Nouvelles voies de fabrication d'alliages métalliques à hautes performances à partir de poudres

La fusion sélective par laser (Selective Laser Melting, SLM), une des techniques de la fabrication additive (AM), permet la production de pièces en trois dimensions (3D) de formes complexes directement à partir de poudres métalliques. Elle présente de nombreux avantages significatifs par rapport aux méthodes traditionnelles de fabrication mais se heurte encore à une faible disponibilité des matériaux en poudre.Le travail effectué dans cette étude a donc consisté à étudier et à développer un nouveau moyen pour réaliser in situ des pièces en alliages et en composites à partir de mélanges de poudres.Au niveau expérimental le choix s est porté sur le système Fer-Aluminium et sur un renforcement par des particules de SiC.Les essais ont permis de constater que dans le processus de fabrication de pièces par SLM la puissance du laser et la vitesse de balayage déterminent au premier chef la densité, la microstructure, la composition de phase et les propriétés mécaniques.À partir d un mélange de poudres, des phases intermétalliques ont été obtenues en contrôlant les paramètres SLM. Un traitement thermique ultérieur influence les paramètres cristallins, le degré d ordre et les propriétés mécaniques des pièces ainsi formées.Avec l utilisation de poudres préalliées, un phénomène de texture a été observé prenant la forme de grains allongés/colonnaires orientés dans la direction de construction.Le renforcement de la matrice de fer par des particules de SiC de différentes tailles conduit à une modification structurale avec la formation de produits d interaction, perlitie et martensite, conduisant à une amélioration de la résistance à la traction par rapport au Fe pur.Selective laser melting (SLM), as one of the additive manufacturing (AM) technologies, enables the production of three dimensional (3D) complex parts directly from metal powders. It offers many significant advantages compared with traditional manufacturing methods; however it faces a limited availability of powder materials.The work done during this study consisted in investigating and developing a new way of in situ producing alloys and composites from powder mixtures.The iron-aluminum system and reinforcement by SiC particles were considered.Experiments have shown that the laser power and scanning speed primarily determine the density, microstructure, phase composition and mechanical properties in the manufacturing process of SLM parts.Using pre-alloyed powders, a phenomenon of texture was observed in the form of elongated/columnar grains oriented in the building direction.Using powder mixtures, intermetallic phases were obtained by controlling the SLM parameters. A heat treatment influences the crystal parameters, the degree of order and the mechanical properties of the formed parts.The reinforcement of the iron matrix by SiC particles of several sizes leads to a structural change with the formation of interaction products, perlite and martensite, leading to an improvement in tensile strength compared to pure Fe.BELFORT-UTBM-SEVENANS (900942101) / SudocSudocFranceF

Fusion sélective par laser - influence de l'atmosphère et réalisation d'alliage in situ

Au cours de la dernière décennie, le procédé de fabrication additive par fusion sélective d'un lit de poudre SLM a attiré une grande attention dans le domaine de l'industrie, car il permet de produire rapidement des pièces de formes complexes. Le but de ce travail est d'étendre les performances des procédés SLM en étudiant la possibilité d'élaborer des pièces en atmosphère raréfiée. Pour atteindre cet objectif, une approche théorique et expérimentale a été développée, avec la mise en place d'une machine de fusion sélective par laser capable de travailler dans le domaine de pression de 1 à 10-2 mbar.Le travail sous vide permet d'éviter la formation du "bouclier" de plasma généré à partir de l'atmosphère de gaz ionisé par l'énergie du laser. Ceci permet d'une part d'éviter la contamination chimique du matériau (oxydation, nitruration,...) au cours des processus de fusion et d'autre part de réduire le taux de porosité. L'effet des paramètres du laser et des variables d'environnement sur la qualité de pièces a été étudié en considérant le cas du fer pur, de l'acier Inox 316L et du titane.Par ailleurs nous avons étudié la possibilité d'obtenir des alliages in-situ au cours de la fabrication par la technique SLM à partir de mélanges de poudres.Des essais ont été conduits à partir de mélanges Mg/Al, Fe/Ni et Ti/Ni. Dans tous les cas nous avons pu obtenir des alliages in-situ pour les domaines de composition visés qui correspondent à des applications pratiques (structures légères, alliage magnétique à faible coercivité, alliage à mémoire de forme). Les propriétés des matériaux obtenus, d'après les premières caractérisations effectuées, se comparent de façon favorable par rapport aux techniques classiques d'élaboration et de mise en œuvre.During the last decade, selective laser melting attracted attention in industry because it could allow producing parts with complex shapes rapidly and accurately. The aim of this work is to obtain parts with desired properties by SLM technology. To achieve this point, a theoretical and experimental approach was developed concerning a new process which carries out the selective laser melting process at pressures in the range 1 to 1.10-2 mbar.Vacuum operating under allows avoiding the plasma shield generated from the gas atmosphere ionized by the high laser energy, which on the one hand avoids the chemical contamination (oxidizing, nitriding ) during the melting process and on the other hand reduces the porosity rate. The effect of laser parameters and environment variables on the quality of parts was studied by considering the case of pure iron, stainless steel 316L and titanium.Moreover, we studied the possibility of obtaining in-situ alloys during the SLM manufacturing technique from mixtures of powders.Tests were conducted from mixtures Mg/Al, Fe/Ni and Ti/Ni. In all cases we were able to obtain in-situ alloys for areas covered composition corresponding to practical applications (lightweight structures, low coercivity magnetic alloy, shape memory alloy). The properties of material obtained from the characterizations performed, which are comparable with the conventional development and implementation.BELFORT-UTBM-SEVENANS (900942101) / SudocSudocFranceF

Effet de projection de pellettes bioxycarbonées sur la qualité de revêtements élaborés par la projection thermique

La technologie de projection plasma atmosphérique (APS) est largement utilisée pour des applications industrielles. Les revêtements élaborés par APS présentent généralement certains défauts. Les travaux effectués dans cette étude ont consisté à étudier et à développer un nouveau moyen pour assurer à la fois un refroidissement efficace au cours de procédé de projection APS et une adaptation des conditions superficielles en vue d élaborer des revêtements de haute qualité. Ce moyen consiste à la projection de glace carbonique (glace sèche ou dioxyde de carbone solide) en association avec la projection plasma. Des simulations numériques ont été réalisées, qui ont permis de constater que les dimensions de la buse de projection de glace carbonique, la pression du gaz propulsif, et les propriétés des pellets de CO2 influencent sensiblement la vitesse des pellets de CO2. A partir de ces éléments, des dimensions optimales ont été évaluées. Afin d examiner l effet de la projection de glace carbonique sur les revêtements réalisés par projection thermique, plusieurs types de matériaux ont été considérés, trois métalliques (acier, CoNiCrAlY et aluminium pur) et trois céramiques (Al2O3, Cr2O3 et ZrO2-Y2O3). Les microstructures des revêtements metalliques réalisés avec projection de glace sèche présentent moins d'oxydes et moins de porosité par rapport à ceux déposés par APS classique. Dans certains cas l adhérence peut aussi être améliorée. Pour les revêtements céramiques, une réduction de la porosité ainsi qu une amélioration significative de l adhérence des revêtements ont été constatés. Pour le dépôt de ZrO2-Y2O3, la résistance aux chocs thermiques a été améliorée en utilisant des paramètres spécifiques. La projection de CO2 peut légèrement déformer la surface des substrats de faible dureté, et nettoyer les pollutions superficielles sur le substrat et conduire à une contrainte de compression plus élevée et à un refroidissement efficace. Il est à noter toutefois qu un problème de condensation de la vapeur d eau peut intervenir en cas de refroidissement du substrat trop important.The technology of atmospheric plasma spraying (APS) is widely used for industrial applications. The coatings produced by APS generally show defects. The work was conducted to investigate and develop a new method to ensure both an effective cooling during the APS process and the adaptation of the surface condition in order to develop high quality coatings. This solution is dry ice (CO2) blasting in combination with thermal spraying. Firstly, numerical simulations were carried out, which revealed that the nozzle size of dry ice blasting, the propellant pressure and the properties of CO2 pellets, significantly affect the velocity of CO2 pellets. From these elements, the optimal dimensions were evaluated. To examine the effects of dry ice blasting on the coatings produced by thermal spraying, several types of materials were considered, three metals (steel, CoNiCrAlY and pure aluminum) and three ceramics (Al2O3, Cr2O3 and ZrO2-Y2O3). The microstructure of metal coatings produced with dry ice blasting show fewer oxides and less porosity compared to those deposited by conventional APS. In some cases the adhesion can be improved. Regarding ceramic coatings, a reduction in porosity and a significant improvement in the coating adhesion were observed. For the deposition of ZrO2-Y2O3, an improvement in thermal shock resistance was achieved using specific parameters. Dry-ice blasting may slightly impact the surface of the substrates with low hardness and could clean the surface pollutions on the substrate and lead to a higher compressive stress and an effective cooling. However, it is noted that the problem of the condensation of water vapor can occur in case of intense cooling of the substrate.BELFORT-UTBM-SEVENANS (900942101) / SudocSudocFranceF

Nano-wear-induced behavior of selective laser melting commercial pure titanium

In this work, the nano-wear-induced behavior of selective laser melting (SLM) processed commercial pure titanium was investigated under several applied loads from 1 mN to 100 mN. The dense (over 99%) commercial pure titanium sample was manufactured using SLM process with optimized process parameters (900 J m-1). Nano-wear testing was performed on the polished surface of SLM processed commercial pure titanium. The friction coefficient increased from 0.04 to 0.9 as the load increased from 1 mN to 100 mN. Additionally, the sliding behavior changed along with the applied loads, from elastic to plastic and unstable friction behaviors. The elastic-plastic transition appeared at applied load of 50 mN, which was also confirmed by the calculation results. While the applied load ranged between 50 mN and 80 mN (plastic friction), the average friction coefficient was light smaller than that of the macroscopic ball-on-disc test. During the sliding, a friction vibration appeared and its mechanism was also investigated and discussed combine the wear surface morphologies

Assessment of the Addition of Fluorapatite in Hydroxyapatite Coatings: Implementation Prosthetics/Bone in Vivo

Hydroxyapatite (Hap: Ca10 (PO4)6 OH2)-Fluorapatite (Fap: Ca10 (PO4)6F2) composite coating on 316 L stainless steel, using the High-Velocity Oxy-Fuel Spray (SHVOF), was investigated. This work is an evaluation of the bioactivity of bone/Hap–Fap composite coatings implanted in the tibia of the rabbit. A small amount of Fap (6.68, 13.26 and 26.52 w% Fap attributed to 0.25, 0.5 and 1% fluor) was introduced into Hap. The fluorapatite provides more stable and adherent deposits. The characteristics of the coatings were investigated with various instruments including Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD) and biological (in-vivo and in-vitro) tests. Hap−Fap coating showed excellent behavior in vitro and in vivo tests revealing that the Fap is effective in improving biocompatibility and bioactivity. This study draws inspiration from technological and biological selection solutions adopted by evolution, to transpose the principles and processes of human engineering

In-situ synthesis of aluminum/nano-quasicrystalline Al-Fe-Cr composite by using selective laser melting

In this research, Al-Fe-Cr quasicrystal (QC) reinforced Al-based metal matrix composites were in-situ manufactured by using selective laser melting (SLM) from the powder mixture. The parametrical optimization based on our previous work was performed with focus on laser scanning speed. From the optimized parameters, an almost dense (99.7%) free-crack sample was fabricated with an ultra-fine microstructure. A phase transition from decagonal QC Al65Cu25Fe10Cr5 to icosahedral QC Al91Fe4Cr5 could be observed as laser scanning speed decreases. Differential scanning calorimetry curves show that the QC phase is quiet stable until 500 °C. And then, the effects of annealing temperature on the microstructural and mechanical properties were determined. The results indicate that the recrystallization and growth behavior of α-Al grains could be prevented by QC particle during annealing. Furthermore, the growth of QC particle, which tends to form a porous structure, leads an improvement of Young modulus and decline of ductility

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Heat treatment of cold-sprayed C355 Al for repair: microstructure and mechanical properties

Cold gas dynamic spraying of commercially pure aluminum is widely used for dimensional repair in the aerospace sector as it is capable of producing oxide-free deposits of hundreds of micrometer thickness with strong bonding to the substrate, based on adhesive pull-off tests, and often with enhanced hardness compared to the powder prior to spraying. There is significant interest in extending this application to structural, load-bearing repairs. Particularly, in the case of high-strength aluminum alloys, cold spray deposits can exhibit high levels of porosity and microcracks, leading to mechanical properties that are inadequate for most load-bearing applications. Here, heat treatment was investigated as a potential means of improving the properties of cold-sprayed coatings from Al alloy C355. Coatings produced with process conditions of 500 °C and 60 bar were heat-treated at 175, 200, 225, 250 °C for 4 h in air, and the evolution of the microstructure and microhardness was analyzed. Heat treatment at 225 and 250 °C revealed a decreased porosity (~ 0.14% and 0.02%, respectively) with the former yielding slightly reduced hardness (105 versus 130 HV0.05 as-sprayed). Compressive residual stress levels were approximately halved at all depths into the coating after heat treatment, and tensile testing showed an improvement in ductility