microstructure of an alloy. In this work, the effect of FSP on the microstructure of an A356 cast aluminum alloy, and the resulting effect on its tensile and fatigue behavior have been studied. The main focus is on crack initiation and propagation mechanisms, and how stage I and stage II cracks interact with the different microstructural features. Three unique microstructural conditions have been tested for fatigue performance at room temperature, 150 °C and 200 °C. Detailed fractography has been performed using optical microscopy, scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). These tools have also been utilized to characterize microstructural aspects like grain size, eutectic silicon particle size and distribution. Cyclic deformation at low temperatures is very sensitive to the microstructural distribution in this alloy. The findings from the room temperature fatigue tests highlight the important role played by persistent slip bands (PSBs) in fatigue crack initiation. At room temperature, cracks initiate along PSBs in the absence of other defects/stress risers, and grow transgranularly. Their propagation is retarded when they encounter grain boundaries. Another major finding is the complete transition of the mode of fatigue cracking from transgranular to intergranular, at 200 °C. This occurs when PSBs form in adjacent grains and impinge on grain boundaries, raising the stress concentration at these locations. This initiates cracks along the grain boundaries. At these temperatures, cyclic deformation is no longer microstructure- dependent. Grain boundaries don’t impede the progress of cracks, instead aid in their propagation. This work has extended the current understanding of fatigue cracking mechanisms in A356 Al alloys to elevated temperatures.

Das ultraschallunterstützte Rührreibschweißen (USE-FSW) als innovatives Hybrid-Pressschweißverfahren zeichnet sich durch eine Reihe von Vorteilen aus, welche es für die Kombination artfremder metallischer Werkstoffe mit deutlich unterschiedlichem Schmelzpunkt ermöglichen, qualitativ hochwertigere Verbunde zu realisieren. Die vorliegende Arbeit thematisiert experimentelle Untersuchungen der Auswirkungen des zusätzlich eingekoppelten Leistungsultraschalls auf das Prozessverhalten und die Bindungsmechanismen sowie daraus resultierender mechanischer Verbundeigenschaften beim ultraschallunterstützten Rührreibschweißen von Aluminium/Stahl-Verbunden. Im Anschluss an die Ermittlung geeigneter Parameter für das konventionelle Rührreibschweißen erfolgen grundlegende Betrachtungen des Einflusses des Leistungsultraschalls auf das Schwingungsverhalten, das thermische Verhalten und das insitu- Prozesskraftverhalten, aus denen bestmögliche Ultraschallparameter abgeleitet werden. Nachfolgende detaillierte, vergleichende Untersuchungen des konventionellen und des ultraschallunterstützten Rührreibschweißprozesses belegen unter anderem eine Reduktion der Dicke spröder, aluminiumreicher intermetallischer Phasen am Verbund-Interface des USE-FSW-Verbundes, was in einer Erhöhung der Zugfestigkeit und der Duktilität resultiert. / The ultrasound enhanced friction stir welding (USE-FSW) as an innovative hybrid solid state joining process is characterized by a number of advantages that enable the realization of higher quality joints for the combination of dissimilar, metallic material combinations with strongly differing melting points. The present work addresses the impact of the additional power ultra- sound transmission on the process behavior and the bonding mechanisms as well as resulting mechanical joint properties for the ultrasound enhanced friction stir welding of aluminum/steel joints via experimental investigations. Subsequent to the determination of suitable parameters for the conventional friction stir welding basic considerations of the power ultrasound influence on the oscillation behavior, the thermal behavior and the in-situ process force behavior take place for deriving a best possible set of ultrasound parameters. Moreover, the conventional and the ultrasound enhanced friction stir welding process are investigated comparatively in detail, proving a reduction in thickness for brittle, aluminum-rich intermetallic phases at the USE-FSW joint interface among other things, resulting in an improved tensile strength and ductility.

The current study focus on investigating a relationship between processing variables and microstructure evolution mechanism in 304L stainless steel subjected to hot torsion. The Gleeble 3800 with Mobile Torsion Unit (MTU) is utilized in the current study to conduct hot torsion test of 304L stainless steel. Samples are rotated at 1100℃ in the shear strain rate range of 0.02s-1 to 4.70s-1 and the shear strain range of 0.5 to 4. Orientation imaging microscopy (OIM) technique is used to collect and analyze the microstructure. At low strains (≤1) and strain rate (0.02s-1), average grain size remains relatively constant, but the lengths of DSs and LABs increase within grains. These are characteristics of the dynamic recovery (DRV). With increasing strain and strain rate, the lengths of DSs, LABs and HABs increase, accompanied by the decrease of average grain size. Subgrains with HAB segments are observed. These are characteristics of continuous dynamic recrystallization (CDRX). At strain rates greater than or equal to 0.94s-1, the fraction of deformation texture is about 3 times higher than that of rotated cube texture. The average grain size increases relative to that at a strain rate of 0.20s-1, accompanied by the increase of twin length per area. This indicates that grain growth take place after CDRX. Sigma phase is not observed in the current study due to the lack of static recrystallization (SRX) and the higher cooling rate.

Ceramic metal matrix composites (CMMCs) are materials generally created by mixing of hard ceramic particles in a metal matrix. They were expected to combine the ductility and toughness of the metal with the high strength and elastic modulus of the ceramic. MMCs have potential applications in automotive, aeronautical and aerospace industries. Hence, a simple and economical method for fabricating MMCs is an area of intense research. In MMCs, damage evolution starts preferentially at particle matrix interface or at particle clusters in the matrix. This is due to the different physical and mechanical properties of the particle and matrix. Higher local particle volume content leads to higher stress triaxiality making it a preferential site for damage nucleation. Problems with lowering of ductility, fatigue, fracture and impact resistance, agglomeration of ceramic phase and issues related to the predictability of properties of MMCs have been the major issues that have limited their use. In order to overcome some of these shortcomings, the use of nano particles has been attracting increasing attention. The reason is their capability in improving the mechanical and physical properties of traditional MMCs. The dispersion of a nanoscale ceramic phase is needed in order to overcome the problems related to fatigue, fracture toughness, and creep behaviour at high temperatures. However, manufacturing costs, preparation of nano composites and environmental concerns have to be addressed. Agglomeration of nano particles, when produced by the melt stir casting route, the primary route to produce MMCs, is a serious issue that limits the use of nano-particles to produce MMCs with good properties. To avoid agglomeration of the ceramic phase MMCs/nano MMCs have been produced through the powder metallurgy route. Agglomeration is avoided as this is a solid state process. Secondary processing, such as extrusion and rolling are often needed to fully consolidate materials produced in this manner. A high extrusion ratio is often required to get MMCs without porosity. A new method of making nano-ceramic MMC using a polymer derived ceramics (PDC) has been reported. A polymer derived ceramic is a material that converts itself into a ceramic when heated above a particular temperature. In the PDC method a polymer precursor is dispersed in the metal and then converted in-situ to a ceramic phase. A feature of this process is that all the constituents of the ceramic phase are built into the organic molecules of the precursor (e.g., polysilazanes contain silicon, carbon, and nitrogen); therefore, a reaction between the polymer and the host metal or air is not required to produce the ceramic phase. The polymer can be introduced through casting or powder metallurgy route. In the casting route, the polymer powder is directly added to molten metal and pyrolyzed in-situ to create castings of metal-matrix composites. These composites have shown better properties at elevated temperatures but the problem of agglomeration of particles due to Van der Waal's forces and porosity still remains. In the powder method, the organic precursor was milled with copper powder and then plasma sprayed to produce a metal matrix composite. It is reported that these composites retains its mechanical strength close to the melting point of the copper. However, getting a nano sized distribution is difficult through this route as the plasma spray route is a melting and solidification method. Solid state processing by powder metallurgy is possibly a better method to produce well dispersed nano-MMCs. However, powder metallurgy routes are much more expensive and only parts of limited sizes can be produced by this method. Another solid state process Friction Stir Processing (FSP) has successfully evolved as an alternative technique to fabricating metal matrix composites. FSP is based on the principles of Friction Stir Welding (FSW). In FSW, a rotating tool with a pin and a shoulder is inserted into the material to be joined, and traversed along the line of the joint. The friction between the tool and the work piece result in localized heating that softens and plasticizes the material. During production of MMCs using FSP method, the material undergoes intense plastic deformation resulting in mixing of ceramic particles and the metal. FSP also results in significant grain refinement of the metal and has also been used to homogenize the microstructure. FSP technology has also been used to fabricate surface/bulk composites of Al-SiC, friction stir surfacing of cast aluminum silicon alloy with boron carbide and molybdenum disulphide powders and to produce ultra-fine grained Cu-SiC composites. A major problem in the FSP of MMCs is severe tool wear that results from abrasion with hard ceramic particles. The progressive wear of the tool has been reported to increase the likelihood of void or defect development. This change in geometry has been reported in the friction stir welding of several MMCs. The problems concerning the tool life has become a serious issue in the application of FSP for producing MMCs. In the present work the advantages of the PDC method and FSP have been combined to produce polymer derived nano ceramic MMCs. This method mainly consists of three steps. In the first step, a polymer, which pyrolysis to form a PDC at temperatures lower than the melting point of the metal, is dispersed in the metal by FSP. This step is different from the melt route where the PDC forms at temperatures above the melting point of the metal. In the second step, external pyrolysis of the polymer dispersed material is carried out. Since this is a solid state process at stresses much higher than the shear or fracture of the polymer is expected to get evenly and finely distribution in the metal. This is done by heating the polymer dispersed material to a temperature above the pyrolysation temperature of the ceramic but lower than the melting point of the metal matrix. It should be mentioned that some pyrolysis of the polymer is possible during the FSP process itself. In the third step FSP is carried out on the pyrolised material for removing porosity that would form due to gas evolution during pyrolysis and to get a more uniform dispersion of polymer derived ceramic particles in the matrix. This method will produce nano-scale metal matrix composites with a relatively high volume fraction of the ceramic phase. This method can be extended to big sheets or a particular region in a sheet with no or low wear of tools. The material selected for the present study were pure Copper (99.9%) and Nickel Aluminum Bronze (NAB) copper alloy. The polymer precursor was poly (urea methyl vinyl) silazane, which is available commercially as CERASET. The polymer consists of silicon, carbon, nitrogen, oxygen and hydrogen atoms. The liquid precursor was thermally cross-linked into a rigid polymer, which was milled into a powder. This powder, having angular shaped particles of an average size of 10 µm, was used as the reinforcement. The polysilazanes convert into a highly refractory and amorphous ceramic upon pyrolysis and is known as polymer-derived silicon carbonitride which consists principally of silicon, carbon and nitrogen. The in-situ process is feasible because copper melts above the temperature at which the organic phase begins to pyrolise. The polysilazanes pyrolise in the temperature range of 973 to 1273 K, which lie below the melting temperature of copper, 1356K.The precursor has a density of approximately 1 gcm-3 in the organic phase and approximately 2 gcm-3 in the ceramic state. In the present work, we seek to introduce approximately 20 vol% of the ceramic phase into copper. The microstructure and mechanical properties of the developed copper-based in-situ polymer derived nano MMCs have been characterized in detail to understand the distribution of particles. The microstructure of the as received, processed as well as the FSP composite material was characterized using Optical Microscope (OM), Scanning Electron Microscope (SEM), Electron Probe Micro Analyzer (EPMA) and Transmission Electron Microscope (TEM). OM and SEM microstructural observations show that PDC particles are distributed uniformly with a bimodal (submicron+micron) distribution. In addition, TEM micrographs reveal the formation of very fine PDC particles of diameter 10-30 nm. X-ray diffraction and Thermo-gravimetric analysis confirms the presence of ceramic phase (Si3N4/SiC) in the matrix. Significant improvement in mechanical properties of the FSP PD-MMCs has been observed. This in-situ formed Cu/PDC composites show five times increase in micro-hardness (260Hv - 2.5GPa) compared to processed copper base metal and in-situ NAB/PDC composite shows two times increase in micro-hardness (325Hv- 3.2GPa) compared to NAB matrix. The Cu-PDC composites exhibited better tensile strength at room temperature. In-situ formed Cu-PDC composite’s yield strength increased from 110MPa to 235MPa as compared to processed base metal, where as ultimate tensile strength increases from 246MPa to 312MPa compared to processed base metal at room temperature. This strengthening could be attributed to the presence of in-situ formed hard phases and the concomitant changes in the microstructure of the matrix material such as reduction in grain size and contribution from Orowan strengthening. In the present work, we have observed tool wear by observing tool after each FSP pass and apart from producing a significantly harder material with higher elastic modulus, possibly for the first time, the issue of tool wear has been overcome. This is due to the fact that the composite is made by the polymer route and that the ceramic fractures easily till it reaches the nano-size. Wear studies of this composite was carried out in a pin-on-disc machine by sliding a pin made from the composite against an alumina disc. The wear rate of the FSP PD-MMC composites increased from 1.63×10-5 to 5.72×10-6 mm3/Nm. Improved wear resistance could be attributed to the presence of the in-situ formed hard nano-phase.

Le travail présenté dans cette thèse concerne la modélisation et la commande robuste en force de robots manipulateurs industriels à articulations flexibles utilisés pour le procédé FSW. Afin de réduire les temps de calcul et l'occupation de la mémoire, une approche basée sur la méthode par intervalle est proposée en vue de la simplification des modèles dynamiques des robots industriels, et contribue à identifier les paramètres d'inertie qui sont négligeables. Des études de cas sur trois types de trajectoires de test et l’analyse des couples moteurs ont démontré l'efficacité et les bonnes performances de la méthode de simplification. Ensuite, la modélisation dynamique et l'identification des paramètres du procédé FSW ont été effectuées. Les paramètres des modèles linéaires et non-linéaires de forces axiales sont identifiés. Sur la base de la modélisation du procédé FSW qui considère simultanément la cinématique du système complet, le modèle de déplacement du robot rigide, les flexibilités des articulations et le modèle dynamique de la force axiale, un contrôleur robuste en force est obtenu par la méthode de réglage fréquentielle. En outre, un simulateur du procédé FSW robotique est développé et les résultats de simulation montrent les bonnes performances du contrôleur en force. L'oscillation de la force axiale dans le procédé FSW peut être simulée en utilisant un modèle de perturbation de la position verticale de référence. / The work presented in this thesis focuses on the modeling and robust force control of flexible joints industrial robot manipulators used for FSW process. In order to reduce computation time and memory occupation, a novel interval-based approach for dynamic model simplification of industrial robots is proposed, which applies to arbitrary trajectories of whole robot workspace and contributes to obtaining negligible inertia parameters. Cases studies have been carried out on three kinds of test trajectories and torques analysis of robot dynamic equation, demonstrating the effectiveness and good performance of the simplification method. Then, the dynamic modeling and identification of robotic FSW process is performed, and the parameters of linear and nonlinear dynamic axial force process models are identified by using the plunge depth and its derivative. On the basis of the modeling of robotic FSW process which simultaneously considers the complete kinematics, the rigid robot displacement model, the joint flexibility and the dynamic axial force process model, a robust force controller can be obtained by using the frequency response approach. Besides, a simulator of robotic FSW process is developed and simulation results show good performance of the force controller. The oscillation of axial force in FSW process can be simulated when a disturbance model of initial vertical reference position is proposed and used in the simulation.