Since current prosthetic heart valve replacements are costly, cause medical complications, and lack the ability to regenerate, tissue-engineered heart valves are an attractive alternative. These could provide an unlimited supply of immunological-tolerated biological substitutes, which respond to patients' physiological condition and grow with them. Since collagen is a major extra cellular matrix component of the heart valve, it is ideal material for constructing scaffolds. Collagen sources have been shown to influence the manufacturing of collagen scaffolds, and two commercial sources of collagen were obtained from Sigma Aldrich and Devro PLC for comparison. Consistencies between the collagens were shown in the primary and secondary structures of the collagen, while inconsistencies were shown at the tertiary level, when a higher level of natural crosslinking in the Sigma collagen and longer polymer chains in the Devro collagen were observed. These variations were reduced and the consistency increased by introducing crosslinking via dehydrothermal treatment (DHT). Collagen scaffolds produced via freeze-drying (FD) and critical point-drying with cross-linking via DHT or 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide /N-hydroxysuccinimide (EDC/NHS) were investigated. All the scaffolds were compatible with mesenchymal stem cells (MSCs) according to the proliferation of the cells and their ability to produce ECM, without differentiating between osteogenic, chondrogenic or endothelial lineages. The FD EDC/NHS scaffold demonstrated the most suitable physical property of all. This result illustrates that FD EDC/NHS crosslinking is the most suitable scaffold investigated as a start for heart valve tissue engineering. To prepare a scaffold with a controlled local, spatial and temporal delivery of growth factor, a composite scaffold comprising poly (lactic-co-glycolic acid) (PLGA) microspheres was developed. This composite scaffold demonstrated the same compatibility to the MSCs as untreated scaffold. However, the PLGA microspheres showed an increase in the deterioration rate of Young's modulus because of the detachment of the microspheres from the scaffold via cellular degradation.

<p>Mechanical property and thermal stability of Zr-Si-N films of varying silicon contents deposited on Al₂O₃ (0001) substrates are characterized. All films provided for characterization were deposited by reactive DC magnetron sputter deposition technique from elemental Zr and Si targets in a N₂/Ar plasma at 800 ^oC. The hardness and microstructures of the as deposited films and post-annealed films up to 1100 ^oC are evaluated by means of nanoindentation, X-ray diffractometry and transmission electron microscopy. The Zr-Si-N films with 9.4 at.% Si exhibit hardness as high as 34 GPa and a strong (002) texture within which vertically elongated ZrN crystallites are embedded in a Si₃N₄ matrix. The hardness of these two dimensional nanocomposite films remains stable up to 1000 ^oC annealing temperatures which is in contrast to ZrN films where hardness degradation occurs already above 800 ^oC. The enhanced thermal stability is attributed to the presence of Si₃N₄ grain boundaries which act as efficient barriers to hinder the oxygen diffusion. X-ray amorphous or nanocrystalline structures are observed in Zr-Si-N films with silicon contents > 13.4 at.%. After the annealing treatments, crystalline phases such as ZrSi₂, ZrO₂ and Zr₂O are formed above 1000 ^oC in the Si-containing films while only zirconia crystallites are observed at 800 ^oC in pure ZrN films because oxygen acts as artifacts in the vacuum furnace. The structural, compositional and hardness comparison of as-deposited and annealed films reveal that the addition of silicon enhances the thermal stability compared to pure ZrN films and the hardness degradation stems from the formation of oxides at elevated temperatures.</p>

Mechanical property and thermal stability of Zr-Si-N films of varying silicon contents deposited on Al2O3 (0001) substrates are characterized. All films provided for characterization were deposited by reactive DC magnetron sputter deposition technique from elemental Zr and Si targets in a N2/Ar plasma at 800 oC. The hardness and microstructures of the as deposited films and post-annealed films up to 1100 oC are evaluated by means of nanoindentation, X-ray diffractometry and transmission electron microscopy. The Zr-Si-N films with 9.4 at.% Si exhibit hardness as high as 34 GPa and a strong (002) texture within which vertically elongated ZrN crystallites are embedded in a Si3N4 matrix. The hardness of these two dimensional nanocomposite films remains stable up to 1000 oC annealing temperatures which is in contrast to ZrN films where hardness degradation occurs already above 800 oC. The enhanced thermal stability is attributed to the presence of Si3N4 grain boundaries which act as efficient barriers to hinder the oxygen diffusion. X-ray amorphous or nanocrystalline structures are observed in Zr-Si-N films with silicon contents &gt; 13.4 at.%. After the annealing treatments, crystalline phases such as ZrSi2, ZrO2 and Zr2O are formed above 1000 oC in the Si-containing films while only zirconia crystallites are observed at 800 oC in pure ZrN films because oxygen acts as artifacts in the vacuum furnace. The structural, compositional and hardness comparison of as-deposited and annealed films reveal that the addition of silicon enhances the thermal stability compared to pure ZrN films and the hardness degradation stems from the formation of oxides at elevated temperatures.

科学研究費補助金 研究種目:一般研究(B) 課題番号:04452280 研究代表者:金武 直幸 研究期間:1992-1993年度

Today, there is an essential need for lightweight, energy-efficient, environmentally benign engineering systems, and this is the driving force behind the development of a wide range of structural and functional materials for energy generation, energy storage, propulsion, and transportation. These challenges have motivated the use of magnesium alloys for lightweight structural systems. Magnesium has a density of 1.74 g/cm3, which is almost 30% less than that of aluminium, one quarter of steel, and almost identicalto polymers. The ease of recycling magnesium alloys as compared to polymers makes them environmentally attractive, but their poor mechanical performance is the primary reason for the limited adoption of these alloys for structural applications. The Mg-Al-Zn alloy AZ91D exhibits an excellent combination of strength, die-castability, and corrosion resistance. However, its mechanical performance with regard to creep strength, for example, at evaluated temperatures is poor. Moreover, very little is known about the correlation between its mechanical properties and microstructural features. This thesis aims to provide new knowledge regarding the role played by microstructure in the mechanical performance of the magnesium alloy. The properties/performance of the material in relation to process parameters became of great interest during the investigation. An exhaustive characterisation of the grain size, secondary dendrite arm spacing (SDAS) distribution, and fraction of Mg17Al12 was performed using optical and electron backscatter diffraction (EBSD). These microstructural parameters were correlated to the offset yield point (Rp0.2), fracture strength, and elongation to failure of the material. It was proposed that the intermetallic phase, Mg17Al12, plays an important role in determining the mechanical and physical properties of the alloy in a temperature range of room temperature to 190°C by forming a rigid network of intermetallic. The presence of this network was confirmed by studying the thermal expansion behaviour of samples of the alloy containing different amounts of Mg17Al12. A physically based constitutive model with a wide validity range was successfully adapted to describe the flow stress behaviour of AZ91D with various microstructures. The temperature-dependent variables of the model correlated quite well with the underlying physics of the material. The model was validated through comparison with dislocation densities obtained using EBSD. The influence of high-pressure die-cast parameters on the distortion and residual stress of the cast components was studied, as were distortion and residual stress in components after shot peening and painting. Interestingly, it was found that intensification pressure has a major effect on distortion and residual stresses, and that the temperature of the fixed half of the die had a slight influence on the component's distortion and residual stress. / Numera finns det ett väsentligt behov av lätta, energieffektiva och miljövänliga tekniksystem. Detta behov är drivkraften för utveckling av ett brett utbud av material för energigenerering, energilagring, framdrivning och transport. Dessa utmaningar motiverade användningen av magnesiumlegeringar för lättviktskonstruktioner. Magnesium har en densitet på 1,74 g/cm3, vilket är ca 30% lägre än för aluminium, en fjärdedel av densiteten för stål och nästan i nivå med många polymerer. Då magnesiumlegeringar dessutom är lätta att återvinna, jämfört med polymerer, gör det dem miljömässigt attraktiva. Låga mekaniska egenskaper är den främsta orsaken till begränsad användning av dessa legeringar för lastbärande tillämpningar. Mg-Al-Zn-legeringen AZ91D uppvisar en utmärkt kombination av styrka, gjutbarhet och korrosionsbeständighet. Dess mekaniska egenskaper vid förhöjd temperatur, som tex kryphållfasthet, är låga. Dessutom är korrelationen mellan mikrostruktur och mekaniska egenskaper oklar. Denna avhandling syftade till att ge ny kunskap om mikrostrukturens roll för magnesiumlegeringars mekaniska egenskaper. Slutligen var materialets egenskaper i förhållande till processparametrar vid tillverkningen av stort intresse. En omfattande karaktärisering av kornstorleks-, sekundära dendritarmavstånds (SDAS)-fördelning och fraktion av Mg17Al12 utfördes med hjälp av optisk mikroskopering och diffraktion av bakåtspridda elektroner (EBSD). Mikrostrukturen korrelerades till sträckgränsen (Rp0.2), brottstyrkan och brottförlängningen. Det föreslogs att den intermetalliska fasen, Mg17Al12, spelar en viktig roll vid bestämning av legeringens mekaniska och fysikaliska egenskaper vid temperaturintervall från rumstemperatur upp till 190°C genom att bilda ett styvt nätverk av intermetaller. Uppkomsten av ett sådant nätverk stöddes genom en studie av den termiska expansionen av legeringen för olika fraktioner av Mg17Al12. En fysikalisk konstitutiv modell med ett brett giltighetsområde användes framgångsrikt för att beskriva det plastiska flytbeteendet hos AZ91D för olika mikrostrukturer. De temperaturberoende variablerna i modellen korrelerade ganska väl med materialets underliggande fysik. Modellen validerades genom att jämföra dislokationstätheten som predikterades av modellen och den med EBSD uppmätta dislokationstätheten. Påverkan av pressgjutningsparametrar på geometrisk tolerans och restspänning hos de gjutna komponenterna studerades. Vidare studerades geometrisk tolerans och restspänning av komponenter efter pening och målning. Intressant nog hade eftermatningsfasen en stor effekt på geometrisk tolerans och restspänningar. Dessutom hade temperaturen på den fasta formhalvan av verktyget även ett visst inflytande på komponentens geometriska tolerans och restspänning.

Due to its hardness, martensite, perhaps, is the most desirable structure, but at the same time, martensite is very brittle. Balancing between hardness and brittleness is a challenge that steel manufacturers must deal with it. To decrease brittleness and to solve this problem, designers purposely temper the steel. Heat treatment, e.g., slowing down the quenching quota/rate, will form a procedure of martensite formation incomplete phase and consequently a mixture of austenite-martensite. Tempering is another alternative to operate on martensite and make it malleable without losing hardness and preventing brittleness. As its seen, the heat treatment for controlling the mechanical chemical property is crucial. Managing the critical temperature, A1, A3, and Ms) during martensite formation, which influences the transformation process, must be considered. The Prior Austenite Grain Size also has been measured.  This project has examined the critical temperature for three wire steel specimens to determine the martensite start temperature (Ms), microstructure, and hardness. The project has mainly used dilatometry. Besides that, light optical microscopy (LOM), hardness measurement of specimens, and empirical equations for determining the critical temperatures have been used. This work has been made up of two main parts: literature review and experimental work/ project procedure.

No / The advances of the polymer melt flow-induced crystallization behaviour and its influence on mechanical properties of high density polyethylene (HDPE) in micron injection (MI) were studied in the present paper. Analysis of mechanical performance, including yield stress and elongation at break, for samples adopted from different regions in a molded plaque showed that a higher injection speed, a higher mold temperature and a longer cooling time could effectively enhance the yield stress but negatively promoted the ductility. Then, the mechanisms of such variation of mechanical performance and the factors affecting it were investigated by means of differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and polarized light microscopy (PLM). The super high shear rate during cavity feeding in MI molding not only induced a typical three-layered structure but also developed a highly oriented fibrously morphological structure in the skin layer. However, such fully oriented morphology was much negative in the interlayer and even could not be observed in the core layer. The results from SEM and PLM observations indicated that the orientation morphology varied significantly through the plaque's cross-section and thickness of the each layer changed with the process parameters and geometric position, and finally led to variation of the mechanical performance.

A balance between strength and ductility has been one of the most important considerations in the steel industry. Austenitic steel or multi-phase steel with retained austenite has plasticity-enhancing mechanisms, which can make it achieve high strength and good formability. Due to the occurrence of twinning-based mechanisms in high Mn steels, they have improved strength without sacrificing ductility. However, high Mn steels with extraordinary mechanical properties has not been used in mass production because of its high material cost together with welding problems and so on. As a consequence, many researchers have attempted to decrease the Mn concentration of high Mn twinning-induced plasticity steels without significant sacrifice of the mechanical properties. In the present work, a novel medium Mn steel with high C is designed with the aim of obtaining comparable mechanical properties as high Mn TWIP steel. In addition to Mn, C is also common effective austenite stabilizing element. C and Mn both increase the SFE of austenite. It should be possible to substitute at least some of the Mn in high Mn steels with C and still retain the TWIP effect. If the reduction in Mn content is not compensated for by the addition of other alloying elements, the microstructure will additionally contain some ferrite or martensite. The problem with C concentration is that it will result in the formation of carbide during the cooling process. As long as the carbide formation is suppressed, the formation of ferrite/martensite in medium Mn steels can be inhibited by an increase in the C concentration. In such cases, a soft and formable austenitic microstructure can be achieved by quenching from high austenitization temperatures to retain austenite with appropriate mechanical stability. The precipitation and dissolution of cementite in austenitic medium Mn high C steels capable of deformation-induced twinning were analyzed based on the associated length changes. Al addition was found to significantly retard the kinetics of cementite precipitation, indicating its usefulness in the design of cementite-free austenitic medium Mn steels with high C concentrations. Furthermore, Al addition changes the morphology of intragranular cementite from plate-shaped to equiaxed. The tensile properties of alloy were also examined in the present study. The present contribution discusses the mechanical properties of a bulk medium Mn high C steel with special alloying additions to oppose the precipitation of cementite. In particular, it aims to justify the mechanical properties based on crack nucleation and growth mechanisms. The reported mechanical properties enable a comparison with those of the well-known high Mn and Hadfield steels.

No description available.

Les matériaux cellulaires sont des échantillons à très forte porosité qui peuvent être décrits à deux échelles : la mésostructure et la microstructure. Le lien entre l'architecture des matériaux et les propriétés mécaniques a été largement étudié dans la littérature. Les caractéristiques microstructurales peuvent avoir une influence importante sur les propriétés macroscopiques. Le but de ce travail est de relier les caractéristiques architecturales et microstructurales des matériaux cellulaires à leurs propriétés mécaniques grâce notamment à la tomographie aux rayons X. Une nouvelle approche combinant l'imagerie 3D à plusieurs résolutions, le traitement d'images et la modélisation éléments finis a permis de prendre en compte la microstructure de la phase solide. Quatre matériaux cellulaires modèles ont ainsi été étudiés : des mousses d'aluminium, des structures cellulaires périodiques en alliage de cobalt-chrome, des échantillons de β-TCP et des composites hydroxyapatite/β-TCP. Les matériaux métalliques ont été fournis par des collègues d'autres laboratoires, tandis que les matériaux céramiques ont été fabriqués dans le cadre de cette étude. Pour chaque type de matériaux (métaux et céramiques), une structure régulière et une stochastique ont été comparées. Pour utiliser la méthode multi-échelle développée dans ce travail, les échantillons ont d'abord été scannés grâce à la tomographie locale dans laquelle l'échantillon est placé près de la source de rayons X. La tomographie locale permet de scanner la petite partie irradiée de l'échantillon et d'obtenir une image agrandie par rapport aux images à plus basse résolution. Ces images permettent d'observer certains détails de la phase solide non visibles à plus basse résolution. Différentes étapes de traitement d'images ont ensuite été mises en œuvre pour obtenir une image à basse résolution incluant les informations provenant des images à haute résolution. Ceci a été réalisé grâce à une série d'opération de seuillage et sous-résolution des images à haute résolution. Le résultat de ces différentes étapes de traitement d'images donne une image de l'échantillon initial à basse résolution mais qui inclut l'information supplémentaire décelée à haute résolution. Ensuite, des essais mécaniques in situ ont été réalisés dans le tomographe pour suivre à basse résolution l'évolution des échantillons pendant la déformation. Les images initiales citées plus haut ont été utilisées pour produire des maillages éléments finis. Des programmes Java ont été adaptés pour créer des fichiers d'entrée pour les modèles éléments finis à partir des images initiales et des maillages. Les images initiales contenant les informations à propos de la phase solide, les images des essais mécaniques et les modèles éléments finis ont permis d'expliquer le comportement mécanique des échantillons en reliant les sites d'endommagement expérimentaux et les lieux de concentrations de contraintes calculés. / Cellular materials are highly porous systems for which two scales are mainly important: the mesostructure and the microstructure. The mesostructure corresponds to the architecture of the materials: distribution of solid phase “walls” and macroporosity and can be characterized by X-ray tomographic low resolution images. The link between the architecture of the materials and the mechanical properties has been frequently studied. The microstructure refers to the characteristics of the solid phase. Its microstructural features (presence of a secondary phase or of defects due to the sintering) can have a strong influence on the macroscopic properties. The aim of this work is to link the morphological and microstructural features of metallic and ceramic based cellular materials and their mechanical properties thanks to X-ray tomography and finite element modelling. A new method combining X-ray tomography at different resolutions, image processing and creation of finite element modelling enabled to take into account some microstuctural features of the cellular samples. Four different cellular materials were studied as model materials: aluminium foam fabricated by a liquid state process, cobalt periodic structures made by additive manufacturing, β-TCP porous samples fabricated by conventional sacrificial template processing route and hydroxyapatite/β-TCP composites made by additive manufacturing (robocasting). The metal based materials were provided by colleagues while the ceramic based porous materials were fabricated in the frame of the current study. For each type (metals or ceramics), a stochastic and a regular structure have been compared. For implementing the multiscale method developed in this work, the samples were firstly scanned in a so called “local” tomography mode, in which the specimen is placed close to the X-ray source. This allowed to reconstruct only the small irradiated part of the sample and to obtain a magnified image of a subregion. These images enable to observe some details which are not visible in lower resolution. Different image processing steps were performed to generate low resolution images including microstructural features imaged at high resolution. This was done by a series of thresholding and scaling of the high resolution images. The result of these processing steps was an image of the initial sample. Then, in situ mechanical tests were performed in the tomograph to follow the deformation of the sample at low resolution. The above mentioned initial images were used to produce finite element meshes. Special Java programs were adapted to create finite element input files from initial images and meshes. The initial images containing information about the solid phase, the images from the mechanical tests and the finite element models were combined to explain the mechanical behaviour of the sample by linking the experimental damage locations in the sample and the simulated stress concentration sites.