The first part of the thesis discuss general characterization of heterogeneous processes in silicates. This part is focused on kinetics of heterogeneous processes and mathematical description of reactions time behavior. The other part describes important technologies in silicate industry such as sintering, solid matter decomposition, transition modification, etc. Another chapter deals mineralogy, structure and properties of eminent silicate raw materials. Emphases is given to characterization of clay minerals and their utilising. The experimental part handle the analytic techniques used for investigation of thermal decompostion, dehydroxylation, crystalization of Al-Si spinel phase and sintering process of washed kaolin Sedlec Ia from the region Carlsbad (Czech Republic). Concluding chapter reports on results of experimental work.

La mise en forme à froid des alliages d’aluminium peut être limitée par les transferts de matière sur la surface des outillages pouvant mener au grippage. L’objectif de ce travail de thèse est de contribuer à une meilleure compréhension de ces mécanismes pour permettre à terme d’optimiser les procédés de formage d’un alliage Al-Mg-Si. Une approche couplée expérimentale et numérique est développée afin d’alimenter une base de données d’indicateurs de dégradations des surfaces. L’approche expérimentale développée au cours de ces travaux repose sur l’utilisation de l’essai de compression-translation. Ce dispositif permet de reproduire une large gamme de conditions de contact rencontrées en mise en forme à froid. Une méthode d’analyse des surfaces reposant sur des mesures par profilométrie optique et des analyses au microscope électronique à balayage est développée afin d’évaluer le volume de matière adhérée sur les outils de chaque configuration d’essai. Le comportement rhéologique de l’alliage Al-Mg-Si est caractérisé à l’aide du simulateur thermomécanique GLEEBLE 3500 sur la gamme de températures de 298 à 423 K et à deux vitesses de déformation de 0,1 et 1 s-1. Un modèle de comportement physique reposant sur l’analyse du taux d’écrouissage et l’utilisation du modèle de la contrainte mécanique seuil est développé puis implémenté dans un logiciel éléments finis. Un modèle numérique de l’essai de caractérisation tribologique est développé. Il s’agit d’une analyse thermomécanique utilisant la formulation arbitrairement lagrangienne-eulérienne. Les données locales telles que la pression de contact et la vitesse de glissement calculées par ce modèle permettent de mieux comprendre les mécanismes de collage observés expérimentalement. Enfin, un programme de traitement des résultats numériques est développé afin de réaliser les modifications géométriques de la surface de l’outil en fonction du dépôt relevé expérimentalement. Un modèle d’usure basé sur le travail des forces de frottement est identifié. Ce dernier est un bon indicateur de la tendance au collage et permet une première approximation de ce mécanisme. / Cold forming of aluminium alloys can be limited by a severe material transfer to the die surfaces, compromising the process viability. The purpose of this research work is to contribute to a broader understanding of the galling mechanisms which would further allow the optimisation of the forming processes of an Al-Mg-Si alloy. A methodology combining experimental and numerical approaches is introduced in order to build up a database of surface degradations indicators. The experimental approach is carried out by means of upsetting-sliding tests which reproduce a wide range of contact conditions experienced at the tool/workpiece interface during cold forming operations. To evaluate the amounts of adhered material on the tools of each test configuration, surface topography acquisitions are performed by optical profilometry and coupled to scanning electron microscope analyses. Axisymmetric compression tests are carried out by means of the GLEEBLE 3500 thermomechanical simulator to determine the deformation behaviour of the Al-Mg-Si alloy at high strains, in the temperature range of 298 to 423 K and strain rates of 0.1 and 1 s¡1. A constitutive model based on both the Mechanical Threshold Stress model and the analysis of the work-hardening rate is proposed and then implemented in a finite element code. A finite element simulation of the upsetting-sliding test, which is a thermomechanical analysis using the arbitrary lagrangian-eulerian formulation, is introduced. The local contact variables such as the contact pressure and the sliding velocity are evaluated through this simulation and allow a better understanding of the galling mechanisms observed experimentally. Finally, a post-processing program, which analyses the results of the finite element simulation and updates the tool shape according to the amount of adhered material determined experimentally, is developed. A wear model based on the friction work is introduced. This model is a good indicator of the galling tendency and allows a first approximation of this mechanism.

Les raccords et connexions de caténaires ont un rôle important dans l’intégrité électrique et mécanique des caténaires. Ces pièces sont pour la plupart constituées d’un alliage de cuivre Cu-Ni-Si mis en forme par forgeage à chaud. Dans un contexte de fiabilisation du réseau ferroviaire, l’amélioration de leurs performances et de leurs procédés de fabrication est recherchée. Ces travaux se concentrent sur l’étape de mise en forme de ces pièces, et ont pour objectif de mieux comprendre les couplages matériaux-procédés des alliages Cu-Ni-Si.Une campagne expérimentale de compression est menée. Elle permet de développer un modèle rhéologique à base physique décrivant le comportement d’un alliage Cu-Ni-Si dans les gammes de température 800 - 950 °C et de vitesse de déformation 0.1 - 10 s−1. Il tient compte des phénomènes d’adoucissement par restauration et recristallisation dynamiques. Le modèle ainsi créé est ensuite implémenté dans un logiciel éléments finis.Un nouvel essai de formabilité est proposé. Il permet de reproduire les sollicitations mécaniques rencontrées lors d’un procédé de forgeage et vise à déterminer les conditions limites de formabilité d’un matériau. La mise en forme d’une pièce de référence est étudiée par le biais de cet essai. Sa caractérisation précise en matière de champ de déformations et de contraintes permet d’identifier les paramètres expérimentaux. Les résultats identifient une température limite de forgeage en-deçà de laquelle des fissures sont prédites dans la pièce. / Contact wire splices play a leading role in the electric and mechanical integrity of the catenary systems. Most of these parts are made of Cu-Ni-Si alloys and manufactured by a hot forging process. With the aim of increasing the reliability of the railway network, the improvement of their performances and their manufacturing processes is sought. This work is focused on the forming stage of these parts and aims to give a better understanding of the materials-processes couplings for the Cu-Ni-Si alloys.An experimental campaign including compression tests is conducted. It allows the development of a physically-based model to describe the rheological behavior of a Cu-Ni-Si alloy deformed in the temperature range between 800 °C and 950 °C, at strain rates in the range of 0.1 - 10 s−1. It takes into account the work-softening implied by dynamic recovery and dynamic recrystallization. The model thus created is then implemented in a finite element software.A new workability test is proposed. Its purpose is to reproduce the mechanical conditions encountered in a forming process and to determine the critical conditions of workability related to a material. The forging process of a reference part is studied by means of this test. An accurate characterization of the process in terms of strain magnitude and stress field allows the identification of the experimental parameters. The results lead to the identification of a limit temperature of workability below which fractures are predicted in the part.

The magnetic Fe–6.5 wt% Si powder was produced by gas atomization and its microstructure was also investigated. The secondary dendritic arm spacing (SDAS) is related to the droplet size, λ = 0.29 · D⁰·⁵, and the numerical solidification model was applied to the system, giving rise to the correlation of microstructure to the solidification process of the droplet. It is found that the solid fraction at the end of recalescence is strongly dependent on the undercooling achieved before nucleation; the chances for the smaller droplets to form the grain-refined microstructures are less than the larger ones. Furthermore, the SDAS is strongly influenced by the cooling rate of post-recalescence solidification, and the relationship can be expressed as follows, λ = 74.2 · (T)⁻⁰·³⁴⁷. Then, the growth of the SDAS is driven by the solute diffusion of the interdendritic liquids, leading to a coarsening phenomenon, shown in a cubic root law of local solidification time, λ = 10.73 · (tf)⁰·²⁹⁶.

The present thesis investigates the grain refinement in solidifying Al-7wt%Si hypoeutectic alloy driven by electric currents. The grain size reduction in alloys generated by electric currents during the solidification has been intensively investigated. However, since various effects of electric currents have the potential to generate the finer equiaxed grains, it is still argued which effect plays the key role in the grain refinement process. In addition, the knowledge about the grain refinement mechanism under the application of electric currents remains fragmentary and inconsistent. Hence, the research objectives of the present thesis focus on the role of electric current effects and the grain refinement mechanism under the application of electric currents. Chapter 1 presents an introduction with respect to the subject of grain refinement in alloys driven by electric current during the solidification process in particular, including the research objectives; the research motivation; a brief review about the research history; a short introduction on the electric currents effects and a review relevant to the research status of grain refinement mechanism. Chapter 2 gives a description of research methods. This chapter shows the employed experiment materials, experimental setup, experimental procedure, the analysis methods of solidified samples, and numerical method, respectively. Chapter 3 focuses on the role of electric current effects in the grain refinement process. A series of solidification experiments are performed under various values of effective electric currents for both, electric current pulse and direct current. The corresponding temperature measurements and flow measurements are carried out with the increase of effective electric current intensity. Meanwhile, numerical simulations are conducted to present the details of the flow structure and the distribution of electric current density and electromagnetic force. Finally, the role of electric current effects is discussed to find the key effect in the grain refinement driven by electric currents. Chapter 4 investigates the grain refinement mechanism driven by electric currents. This chapter mainly focuses on the origin of finer equiaxed grain for grain refinement under the application of electric current on account of the importance of the origin for understanding the grain refinement mechanism. A series of solidification experiments are carried out in Al-7wt%Si alloy and in high purity aluminum. The main origin of equiaxed grain for grain refinement is concluded based on the experiment results. Chapter 5 presents three further investigations based on the achieved knowledge in chapter 3 and 4 about the role of electric current effects and the grain refinement mechanism. According to the insight into the key electric current effect for the grain refinement shown in chapter 3, this chapter presents a potential approach to promote the grain refinement. In addition, the solute distribution under the influence of electric current is examined based on the knowledge about the electric current effects. Moreover, the grain refinement mechanism under application of travelling magnetic field is investigated by performing a series of solidification experiments to compare with the experiments about the grain refinement mechanism driven by electric currents shown in chapter 4. Chapter 6 summarizes the main conclusions from the presented work.:Abstract VII Contents IX List of figures XI List of tables XVII 1. Introduction 1 1.1 Research objectives 1 1.2 Research motivation 2 1.3 Research history 5 1.4 Electric currents effects 9 1.4.1 Some fundamentals 10 1.4.2 Role of electric currents effects in grain refinement 12 1.5 Grain refinement mechanism 13 1.5.1 Nucleation theory 13 1.5.2 Equiaxed grain formation without the application of external fields 18 1.5.3 Grain refinement mechanism under the application of electric currents 23 1.5.4 Grain refinement mechanism under the application of magnetic field 29 2. Research methods 31 2.1 Introduction 31 2.2 Experimental materials 31 2.2.1 Solidification 31 2.2.2 Similarity of GaInSn liquid metal and Al-Si melt 32 2.3 Experimental setup 33 2.3.1 Solidification 33 2.3.2 Flow measurements 35 2.3.3 External energy fields 36 2.4 Experimental procedure 38 2.4.1 Solidification 38 2.4.2 Flow measurements 39 2.5 Metallography 39 2.6 Numerical method 41 2.6.1 Numerical model 41 2.6.2 Numerical domain and boundary conditions 42 3. Role of electric currents effects in the grain refinement 45 3.1 Introduction 45 3.2 Experimental parameter 45 3.3 Results 46 3.3.1 Solidified structure 46 3.3.2 Forced melt flow 50 3.3.3 Temperature distribution 58 3.4 Discussion 61 3.5 Conclusions 67 4. Grain refinement mechanism driven by electric currents 69 4.1 Introduction 69 4.2 Experimental parameter 69 4.3 Results 73 4.3.1 Solidified structure of Al-Si alloy 73 4.3.2 Cooling curves of Al-Si alloy 77 4.3.3 Solidified structure of high purity aluminum 78 4.4 Discussion 80 4.5 Conclusions 83 5. Supplemental investigations 85 5.1 A potential approach to improve the grain refinement 85 5.1.1 Introduction 85 5.1.2 Experimental parameter 86 5.1.3 Results and discussion 87 5.2 Macrosegregation formation 90 5.2.1 Introduction 90 5.2.2 Experimental parameter 91 5.2.3 Results and discussion 92 5.3 Grain refinement driven by TMF 97 5.3.1 Introduction 97 5.3.2 Experimental parameter 97 5.3.3 Results and discussion 98 5.4 Conclusions 102 6. Summary 103 Bibliography 105

Nature of Science (NOS) har varit i utbildares och forskares blickfång länge. Elevers kunskaper är av intresse att analysera eftersom det kan bidra till en utveckling av lärares undervisning och förståelse av lärandeprocesser i no-ämnena. Syftet med studien var att analysera hur elever i årskurs 4 ser på vad som är en vetenskaplig undersökning och ett experiment. Den data som används i studien består av redan insamlade frågeformulär från 2019. Studiens data analyseras genom en innehållsanalys. Resultatet visar att elevers kunskaper om undersökningar och experiment är varierande. Eleverna ger exempel på att undersökningar kan innefatta att antingen titta först och sedan ställa en fråga eller tvärtom och att ett experiment kan innebära att blanda eller att prova sig fram. Lärare kan utveckla sin undervisning genom att exempelvis använda elevnära innehåll som eleven känner igen och kan relatera till eller använda modeller och metoder för att visa på systematik och underbyggda slutsatser för att bidra till en högre förståelse om naturvetenskaplig kunskap hos eleverna.

Pressgjutna Al-Si komponenter förekommer mer och mer i förbränningsmotorer med syfte att reducera vikt och förbättra hållbarhet. Ett problem vid pressgjutning, en process kännetecknad av kostnadseffektivitet vid massproduktion, är porositetsbildning vilket kan resultera i läckage, strukturell svaghet och försämrad hållbarhet och livslängd för tillverkade komponenter. Då porer oftast bildas internt försvåras dessutom identifiering av potentiellt trasiga komponenter. Det är därför av vikt att finna parameterinställningar i pressgjutningsprocessen vilka konsekvent minimerar porositetsbildning. Ett företag som drabbas av återkommande porositets-relaterade defekter är Husqvarna Group. De använder vakuumassisterad pressgjutning för att, bland annat, producera motorcylindrar av Al-Si. Kassationsgraden, specifikt hänförbar till porositet, för en cylindermodell har under de senaste tre åren fördubblats vilket har resulterat i slöseri av produktionstid och kvalitetsbristkostnader. Vakuumassisterad pressgjutning kan beskrivas stegvis: (1) smält metall hälls i en cylindrisk fyllkammare, (2) en skottkolv trycker smältan mot ett mindre inlopp i låg hastighet för att undvika turbulens, samtidigt som vakuum ansätts i fyllkammare och gjutverktyg, (3) skottkolvshastigheten ökar markant vid en förinställd omslagspunkt, vilket spray-fyller gjutverktyget, och (4) högt tryck ansätts för att eftermata smälta till gjutverktyget när solidifiering sker. Syftet med detta examensarbete har varit att undersöka om och hur diverse parametrar, hänförbara till de nämnda processtegen, påverkar porositetsbildning i en industriell produkt. Därefter applicerades den erhållna processförståelsen för att identifera parametrar kritiska för porositetsbildning och slutligen rekommendera parameterinställningar som konsekvent minimerar porositetsgraden. Det experimentella upplägget bestod av två steg varav det första ämnade undersöka, via simulering, vilka av 6 parametrar som påverkade porositetsgraden utifrån en reducerad tvånivåers försöksdesign. Det andra steget var ett verkligt experiment i produktionsmiljö där de tre identiferade parametrarna från screening-experimentet varierades enligt en central-composite design. Analysen av experimenten resulterade i parameterinställningar som förväntas reducera porositetsgraden med över 70%. En lägre porositetsgrad kommer troligen reducera kassationsgraden av den undersökta cylindermodellen, vilket hade resulterat i finansiell besparing och effektivare produktion. I ett industriellt kontext bidrar detta exjobb huvudsakligen med en systematisk kvalitetsförbättrande metod för pressgjutna komponenter baserad i såväl simulerad som verklig miljö. / Pressure die casted Al-Si components are increasingly found inside internal combustion engines, resulting in weight reduction and increased durability. Characteristic to die casting, commonly associated with cost-effective mass production, is the formation of pores which, if unnoticed, can cause leakage, structural deficiencies, and thus reduced durability and life-length of components. Pores commonly appear internally, making identification of faulty components difficult. Therefore, finding parameter settings in the die casting process that consistently minimizes the formation of pores is of importance. A company struggling with porosity-related defects is Husqvarna Group, currently using vacuum-assisted die casting to produce engine cylinders of Al-Si. Scrap-rate, specifically related to porosity, of a particular cylinder model has doubled in the last three years, causing waste of both precious production time and higher quality deficiency costs. A vacuum-assisted die casting process consists of several steps: (1) liquid Al-Si is poured into a cylindrical shot sleeve, (2) a plunger is moved towards a small gate, leading to the die cavity, at low velocity as to not cause turbulence, whilst vacuum is applied throughout the cavity and shot sleeve, (3) plunger velocity is increased substantially at a predetermined switch point, resulting in a spray-filling of the die cavity, and (4) high pressure is applied to continue the feed of molten metal into the cavity as solidification occurs. The purpose of the thesis has been to investigate if and how various parameters, related to the aforementioned four steps of the die casting process, impact the porosity amount in an industrial product. The acquired process knowledge was then applied to identify parameters affecting porosity and recommend settings that consistently minimize the porosity amount. The experimental procedure consisted of two steps: firstly, a screening experiment of six process parameters was made by simulating the die casting process according to a fractional factorial design. Secondly, a real-world experiment was conducted following a central-composite design by varying the three most impactful parameters from the screening experiment.   Analysis of the experiments resulted in a selection of parameter settings, anticipated to reduce porosity by over 70%. A lower porosity amount will most likely reduce the scrap rate of the cylinder model, resulting in substantial savings and higher production efficiency. For practitioners, the main contribution of this thesis is a method of systematic quality-improvement to die-casted components by a combination of simulation experiments and real-world tests.

Nickel superalloys are used for high-temperature application in energetic and aerospace industry. They are exposed to aggressive environment at high temperatures with the interactions between fatigue and creep processes, high-temperature oxidation, corrosion and erosion. Lifetime extension of such strained parts while increasing the performance of particular machine is possible by applying protective surface coatings. The subject of this work is to investigate the fatigue failure mechanisms of superalloy Inconel 713LC at 800 °C and to compare these mechanisms between material with a protective coating based on Al-Si and material without coating. The location of initiation fatigue cracks, their propagation and the fatigue crack propagation rate in some areas were analyzed by optical microscopy, scanning electron microscopy and confocal laser scanning microscopy. Based on previous research it was found that the application of the coating AlSi has a positive effect on lifetime of alloy Inconel 713LC. These results were confirmed and estimated in the diploma thesis.

Selective laser melting (SLM) is an additive manufacturing technology. In this thesis, a heat-treatable Al-3.5Cu-1.5Mg-1Si alloy and related materials (composites and hybrid materials) have been successfully fabricated by selective laser melting and characterized in terms of densification, microstructure, heat treatment, mechanical properties as well as tribological and corrosion behavior. Firstly, the fully dense SLM Al-Cu-Mg-Si alloy was fabricated by SLM successfully. The alloy shows a higher yield strength than SLM Al-12Si alloy, and lower wear resistance and corrosion rate than commercial 2024 alloy before and after T6 heat treatment. Secondly, with the aim of designing new alloy compositions and to examine the phases and microstructures of SLM Al-Cu alloys and to correlate their microstructures with the observed mechanical properties, Al-xCu (x = 4.5, 6, 20, 33 and 40 wt. %) alloys have been synthesized in-situ by SLM from mixtures of Al-4.5Cu and Cu powders. The results indicate that the insufficient Cu solute diffusion during the layer-by-layer processing results in an inhomogeneous microstructure around the introduced Cu powders. With increasing Cu content, the Al2Cu phase in the alloys increases improving the strength of the material. These results show that powder mixtures can be used for the synthesis of SLM composites but the reaction between the matrix and the second-phase should be considered carefully. Thirdly, the TiB2/Al-Cu-Mg-Si composite was also designed and fabricated successfully by SLM and it shows a higher strength than the unreinforced SLM alloy before and after T6 heat treatment. Finally, an Al-12Si/Al-3.5Cu-1.5Mg-1Si hybrid with a good interface was fabricated successfully. This hybrid alloy shows a good yield strength and elongation at room temperature, indicating an effective potential of selective laser melting in the field of hybrid manufacturing.

Intermediate band (IB) materials have attracted considerable research interest since they can dramatically enhance the near infrared light absorption and lead to applications in the fields of so-called intermediate band solar cells or infrared photodetectors. Hyperdoping Si with deep level impurities is one of the most effective approaches to form an IB inside Si. In this thesis, titanium (Ti) or chalcogen doped Si with concentrations far exceeding the Mott transition limits (~ 5×10^19 cm-3 for Ti) are fabricated by ion implantation followed by pulsed laser annealing (PLA) or flash lamp annealing (FLA). The structural and electrical properties of the implanted layer are investigated by channeling Rutherford backscattering spectrometry (cRBS) and Hall measurements. For Si supersaturated with Ti, it is shown that Ti-implanted Si after liquid phase epitaxy shows cellular breakdown at high doping concentrations during the rapid solidification, preventing Ti incorporation into Si matrix. However, the out-diffusion and the cellular breakdown can be effectively suppressed by solid phase epitaxy during FLA, leading to a much higher Ti incorporation. In addition, the formed microstructure of cellular breakdown also complicates the interpretation of the electrical properties. After FLA, the samples remain insulating even with the highest Ti implantation fluence, whereas the sheet resistance decreases with increasing Ti concentration after PLA. According to the results from conductive atomic force microscopy (C-AFM), the decrease of the sheet resistance after PLA is attributed to the percolation of Ti-rich cellular walls, but not to the insulator-to-metal transition due to Ti-doping. Se-hyperdoped Si samples with different Se concentrations are fabricated by ion implantation followed by FLA. The study of the structural properties of the implanted layer reveals that most Se atoms are located at substitutional lattice sites. Temperature-dependent sheet resistance shows that the insulator-to-metal transition occurs at a Se peak concentration of around 6.3 × 10^20 cm-3, proving the formation of an IB in host semiconductors. The correlation between the structural and electrical properties under different annealing processes is also investigated. The results indicate that the degrees of crystalline lattice recovery of the implanted layers and the Se substitutional fraction depend on pulse duration and energy density of the flash. The sample annealed at short pulse durations (1.3 ms) shows better conductivity than long pulse durations (20 ms). The electrical properties of the hyperdoped layers can be well-correlated to the structural properties resulting from different annealing processes.:Chapter 1 Introduction 1 1.1 Shallow and Deep level impurities in semiconductors 1 1.2 Challenges for hyperdoping semiconductors with deep level Impurities 2 1.3 Solid vs. liquid phase epitaxy 5 1.4 Previous work 7 1.4.1 Transition metal in Si 7 1.4.2 Chalcogens in Si 10 1.5 The organization of this thesis 15 Chapter 2 Experimental methods 18 2.1 Ion implantation 18 2.1.1 Basic principle of ion implantation 18 2.1.2 Ion implantation equipment 19 2.1.3 Energy loss 20 2.2 Pulsed laser annealing (PLA) 23 2.3 Flash lamp annealing (FLA) 24 2.4 Rutherford backscattering and channeling spectrometry (RBS/C) 27 2.4.1 Basic principles 27 2.4.2 Analysis of the elements in the target 28 2.4.3 Channeling and RBS/C 29 2.4.4 Analysis of the impurity lattice location 31 2.5 Hall measurements 31 2.5.1 Sample preparation 32 2.5.2 Resistivity 32 2.5.3 Hall measurements 33 Chapter 3 Suppressing the cellular breakdown in silicon supersaturated with titanium 34 3.1 Introduction 34 3.2 Experimental 35 3.3 Results 36 3.4 Conclusions 42 Chapter 4 Titanium-implanted silicon: does the insulator-to-metal transition really happen? 44 4.1 Introduction 44 4.2 Experimental section 45 4.3 Results 47 4.3.1 Recrystallization of Ti-implanted Si 47 4.3.2 Lattice location of Ti impurities 48 4.3.3 Electrical conduction 50 4.3.4 Surface morphology 52 4.3.5 Spatially resolved conduction 53 4.4 Discussion 55 4.5 Conclusion 56 Chapter 5 Realizing the insulator-to-metal transition in Se hyperdoped Si via non-equilibrium material processing 57 5.1 Introduction 57 5.2 Experimental 59 5.3 Results 60 5.4 Conclusions 65 Chapter 6 Structural and electrical properties of Se-hyperdoped Si via ion implantation and flash lamp annealing 67 6.1 Introduction 67 6.2 Experimental 68 6.3 Results 69 6.4 Conclusions 76 Chapter 7 Summary and outlook 78 7.1 Summary 78 7.2 Outlook 81 References 83 Publications 89