Abstract In this thesis, methods to process ultrafine ferritic (UFF) structures in steels, i.e. grain sizes below about 3 μm have been investigated. It is shown here, in accordance with the results in the literature, that a steel with a UFF grain size can be obtained by two methods, more or less convenient to mass production: deformation-induced ferrite transformation from fine-grained austenite (the DIF route) and the static recrystallization of various heavily cold-worked initial microstructures (the SRF/SRM route). In the present work, the influencing factors in the processing of UFF structure in the DIF route have been systematically studied in four low-carbon steels: one C-Mn steel and Nb, Nb-Ti and Nb-high Ti microalloyed steels. A high strain, a low deformation temperature close to Ar3 and a fine prior austenite grain size are beneficial to promote the formation of UFF grains. Especially by using complex pretreatments to refine the prior austenite grain size, cold rolling, repeating the low-temperature reheating cycle or using martensitic initial microstructure, a UFF grain size can be obtained in these steels at the strain of 1.2 (70% reduction) at 780 °C. By controlling the cooling rate, the type of the second phase can be adjusted. When using the static recrystallization route, it was found that UFF is difficult to obtain from a single-phase ferrite, but it is relatively readily obtained from deformed pearlite, bainite or martensite, especially in high-carbon steels with 0.3–0.8%C. In deformed pearlite, the cementite lamellae fragmented and spheroidised in the course of heavy deformation can provide numerous nucleation sites by the particle stimulated nucleation mechanism and retard the subgrain and recrystallized grain growth. Nucleation and retardation of grain growth are effective also in deformed bainite, martensite or high-carbon tempered martensite, as discussed in detail in the work. The thermal stability of UFF grained steels was tested and found to be generally excellent, but it varies depending on the processing method. The UFF structure obtained by the SRM route has a thermal stability somewhat weaker than that of the DIF route. For a given steel, UFF grains may show different grain growth modes, related to the dispersion of second phase particles. In the DIF structure, abnormal grain growth occurs at 700 °C after about 2.5 h, while in the SRM structure, normal grain growth takes place slowly at 600 °C. Carbides on the grain boundaries seem to play an important role in inhibiting grain coarsening. No coarse-grained zone was formed at the HAZ of electron beam or laser welded seams, as performed at low heat inputs (up to 1.5 kJ/cm) on thin strips. The hardness even increased from the base metal towards the HAZ and the weld metal in all seams as an indication that they were hardened during the rapid cooling.

No description available.

La synthèse par métallurgie des poudres de nickel à grains ultrafins (UFG) a été effectuée, et l’effet de l’affinement de la microstructure sur le comportement mécanique et les propriétés physiques a été étudié. La possibilité de coupler le broyage et le frittage flash est étudiée avec des résultats prometteurs. Des échantillons de haute densité avec des tailles de grains d = 0.65 – 4 µm, caractérisés par une fraction élevée des joints de grains Σ3 et un faible niveau de contrainte ont été synthétisés. Les propriétés mécaniques des échantillons UFG montrent une bonne combinaison ductilité-résistance mécanique, avec un impact mineur des porosités présentes. L’étude de l’influence de la taille de grain dans le régime UFG sur les propriétés mécaniques montre une limite d’élasticité supérieure à celle attendue et une capacité d’écrouissage plus faible. Ces observations sont cohérentes avec la microstructure déformée à rupture, étudiée par diffraction d’électrons rétrodiffusés et microscopie électronique en transmission. Une haute diffusivité, mesurée par des expériences de traceurs radioactifs, montrent des profils de pénétration très différents liés aux structures de porosités diverses présents dans les échantillons. Ces différentes structures sont aussi responsables de la densification rétrograde observée, uniquement pour les échantillons frittés à partir de poudres broyées. / The present manuscript concerns the synthesis of ultrafine grained (UFG) Ni by powder metallurgy, and the study of the influence of UFG microstructures on the mechanical behavior and physical properties. The possibilities of coupling ball milling and Spark Plasma Sintering are presented showing promising results. Highly dense homogeneous specimens are obtained, with average grain sizes d = 0.65 - 4 µm, and microstructures highlighted by a high fraction of Σ3 grain boundaries dependent on grain size. The mechanical properties in tensile testing for UFG samples are evaluated showing a good combination of strength and ductility, with little impact from porosities, the major drawback of powder metallurgy. The influence of grain size in the UFG regime on the mechanical properties is investigated, showing strength values that deviate from the expected behavior for grain refinement. Likewise, a reduced strain hardening capacity is depicted which correlates to the microstructural observations performed on the deformed state. High diffusivity measured by means of radiotracer experiments is observed in the sintered samples, displaying different penetration profiles that relate to diverse porosity structures. Such structures are also responsible for retrograde sintering observed exclusively in samples processed from BM powders.

Tillverkning av portlandklinker står för ungefär fem procent av världens totala koldioxidutsläpp. Det finns därför ett allmänt intresse att minska användandet av portlandklinker. Klinkern kan antingen ersättas av andra cementerande material, eller så kan nya cementsnåla recept utformas. I den här rapporten har två cement med inmald flygaska respektive slagg från Cementa AB undersökts. För att undersöka klinkerersättnings-materialens potential har tester för tryckhållfasthet, uttorkningskrympning, bindetid, värmeutveckling och arbetbarhet utförts. Resultaten visar att skillnaderna mellan försökscementen och byggcementet är så pass små att båda bör kunna användas som byggcement. Ytterligare har ultrafiller av kalksten använts som ersättare för att minska cementhalten i betongen. Det går lika bra att delvis ersätta försökscementen med ultrafiller som det gör för byggcementet. Med cementsnåla recept och större del ersättningsmaterial finns det stora möjligheter att spara på energi och miljö. Detta borde i framtiden kunna leda till ett bättre och mer miljövänligt byggmaterial. / Manufacture of clinker is responsible for about five percent of the total global carbon dioxide emissions. Therefore, there is a general interest in reducing the use of clinker. Clinker can either be replaced by other cementitious materials, or reduced by using lean-cement recipes. This report examines two experimental cements, one with fly ash and one with slag, developed by Cementa AB. To examine the potential of clinker replacement materials, tests for compressive strength, drying shrinkage, initial setting, heat generation and workability, were performed. The results show that the differences between the experimental cements and the reference are so small that both are useable as building cements. In addition, an ultrafine filler of limestone is used as a replacement material for further reduction of the clinker content in concrete. It was also found, that it is just as efficient to partly replace the experimental cements with ultrafine filler as in the reference cement. There are great opportunities to save energy and the environment impact with both clinker-saving cement recipes and with cement replacement materials. This should lead to a better, more environmentally friendly, building material in the future.

La pollution de l’air cause de près de 7 millions de décès annuels dans le monde. L’exposition aux Particules Ultrafines (PUF), polluants parmi les plus néfastes pour la santé, atteint ses niveaux les plus importants en milieu urbain, principalement dus au transport routier. Dans cette thèse, nous examinons les liens entre les champs de concentration en nombre des PUF émises à l'échappement dans le sillage de modèles simplifiés d'automobiles (corps d’Ahmed) et les propriétés de ces écoulements. Ces travaux permettent de mieux comprendre les niveaux d'exposition aux PUF auxquels sont soumis tous les usagers de la route à l’échelle du sillage du véhicule. Trois modèles simplifiés de véhicules ont été utilisés. Ils sont caractérisés par leur angle de lunette arrière permettant de reproduire en soufflerie les structures principales des écoulements de sillage automobile. A l’aide d’une méthode innovante de traitement des données, des mesures de vitesses acquises grâce à des techniques différentes (LDV/PIV) ont été analysées. Elles ont révélé que l’angle d’inclinaison de la lunette a un rôle déterminant sur la structure des écoulements de sillage. Par ailleurs, la comparaison avec les mesures des concentrations en nombre de PUF a permis de montrer que le volume de la structure torique de recirculation en proche culot, dépendant de la géométrie, a un impact majeur sur la dispersion des particules dans la direction verticale. Enfin, il est mis en évidence que les structures tourbillonnaires longitudinales existantes pour une inclinaison intermédiaire de la lunette ont un impact prépondérant sur la dispersion transversale ainsi que sur la symétrie des champs de concentration. / Around 7 million worldwide annual death sare due to air pollution. Among all pollutants, UltrafineParticles (UFP) cause strong adverse effects. Due to road transport, UFP exposure reaches its most significant levels in urban areas. In this thesis, the aim is to assess the links between the wake flow properties of simplified car models(Ahmed bodies) and UFP number concentration fields due to exhaust emission. This study enables the knowledge about UFP exposure levels of all road users at vehicle wake scale to be better understood. Three simplified car models with three corresponding rear slant angles have been used in order to reproduce the principal wake structures of road vehicles in a wind tunnel. Thanks to an innovative data processing method, velocity measurements with two techniques(LDV/PIV) point out the major role of the rear slantangle on the model wake structures. Moreover, comparisons have been made with particle number concentration measurements of UFP in the wake of the same models. We highlighted the link between the volume of the toric recirculation region close to the rear and the vertical dispersion of UFP. Furthermore, longitudinal vortices that exist with the intermediate rear slant angle geometry play an important role on the transversal dispersion as well as on the concentration field symetry.

This work deals with fatigue properties and stability of microstructure of ultrafine-grained (UFG) copper prepared by severe plastic deformation by means of equal channel angular pressing (ECAP) method. The effect of different fatigue loading regimes and thermal exposition on microstructural changes was investigated and the fatigue lifetime curves were experimentally determined. The research attention was focussed on localization of cyclic plastic deformation and fatigue crack initiation in UFG structure. Experimental results indicate that after stress-controlled fatigue loading (both symmetrical and asymmetrical) the microstructure remains ultrafine; no grain coarsening was observed. Contrary to this, strain-controlled fatigue loading results in formation of bimodal structure. Grain coarsening was observed also after thermal exposition at 250 °C for 30 minutes. Annealing at lower temperatures does not result in grain coarsening or development of bimodal structure. Fatigue loading results in development of surface relief in form of cyclic slip markings. Their density, distribution and shape differ for particular fatigue loading regimes. Differences in crack initiation mechanism in low- and high-cycle fatigue region were found. Nevertheless, the characteristic feature for all loading regimes was stability of UFG microstructure in the region of cyclic slip bands and fatigue cracks.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第20703号 / 工博第4400号 / 新制||工||1684(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 乾 晴行, 教授 安田 秀幸 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

<p>Additive manufacturing (AM) can be an advantageous substitute to various traditional manufacturing techniques. Due to the ability to rapidly create products, AM has been traditionally used to prototype more efficiently. As the industry has progressed, however, use cases have gone beyond prototyping into production of complex parts with unique geometries. Amongst the most popular of AM processes is fused deposition modeling (FDM). FDM fabricates products through an extrusion technique where plastic filament is heated to the glass transition temperature and extruded layer by layer onto a build platform to construct the desired part. The purpose of this research is to elaborate on the potential of this technology, while considering environmental impact as it becomes more widespread throughout industry, research, and academia.</p> <p>Although AM consumes resources more conservatively than traditional methodologies, it is not free from having environmental impacts. Several studies have shown that additive manufacturing can affect human and environmental health by emitting particles of a dynamic size range into the surrounding environment during a print. To begin this study, chapters investigate emission profiles and characterization of emissions from FDM 3D printers with the intention of developing a better understanding of the impact from such devices. Background work is done to confirm the occurrence of particle emission from FDM using acrylonitrile butadiene styrene (ABS) plastic filament. An aluminum bodied 3D printer is enclosed in a chamber and placed in a Class 1 cleanroom where measurements are conducted using high temporal resolution electrical low-pressure impactor (ELPI), scanning mobility particle sizer (SMPS), and optical particle sizer (OPS), which combined measure particles of a size range 6-500nm. Tests were done using the NIST standard test part and a honeycomb infill cube. Results from this study show that particle emissions are closely related to filament residence time in the extruder while less related to extruding speed. An initial spike of particle concentration is observed immediately after printing, which is likely a result of the long time required to heat the extruder and bed to the desired temperature. Upon conclusion of this study, it is theorized that particles may be formed through vapor condensation and coagulation after being released into the surrounding environment.</p> <p>With confirmation of FDM ultrafine particle emission at notable concentrations, an effort was consequently placed on diagnosing the primary cause of emission and energy consumption based on developed hypotheses. Experimental data suggests that particle emission is mainly the result of condensing and agglomerating semi-volatile organic compounds. The initial emission spike occurs when there is dripping of semi-liquid filament from the heated nozzle and/or residue left in the nozzle between prints; this supports the previously stated hypothesis regarding residence time. However, the study shows that while printing speed and material flow influence particle emission rate, the effects from these factors are relatively insignificant. Power profile analysis indicates that print bed heating and component temperature maintaining are the leading contributors to energy consumption for FDM printers, making time the primary variable driving energy input.</p> <p>To better understand the severity of FDM emissions, further investigation is necessary to diligence the makeup of the process output flows. By collecting exhaust discharge from a Makerbot Replicator 2x printing ABS filament and diffusing it through a type 1 water solution, we are able to investigate the chemical makeup of these compounds. Additional exploration is done by performing a filament wash to investigate emissions that may already be present before extrusion. Using solid phase micro-extraction, contaminants are studied using gas chromatography mass spectrometry (GCMS) thermal desorption. Characterization of the collected emission offers more comprehensive knowledge of the environmental and human health impacts of this AM process.</p> <p>Classification of the environmental performance of various manufacturing technologies can be achieved by analyzing their input and output material, as well as energy flows. The unit process life cycle inventory (UPLCI) is a proficient approach to developing reusable models capable of calculating these flows. The UPLCI models can be connected to estimate the total material and energy consumption of, and emissions from, product manufacturing based on a process plan. The final chapter focuses on using the knowledge gained from this work in developing UPLCI model methodology for FDM, and applying it further to the second most widely used AM process: stereolithography (SLA). The model created for the FDM study considers material input/output flows from ABS plastic filament. Energy input/output flows come from the running printer, step motors, heated build plate, and heated extruder. SLA also fabricates parts layer by layer, but by the use of a photosensitive liquid resin which solidifies when cured under the exposure of ultraviolet light. Model material input/output flows are sourced from the photosensitive liquid resin, while energy input/output flows are generated from (i) the projector used as the ultraviolet light source and (ii) the step motors. As shown in this work, energy flow is mostly time dependent; material flows, on the other hand, rely more on the nature of the fabrication process. While a focus on FDM is asserted throughout this study, the developed UPLCI models show how conclusions drawn from this work can be applied to different forms of AM processes in future work.</p>

No description available.

In any underground facilities especially tunnels, it is essential to seal the area against water ingress and leakage of reserved materials. Grouting is a common method used to seal rocks around tunnels, successful grouting reduces the duration and cost of the construction, guarantees better working environment and higher safety, minimizes the maintenance and most important decreases the corresponding environmental hazards significantly. Achieving a sufficient grout spread is one of the prerequisites for a successful and efficient sealing, the penetration of a grout is defined as the length of how far grout penetrates in the rock through fractures from a bore hole. Chemical grouts and cement-based grouts are the prevailing ones among the grouting materials. Despite the better penetrability of chemical grouts, they are unfavorable to use due to environmental hazards associated to them, whilst cement-based grouts are more convenient to use because of their low cost and low environmental impact.The major drawback with cement-based grouts is their limited ability to penetrate the very narrow fractures which is directly related to their filtration tendency which is defined as the tendency of cement grains to agglomerate and build an impermeable filter cake during the flow. Many previous studies investigated the factors that affect the filtration tendency. They drew different conclusions and suggested various methods to improve the penetrability of cement-based grouts.The mixing method is one of the factors that have a great influence on the penetrability of the grout. An effective mixing method improves the dispersion of cement particles in the mixture, thus the penetrability of the grout. As it is known from previous studies, the finer the cement particles the harder to disperse. Grouts based on micro-fine cement (&lt; 30 μm) are essential for the development of grouts that can seal very narrow fractures (20-50) μm compared to (70-80) μm at the present.In this study, the dispersion efficiency of three different mixing methods was evaluated, a conventional lab dissolver equipped with 90-mm disk, a conventional lab dissolver equipped with R/S system and an ultrasound UP400St device. Two cement types, INJ30 and UF12, that are similar in chemical composition but differ in degree of milling were tested. Dispersion was tested with filter pump.The results showed that the conventional lab dissolver equipped with 90-mm disk is ineffective method. The conventional lab dissolver equipped with R/S system is a better method compared to the 90-mm disk but still not effective enough especially when it comes to grouts based on ultra-fine cement (UF12). The ultrasound dispersion is not only the best method between the three methods in comparison, but even more stable and reliable. The best result obtained was grout based on UF12 passing through the 54 μm filter. This could mean that fracture aperture down to 55 μm now can be sealed. This is a significant improvement but there is still a marginal for further improvements. In combination with the dispersion efficiency of different dispersion methods, the study investigated the effect of additives on dispersion in particular and penetrability in general. Results showed that additives do not directly contribute to better dispersion, but they are necessary for better spread since they affect the flow properties.