Le procédé de fusion sélective par laser est un des nombreux procédés de fabrication additive qui permet la production rapide de pièces à partir d'un fichier CAO (conception assistée par ordinateur) et de lits de poudre. Après une description du fonctionnement du procédé par l'intermédiaire de ses paramètres opératoires, le manuscrit décrit les travaux entrepris pour l'élaboration de pièces en Inconel 625. Ce superalliage à base nickel a fait l'objet d'une étude paramétrique pour déterminer un jeu de paramètre optimal permettant de produire des pièces saines. Cette étude est basée sur des considérations énergétiques qui visent à maximiser le rendement de conversion de l'énergie électromagnétique en énergie thermique tout en assurant la cohésion entre couches. Des essais de traction valident la stratégie employée au niveau de l'étude paramétrique. Un second alliage est étudié, l'Inconel 738 qui est un superalliage renforcé par la précipitation d'une phase γ'-Ni3(Al,Ti). Les travaux entrepris ne concernent pas l'élaboration mais la caractérisation de l'alliage. Il est mis en évidence que celui-ci est dans un état hors de l'équilibre thermodynamique lorsque produit par fusion laser sélective. La précipitation de la phase durcissante n'est pas complète. Ce constat peut permettre d'éviter la fissuration de l'alliage pendant la fabrication en adaptant les paramètres opératoires, notamment au niveau du préchauffage. Une étude sur les traitements thermiques montre que la gamme appliquée traditionnellement à l'alliage coulé ne convient pas pour l'alliage élaboré par fusion sélective ; cette étude ouvre sur des alternatives. Enfin, ces travaux apportent quelques éléments de réponse quant à la pertinence énergétique du procédé. / The selective laser melting (SLM) process is one of the many additive manufacturing processes that allow to rapidly build a part from a computer-aided design (CAD) file and from a powder bed. The work described here deals with the different parameters related to the process, namely the building platform stepping and the laser radiation and its interaction with the metallic matter. The first Ni-based superalloy studied here is Inconel 625 which has been subjected to a parametric study with an energetic approach. It was all about finding the maximum in the conversion of electromagnetic energy into thermal energy. Tensile tests validate the use of the energetic strategy for this alloy. The second studied alloy is Inconel 738 which is hardened by fine γ'-Ni3(Al,Ti) precipitates. Microstructure observations and differential thermal analysis reveal that the γ' precipitation is not complete when the alloy is processed by SLM. This leads to give clues for crack-free processing by adjusting the parameters and especially the preheating feature. Different heat treatments on SLMed materials have been investigated. It appears that the standard procedure applied on cast alloy to reach proper microstructure for good mechanical properties is not adapted to the SLMed alloy. New standards must be defined to comply with the initial out of equilibrium state. Last but not least, the manuscript gives information regarding the energetic use of the process which should be compared with the will of environmental impact reduction policy called by the process.

This thesis aims to investigate the use of additive manufacturing (AM) as a novel manufacturing process for the production of milli-scale chemical reaction systems. Five well developed additive manufacturing techniques; stereolithography (SL), selective laser melting (SLM), fused deposition modelling (FDM), ultrasonic additive manufacture (UAM) and selective laser sintering (SLS) were used to manufacture a number of miniaturised flow devices which were tested using a range of organic and inorganic reactions. SL was used to manufacture a range of functioning milli-scale flow devices from Accura 60 photoresin, with both simple and complex internal channel networks. These devices were used to perform a range of organic and inorganic reactions, including aldehyde and ketone functional group interconversions. Conversion of products within these reactors, were shown to be comparable to commercially available milli-scale coil reactors. More complex designs, which allowed SL parts to be integrated to existing flow and analytical instrumentation, allowed us to develop an automated reaction analysis and optimisation platform. This platform allowed precise control over the reaction conditions, including flow rate, temperature and reagent composition. We also designed a simplex type reaction optimisation software package that could input data in the form of reaction conversions, peak intensities, and thermocouple data, and generate a new set of optimal reaction conditions. SL parts which incorporated embedded analytical components were also manufactured, which allowed us to perform inline reaction analysis as a feedback method for input into the optimisation platform. Stereolithography was shown to be a highly versatile manufacturing method for designing and producing these flow devices, however the process was shown to be still limited by the range of processable materials currently commercially available. SLM was also used to manufacture a number of functioning milli-scale flow devices from stainless steel and titanium, which had simplistic internal channel designs of diameters ranging from 1 to 3 mm. Again, SLM parts were manufactured which incorporated embedded analytical components, which could be integrated into an automated reaction platform. These devices, unlike parts produced via SL, could be attached to heating platforms to allow us to perform high temperature reactions. This control over the reaction temperature formed an essential part of the reaction optimisation platform. These parts were again used to perform a ketone functional group interconversion. Internal structures of these SLM parts were also visualised via micro computed tomography (μCT or microCT) scanning as well as optical microscopy. FDM was used throughout the project as an inexpensive method of prototyping parts which were to be manufactured via more expensive manufacturing processes. This prototyping allowed the optimisation of intricate design features, such as the manufacture of an inline spectroscopic flow cell for integration with a commercially available LC system. FDM was also proposed as a customisable approach to designing and manufacturing flow devices with embedded components, however the current limitations in build resolution and materials choices severely limited the use of FDM for this application. UAM was also proposed as a novel manufacturing process whereby the build process would allow discrete components to be embedded directly into a flow channel. This was demonstrated by embedding a type-k thermocouple across a 2 mm channel. The data from this thermocouple was monitored during a heated reaction, and used as a method of determining the exact reaction conditions the reaction medium was being exposed to. SLS was also proposed as a possible manufacturing method for milli-scale flow devices, however it proved difficult to remove un-sintered powder from parts with internal channel diameters as high as 5 mm. It was shown that this powder was forming a dense semi solid, due to the large degree of shrinkage upon cooling of the SLS parts, which was compressing the powder. More research into optimum processing conditions is required before SLS could be used for the production of intricate channel networks.

Les procédés additifs, auxquels appartient la fusion laser de poudres métalliques, ont la capacité de créer des structures à géométries complexes, avec la possibilité d'intégrer des formes creuses, par exemple des canaux de refroidissement assurant un contrôle thermique optimum. Ce procédé permet de fabriquer des pièces réelles à partir de poudres métalliques, par fusion du matériau, couche par couche, en accord avec le modèle CAO. Au cours du procédé, de nombreux cycles thermiques et d'importants gradients thermiques se produisent dans la pièce au cours de sa fabrication. Ces gradients de température induisent des déformations plastiques hétérogènes et de ce fait des contraintes résiduelles. Ces contraintes peuvent nuire à la qualité de la pièce obtenue, par exemple sa résistance mécanique. Ces travaux ont pour objectifs de proposer un modèle numérique, s’appuyant sur la méthode des éléments finis afin d'étudier l'apparition des contraintes résiduelles lors du procédé de fusion laser de poudres métalliques. Le logiciel multiphysique ABAQUS® a été utilisé pour effectuer les analyses thermiques et mécaniques. La technique « d'ajout et de suppression des éléments » a été utilisée afin de simuler la fusion et la solidification de la matière au cours du procédé. Les propriétés mécaniques dépendantes de la température de l'acier maraging, utilisé dans notre cas, ont été obtenues à l’aide d’essais expérimentaux de caractérisations et intégrées dans le modèle. Les calculs sont réalisés de manière découplée, dans un premier temps le calcul thermique est effectué, puis les résultats sont utilisés pour réaliser le calcul mécanique et finalement prédire les champs de contraintes. Dans le cadre de ce travail, une méthode originale s'appuyant sur la technique de mesure des contraintes résiduelles par enlèvement de couches successives a été mise au point pour mesurer ces contraintes en direct au cours du procédé. Les résultats renseignent sur le niveau et la distribution des contraintes dans la pièce créée et le support. Deux paramètres ont été testés afin d'étudier leur influence sur le niveau des contraintes résiduelles : le temps d’étalement de la poudre entre deux couches successives et la hauteur des couches. Le modèle numérique paramétrable permet d'analyser les effets de paramètres liés au procédé sur la répartition des contraintes résiduelles dans les pièces fabriquées. Les résultats montrent que la variation de l'épaisseur du support n'affecte pas la répartition des contraintes dans la pièce créée. Le préchauffage du support à une température de 800°C réduit les contraintes résiduelles L'étude de quelques trajectoires laser montre leurs influences sur la répartition des déformations plastiques cumulées ainsi que la hauteur des couches de poudres ou de la forme du support (embase, colonnes). / The Selective Laser Melting process, belonging to Additive processes , have the ability to create structures with complex geometries , with the possibility of including cavities, such as cooling channels providing optimum temperature control. This process enables the manufacture of three-dimensional parts from metal powders by melting the material , layer by layer, in agreement with the CAD model. In the process , high temperatures and thermal gradients cycles occur in the part during the process. These temperature gradients induce heterogeneous plastic strain and residual stresses. These residual stresses may affect the quality of the part obtained, for example the fatigue life. This work aims to propose a numerical model , based on the finite element method to study the appearance of residual stresses during laser melting process of metallic powders . The ABAQUS® Multiphysics software was used to perform the thermal and mechanical analyzes. The movement of the laser beam and the resolution of the thermal problem can predict the evolution of the temperature in the part and support. The "birth and death elements" technique was used to simulate the melting and solidification of the material during the process. Dependent mechanical properties of the temperature of the maraging steel used in this case were obtained using experimental testing and characterization and were established in the model. The calculations are decoupled : initially thermal calculation is performed and the results are used to perform mechanical calculations and finally predict the residual stress fields. In this work, a novel method based on the technique of measuring residual stresses by removing layers was developed to measure these stresses directly in the process. The results provide information on the level and distribution of stresses in the created part and support. Two parameters were tested to study their influence on the level of residual stress : time to spread the powder between two successive layers and layer height. The model is used to analyze the effects of process parameters related to the distribution of residual stresses in the manufactured parts. The results show that the variation of the thickness of the support does not affect the distribution of stresses in the part created. Preheating the substrate to a temperature of 800 °C reduces the residual stresses. The study of some laser strategies shows their influence on the distribution of plastic strain thus the height of the layers of powder or in the form of support (base, columns).

Das selektive Laserschmelzen (SLM) erlaubt komplexe Geometrien zu fertigen, die, z. B. in Form von integrierten Kühlkanälen, bei Werkzeugen von großer Bedeutung sind. Aktuell werden in der Industrie hauptsächlich Aluminium-, Stahl-, Titan-, Nickel- und Kobaltchromlegierungen mit SLM verarbeitet. Für die additive Fertigung sind Stähle interessant, die besondere Eigenschaften aufweisen. So wird für Konstruktionsbauteile größtenteils korrosionsbeständiger Stahl verwendet. Ein weiteres Anwendungsfeld ist die Herstellung von Werkzeugen. Die besonderen Ansprüche an die mechanischen Eigenschaften, die für Werkzeuge benötigt werden, erfüllen die Werkzeugstähle. Durch die Neigung zu Rissbildung und Verzug resultiert eine herausfordernde Verarbeitbarkeit im SLM-Prozess. Werkzeugstähle wurden bisher auf Grund dieser Herausforderungen selten mit SLM prozessiert. Es besteht daher ein großer Bedarf die Zusammenhänge zwischen dem Prozess, der Verarbeitbarkeit, dem entstehenden Gefüge und den resultierenden Eigenschaften aufzuklären. In dieser Arbeit werden die Mikrostruktur und die mechanischen Eigenschaften dreier hochfester Stahllegierungen, verarbeitet im SLM-Prozess, untersucht. Eine Legierungsentwicklung, speziell auf die Anforderungen des SLM-Prozesses zugeschnitten, ermöglicht, das volle Potenzial des SLM-Prozesses auszuschöpfen. Die Verarbeitbarkeit der neu entwickelten Legierung im SLM-Prozess konnte erfolgreich gegenüber den Ausgangslegierungen verbessert werden.

The thesis focuses on exploring the sub-grain structure in stainless steel 316L prepared by additive manufacturing (AM). Two powder-bed based AM methods are involved: selective laser melting (SLM) and electron beam melting (EBM). It is already known that AM 316L has heterogeneous property and hierarchy structure: micro-sized melt pools, micro-sized grains, nano-sized sub-grain structure and nano-sized inclusions. Yet, the relation among these structures and their influence on mechanical properties have not been clearly revealed so far. Melt pool boundaries having lower amount of sub-grain segregated network structures (Cellular structure) are weaker compared to the base material. Compared with cell boundaries, grain boundaries have less influence on strength but are still important for ductility. Cell boundaries strengthen the material without losing ductility as revealed by mechanical tests. Cellular structure can be continuous across the melt pool boundaries, low angle sub-grain boundaries, but not grain boundaries. Based on the above understanding, AM process parameters were adjusted to achieve customized mechanical properties. Comprehensive characterization were carried out to investigate the density, composition, microstructure, phase, magnetic permeability, tensile property, Charpy impact property, and fatigue property of both SLM and EBM SS316L at room temperature and at elevated temperatures (250°C and 400°C). In general, SLM SS316L has better strength while EBM SS316L has better ductility due to the different process conditions. Improved cell connection between melt pools were achieved by rotating 45° scanning direction between each layer compared to rotating 90°. Superior mechanical properties (yield strength 552 MPa and elongation 83%) were achieved in SLM SS316L fabricated with 20 µm layer thickness and tested in the building direction. Y2O3 added oxide dispersed strengthening steel (ODSS) were also prepared by SLM to further improve its performance at elevated temperatures. Slightly improved strength and ductility (yield strength 574 MPa and elongation 90%) were obtained on 0.3%Y2O3-ODSS with evenly dispersed nanoparticles (20 nm). The strength drops slightly  but ductility drops dramatically at elevated temperatures. Fractographic analysis results revealed that the coalescence of nano-voids is hindered at room temperature but not at elevated temperatures. The achieved promising properties in large AM specimens assure its potential application in nuclear fusion. For the first time, ITER first wall panel parts with complex inner pipe structure were successfully fabricated by both SLM and EBM which gives great confidence to application of AM in nuclear industry. / <p>At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 4: Manuscript. Paper 5: Manuscript.</p>

Residual stresses are one of the major challenges in additive manufacturing of metallic materials today. They are induced during manufacturing because of the rapid local heating and cooling and may cause distortions, cracking and delamination between layers. The magnitude of the residual stresses depends on factors such as manufacturing technology, material, part geometry, scanning strategy, process parameters, preheating temperature and density of the component. In the present work, the magnitudes of residual stresses and distortions in austenitic stainless steel 316L components manufactured by Selective Laser melting have been investigated. Four specimens with rectangular cross-sections where produced with different heights and wall thicknesses. The residual stresses were measured by two different methods, x-ray diffraction and Electronic Speckle Pattern Interferometry (ESPI) incremental hole drilling in order to see how well they correspond to each other. The results showed peaks of high tensile stresses in the building direction in all specimens. The magnitudes of stresses were similar in all four specimens. The largest distortions occurred when the wall thickness was increased, and the height was reduced. It was also shown that the measurements made by x-ray diffraction and ESPI incremental hole drilling were not consistent with each other. The latter showed unrealistically high measurements near the surface.

The effect of annealing on the tribological and corrosion properties of Al–12Si samples produced by selective laser melting (SLM) is evaluated via sliding and fretting wear tests and weight loss experiments and compared to the corresponding material processed by conventional casting. Sliding wear shows that the as-prepared SLM material has the least wear rate compared to the cast and heat-treated SLM samples with abrasive wear as the major wear mechanism along with oxidation. Similar trend has also been observed for the fretting wear experiments, where the as-prepared SLM sample displays the minimum wear loss. On the other hand, the acidic corrosion behavior of the as-prepared SLM material as well as of the cast samples is similar and the corrosion rate is accelerated by increasing the heat treatment temperature. This behavior is due to the microstructural changes induced by the heat treatment, where the continuous network of Si characterizing the as-prepared SLM sample transforms to isolated Si particles in the heat-treated SLM specimens. This shows that both the wear and corrosion behaviors are strongly associated with the change in microstructure of the SLM samples due to the heat-treatment process, where the size of the hard Si particles increases, and their density decreases with increasing annealing temperature.

The diploma thesis deals with the selection of process parameters used for manufacturing of high-strenth materials using SLM technology. The feedstock material was powder with a chemical composition according to standard DIN X3NiCoMoTi 18-9-5. Influence of change in process parameters on mechanical properties was examined by hardness tests and tensile tests. Metallographic and fractographic analysis were conducted with an aim to understand mechanisms of failure present in this type of material. Selection of optimal process parameters was based on the analysis of mechanical properties of manufactured samples. Possible future steps related to the improvement of the process were proposed. Results of this experiment were compared with literature regarding parts produced by SLM technology and conventional methods.

This diploma thesis deals with properties of multi-materials interface composed of pure iron and Cu7Ni2Si1Cr alloy produced by SLM process. The theoretical part of thesis is focused on selective laser melting technology, and on description of defects connected with the production of SLM parts. Furthermore, one section deals with the production of multi-materials prepared by the SLM process. The experimental part of this thesis deals with selections of the SLM process parameters appropriate for bulk samples preparation. Mechanical properties were determined by the tensile tests at room temperature. Metallographic and fractographic analyses were performed for evaluation of the microstructure and description of the fracture mechanisms.

Additive technology (AT) is increasingly used to design unique parts, mainly due to the ability to produce complex structures such as lattice structures. However, this also includes the need to modify the process parameters or the production strategy of the AT, which is usually set to produce volume geometry. Using samples corresponding to the geometries of the lattice structures, the exact input values were measured, which were used to design the SLM (Selective laser melting) production process using a contour strategy. Thanks to this, vertical and angled (35.26°) struts with low porosity (up to 0.2 %), low surface roughness and high dimensional accuracy were produced. Porosity was measured on µCT, surface roughness and dimensional accuracy were measured on STL data. The results show that if the parameters of the SLM process are set correctly, it is possible to produce struts with low porosity and surface roughness using different combinations of laser power and scanning speed. The above findings were used in the creation of script that allow the selection of suitable process parameters to produce lattice structures.