Scanning electron microscopy of Ar-ion milled samples from the Eagle Ford Formation, South Texas shows that the character and abundance of porosity changes significantly across burial conditions as a result of compaction, cementation, bitumen generation, and generation of secondary porosity within organic matter (OM). Samples displaying a range of compositions and maturities are imaged and quantified to provide insight into the effects of these processes. Porosity in low-maturity samples (Ro~0.5%) is volumetrically dominated (0.1% -12.5% bulk volume, average 6.2%) by relatively large, mostly interparticle, primary mineral-associated pores (median sizes range 35.9-52.7 nm). Larger pores are generally associated with coccolith debris that is commonly aggregated into pellets. Porosity and pore size correlate directly with calcite abundance and inversely with OM volumes. OM is dominantly detrital kerogen "stringers" that range in size and have spatial distributions and character suggestive of detrital origin. Destruction of primary porosity in low-maturity samples has occurred due to compaction of ductile kerogen and clays and, to a minor degree, as a result of cementation and infill of early bitumen. Smaller, secondary OM-hosted pores (median size range 11.1-14.9 nm) volumetrically dominate porosity (0.02%-3.6% bulk volume, average of 1.36%), in most high-maturity samples (Ro~1.2%-1.3%). Mineral-associated pores are present, but are typically smaller (median size range from 20.3-40.6 nm) and less abundant (0.0%-10.0% bulk volume, average of 2.5%) than at low maturity. Abundant mineral-associated porosity is present locally in samples where incursion of primary pore space by bitumen has not occurred. OM within high-maturity samples is distributed more evenly throughout the rock fabric, occupying spaces similar in size and morphology to primary interparticle pores, coating euhedral crystals (probable cements), and filling intraparticle porosity. These observations, and positive correlation between calcite and OM volumes (OM-hosted pore volume included) in samples with dominantly OM-hosted pore networks, suggests that a large portion of OM within high-maturity samples is diagenetic in origin and has filled primary pore space. Destruction of primary porosity in high-maturity samples has occurred through cementation, bitumen infill, and, possibly greater compaction. Additional porosity, however, has been generated through maturation of OM. / text

A new method is presented here for petrophysical interpretation of heterogeneous carbonates using well logs and core data. Developing this new method was necessary because conventional evaluation methods tend to yield inaccurate predictions of pore connectivity and permeability in the studied field. Difficulties in the petrophysical evaluation of this field are related to shoulder-bed effects, presence of non-connected porosity, rock layers that are thinner than the vertical resolution of well-logging tools, and the effect of oil-base mud (OBM) invasion in the measurements. These problems give rise to uncommon measurements and rock properties, such as: (a) reservoir units contained within thinly bedded and laminated sequences, (b) very high apparent resistivity readings in the oil-bearing zone, (c) separation of apparent resistivity logs with different depths of investigation, (d) complex unimodal and bimodal transverse relaxation distributions of nuclear magnetic resonance (NMR) measurements, (e) reservoir units having total porosity of 0.02 to 0.26 and permeability between 0.001mD to 4.2D, (f) significant differences between total and sonic porosity, and (g) low and constant gamma-ray values. The interpretation method introduced in this thesis is based on the detection of layer boundaries and rock types from high-resolution well logs and on the estimation of layer-by-layer properties using numerical simulation of resistivity, nuclear, and NMR logs. Layer properties were iteratively adjusted until the available well logs were reproduced by numerical simulations. This method honors the reservoir geology and physics of the measurements while adjusting the layer properties; it reduces shoulder-bed effects on well logs, especially across thinly bedded and laminated sequences, thereby yielding improved estimates of interconnected porosity and permeability in rocks that have null mobile water saturation and that were invaded with OBM. Additionally, dynamic simulations of OBM invasion in free-water depth intervals were necessary to estimate permeability. It is found that NMR transverse relaxation measurements are effective for determining rock and fluid properties but are unreliable in the accurate calculation of porosity and permeability in thinly bedded and highly laminated depth sections. In addition, this thesis shows that low resistivity values are associated with the presence of microporosity, and high resistivity values are associated with the presence of interconnected and vuggy porosity. In some layers, a fraction of the vuggy porosity is associated with isolated pores, which does not contribute to fluid flow. An integrated evaluation using multiple measurements, including sonic logs, is therefore necessary to detect isolated porosity. After the correction and simulation, results show, on average, a 34% improvement between estimated and core-measured permeability. Closer agreement was not possible because of limitations in tool resolution and difficulty in obtaining a precise depth match between core and well-log measurements. / text

Barrier fabrics laminated with nanofiber membranes are used in protective textiles due to their ability to achieve high breathability or water vapor transmission rate (WVTR) while maintaining required barrier properties. The objective of this thesis is to investigate the factors impacting nanofiber membrane breathability. To achieve this objective, the effect of test conditions on breathability, and the relationship between fiber diameter, web porosity and breathability were explored. Nanofiber membranes were solution-spun by electrospinning from 15wt% and 20wt% PA6 solution concentrations, and by forcespinning from 20wt% and 25wt% concentrations. Three web area densities were made from each spinning method and solution combination: 5GSM, 10GSM and 15GSM. In order to investigate the impact of measurement conditions, breathability of all samples was measured by upright cup method (ASTM E96B) at two relative humidity levels (20% and 50%), and three air flow velocity levels (300fpm, 500fpm and 700fpm). The results showed that WVTR of all samples increased significantly when decreasing humidity or increasing air flow velocity. Webs with a lower density (5GSM or 10GSM) had higher changes of WVTR than those with a higher density (10GSM or 15GSM). These results indicate an interaction between the ambient conditions and the nanoweb structure, whereby conditions that are more conducive to water vapor transmission, such as 20%RH and 700fpm, are more discriminant between membranes. Both electropspun and forcespun membranes processed from the lower concentration solutions (15wt%, and 20wt%, respectively) exhibited smaller fiber diameters and smaller mean pore size. Overall, WVTR values varied with membrane thickness, and with solution concentration following a similar pattern as porosity. These effects were more accentuated for the forcespun samples, which had considerably larger pores (2811-5230nm) than the electrospun counterparts (163-298nm). Furthermore, samples forcespun by 20wt% solution were found to have clearly higher WVTR (1587-2194g/m²/24h at 700fpm) than electrospun samples (1526-1614g/m²/24h at 700fpm). This can be explained by the significant difference of pore size between electrospun and forcespun webs. It was concluded that breathability of forcespun samples, particularly those low density ones, could be effectively adjusted by solution concentration and is more sensitive to change of test conditions than that of electrospun webs. / text

Three sets of concrete blocks were cast to investigate the effects of natural exposure conditions, at the macro and microclimate scale, and field curing on the performance and durability of OPC and OPCjGGBS concretes. These are termed the Loughborough winter series, the Loughborough summer series and the Muscat summer series. Three concrete mixes were investigated in the two Loughborough series (30 and 50 MPa OPC concrete mixes and a 30 MPa OPCjGGBS concrete mix) and two in the Muscat weather series (the two 30 MPa concretes). A group of specimens were cast with each mix consisting of 600 x 500 x 150mm concrete blocks plus control cubes and prisms. The samples were cured in-situ and exposed to a range of curing methods and microclimates. Surface zone properties (up to 50mm depth) were evaluated by air permeability, sorptivity, carbonation, thermogravimetry (TG) and mercury intrusion porosimetry (MIP) tests, conducted after 3 and 12 months of site exposure. The results revealed distinct variations due to macroclimate, microclimate, curing, concrete type and age. The air permeability, sorptivity and carbonation of the concrete exposed under moderate and rainy conditions of a Loughborough summer season were lower than identical concrete cast and cured during a very cold and dry Loughborough winter season. Further, the sorptivity of concrete subjected to the hot and dry climatic conditions of Muscat was significantly higher than companion samples subjected to the temperate Loughborough climate. Significant variations in properties were observed within the two sides of the same concrete element, each subjected to a different microclimate. The air permeability, sorptivity, carbonation and porosity were reduced with increased hessian curing duration. However, premature drying of wet hessian during curing had an adverse effect on concrete quality as this produced concrete of higher permeability and carbonation than non-cured concrete. The application of controlled permeability formwork was effective in improving the concrete's sub-surface properties. The curing affected zone (CAZ) extended to approximately 20mm below the surface of the concrete that was exposed to the Loughborough winter and summer climate, and 40-50mm for the concrete exposed to the Muscat climate, with notable variation in properties due to climate and curing. The TG and MlP results provided insights into the mechanisms associated with the variations in the three concrete's properties due to natural field exposure.

Le stockage géologique est aujourd'hui envisagé dans plusieurs domaines tels que le stockage de CO2 ou celui de déchets nucléaires. C'est un projet à long terme qui nécessite un protocole d'étude particulier afin de déterminer et comprendre la formation envisagée, notamment en termes de mécanismes de transports. Les formations étudiées sont fonction du type de stockage dans le sens où un stockage de gaz ou de déchet radioactifs ne vont pas requérir les mêmes besoins. Dans le cas d'un stockage de CO2, la formation hôte doit posséder de bonnes propriétés réservoirs afin de, notamment, faciliter l'injection. Pour un stockage de déchets radioactifs, la formation hôte doit retenir au maximum les éventuelles fuites de fluides contaminés, c'est pourquoi les sites de stockage envisagés sont au sein de formation très peu poreuse et très peu perméable, argilite ou granite notamment.Les travaux présentés dans cette thèse sont liés à deux projets de stockage. Le premier a pour but l'étude pétrophysique d'une formation potentiellement hôte d'un stockage de CO2 dans le Bassin Parisien, la formation carbonatée de l'Oolithe Blanche. Cette formation, composée de trois faciès principaux, présente de faibles propriétés réservoir qui sont influencées par trois paramètres microstructuraux : la nature du liant, la quantité de compaction et, enfin, la taille des pores et leur distribution.Le second projet est basé sur l'étude d'un analogue structurale au laboratoire de Meuse/Haute-Marne de l'Andra pour le stockage de déchets radioactifs. Cet analogue est situé dans l'archipel Maltais, qui présente une structure tabulaire très proche de celle observée dans la région du laboratoire de Meuse/Haute-Marne : calcaire/argile/calcaire. Notre étude a permis la mise en évidence de plusieurs périodes de mouvement de fluides oxydants, dont une traversant l'ensemble de la formation argileuse, remettant ainsi en cause ses propriétés d'imperméabilité. / Geological storage is now considered as a technical solution for CO2 storage andnuclear waste management (for high-level and intermediate-level long-lived radioactivewaste). A geological storage is a long term project which implies a particular protocol in orderto better determine and to better understand the host rock, especially in terms of transportmechanisms. The geological formations studied are chosen in function of their storagecapacity because gas storage or nuclear waste storage do not need the same requirements.In case of CO2 storage, the host formation must provide good reservoir properties in order tofacilitate the injection. Here, the safety of the storage is guaranteed by traps (structural,residual, mineral) and by the presence of a cap rock. Concerning nuclear waste storage, thehost must retain at best the potential radioactive fluids and gaz leaks, and this is the reasonwhy storage sites are studied within low porous and low permeable formation, like argillite orgranite.The work presented in the PhD thesis is related to two storage projects. The first oneis focused on the petrophysical study of a potential host for CO2 storage in the Paris Basin,the “Oolithe Blanche” carbonate formation. The second project is an analogue study of thesedimentary structure explored in the Meuse/Haute-Marne laboratory. This laboratory isstudied by ANDRA to be the first nuclear waste storage in a deep geological formation inFrance. The analogue was found in maltese archipelagos, which presents almost the sametabular structure as the one observed in the Meuse/Haute-Marne laboratory:limestone/clay/limestone affected by a weak tectonique deformation.In the first part, the Oolithe Blanche Formation study allowed to determine thereservoir properties of the three principals facies of the formation. This study was realized onplugs sampled on quarries in Burgundy (France). Those facies are characterized by differentenvironmental processes and deposit energy; nonetheless, they are all located within ashoreface depositional environment. They are composed of ooids, pellets and bioclasts invarying proportions. The reservoir properties studied showed the Oolithe Blanche Formationis a microporous one. Microstructural parameters which influence reservoir properties are:the cement type (sparite or micrite), amount of compaction characterized by the cementquantity and the contact between elements and, at last, the pore size distribution withinporous elements (micro, meso, macropores).The second part of this project is focused on a more petrophysical study which aimedat characterizing the pore network influence (volume, shape in space) on acoustic velocities,6electrical conductivity and on permeability. The study is completed by the use of permeabilitypredictive models based on mercury porosimetry spectra.The maltese archipelagos study is based on observations made by Missenard et al.(in prep.) .), Rocher et al., (2008) and Missenard et al. (2009, 2011) on the Blue ClayFormation, thick clay formation (~ 100 m) and on the underlying Globigerina Limestone. Theclay formation presents an important fracture network characterized by gypsum filling and byan oxidizing zone near the fractures. A similar oxidation, in the shape of lobes andmushrooms, is observed within the Globigerina Limestone.This study is also divided in two parts. In the first one, the focus is on the study ofgypsum filling fractures. Studying this filling is directly linked with the storage topic, because,in the case of a nuclear waste storage, the absence of fractures and fluid motion is animportant condition to insure the storage security. In the case of gypsums filling, the study isbased on geochemical measurements on oxygen (δ18O), sulphur (δ34S) and strontiumisotopes (87Sr/86Sr) coupled with a fluid inclusion study, all measurements performed ongypsum crystal. Those analyses allow us to propose a downward fluids circulation modelthrought the clays. Fluids source which is at the origin of gypsum’s precipitation seems to beyounger than the hosted formation. Because of the position of the maltese islands, inMediterranean sea, one potential source is the Messinian evaporites, which Sr isotopic ratiocorresponds well to our data set.The second part of the maltese study concerns the oxidation shape observed withinthe Globigerina Limestone. The aim is to determine the processes which allowed thisoxidation. The main question is: are those structures the results of an internal heterogeneityin the rock or the sign of a stop in a fluid motion (stop of the fluid or stop of the oxidizingmechanism)? In order to answer those questions we based our interpretaion on the skeletonof the rock (mineralogy, magnetic mineralogy, microstructural study, geochemistry), on poreand porosity (porosity measurements, mercury porosimetry…), on permeability and on therock anisotropy (susceptibility of magnetic anisotropy (SMA) and acoustic velocitiesanisotropy). Some conflicting differences on the dataset exist, especially on anisotropy data,which can suppose some complex processes.

Ce travail de thèse consiste en une étude approfondie du comportement de l'oxyde de silicium implanté Kr ou Xe pour son application comme matériau à faible constante diélectrique. Deux volets sont examinés: une étude structurale par l'utilisation de plusieurs techniques (RBS, PL, MET et PAS) et une étude de la variation de la constante diélectrique par utilisation de la spectroscopie IR avec le développement d'un modèle de la fonction diélectrique et des mesures C(V). Pour la caractérisation structurale, les principaux résultats confirment pour le cas du Kr, une distribution homogène de ce dernier jusqu'à 400°C. Pour le cas du Xe, le profil de distribution en profondeur de Xe est quasi-gaussien. Le Xe reste stable dans le SiO2 jusqu'à 900°C et désorbe à 1100°C et les bulles se transforment en cavités. Les bulles sont formées au niveau du pic des lacunes (p(lacunes)R). Alors qu’en l’absence des bulles, le Xe se localise à la profondeur de fin de parcours du Xe (RpXe) calculée par SRIM. On note aussi la présence de défauts chargés négativement et des défauts paramagnétiques E'. Ces défauts négatifs disparaissent après un recuit à 750°C. La forme des bulles, pour les deux cas Xe et Kr, est influencée par la position de l'interface SiO2/Si; sans doute à cause de la différence des modules d'Young des deux matrices. L'IR et les mesures C(V) ont permis de montrer que l'implantation des deux gaz fait diminuer la valeur de la constante diélectrique jusqu'à 2.8 pour le cas Kr et entre 1.8 et 2.4 pour le cas Xe. La cohérence des résultats obtenus par les deux techniques montrent bien que ces deux gaz rares peuvent être utilisés pour la réalisation de SiO2 de faible constante diélectrique avec un impact plus important quand le Xe est utilisé. Cette étude a permis aussi de montrer la contribution de la polarisabilité et de la porosité sur la réduction de la valeur de la constante diélectrique du SiO2 implanté. / This thesis aims to get a deep insight of Kr and Xe-implanted amorphous SiO2 for its possible application as low-k material. This work is divided in two parts: Two sides are examined: a structural study by using several techniques (RBS, PL, MET et PAS) and investigation of the evolution of the dielectric constant by using IR spectroscopy with a dielectric function model developing and C-V measurements. From structural characterization, our main results confirm, in the case of Kr implantation, an homogeneous distribution for temperature up to 400°C. For Xe, the distribution profile is quasi-gaussian. Xe remains stable in SiO2 then desorbs completely at 1100°C. We demonstrated that Xe-bubbles are located at the projected range of vacancies (RPV) as simulated by SRIM. However, we also showed that if Xe dose is not higher enough to induce bubbles, Xe is located at RP. Such a behavior helps understanding the formation of Xe-bubbles in SiO2. We reported the presence of negative defects charge and the paramagnetic defects E'. These defects disappear after 750°C annealing. The shape of bubbles induced by both Kr and Xe is SiO2/Si interface dependent. They are spherically shaped when interface is closed and quite irregular when this one is far. Differences in Young Modulus of Si and SiO2 can probably explain such a behavior. IR and C-V measurements show that Xe and Kr implantation result in decreasing the dielectric constant value down to 2.8 in the Kr case and in the range 1.8-2.4 in the Xe case. The good agreement between k values provided by IR and C-V measurements clearly valids the fact that Kr or Xe-implantation in SiO2 is a powerful approach to building low-k dielectrics. With Xe leading to a higher decrease. This study has also pointed out the contribution of both the polarisability and the porosity in the reduction of the dielectric constant of the implanted SiO2.

Les travaux de cette thèse s'insèrent dans le cadre de l'étude de défauts détectés par contrôle ultrason dans des pièces forgées en alliage d'aluminium destinées à l'industrie aéronautique.Cette étude a été menée sur deux pièces produites par Aubert&Duval en alliage d'aluminium 7050 fourni par Constellium. Ces pièces ont été sélectionnées sur base d'une étude statistique de l'occurrence des défauts sur cinq années de production industrielle. L'une présente un taux de rebut important du fait de ces défauts, l'autre un taux de rebut quasiment nul, bien qu'elles soient produites avec le même matériau.L'étude de l'origine des défauts a été construite autour de deux axes de recherche:• Axe thermomécanique : formation des défauts pendant la mise en forme par endommagement ductile à chaud.• Axe matériau : caractérisation des défauts préexistants dans le matériau après son élaboration et non refermés pendant la mise en forme.L'axe thermomécanique est basé sur la simulation numérique des gammes de mise en forme des pièces industrielles à l'aide du logiciel Forge® 2009. Le deuxième axe est articulé autour de la caractérisation de l'état de porosité dans un matériau modèle présentant une teneur en hydrogène élevée induisant un taux de porosité plus important que le matériau sain utilisé industriellement. De petits lopins de ce matériau modèle ont été soumis à une campagne de compression alternée simulant le forgeage industriel. La campagne de compression a été conçue par simulation numérique afin de reproduire les conditions thermomécaniques industrielles. Deux techniques de caractérisation complémentaires ont été mises en œuvre pour suivre l'évolution de la porosité : détection indirecte par contrôle ultrason à haute résolution spatiale et observations directes par microscopie électronique à balayage. Une méthode d'analyse quantitative des signaux ultrasonores a été mise au point pour ce travail.La comparaison par simulation numérique du procédé de matriçage des deux pièces industrielles étudiées a permis d'écarter l'hypothèse de la création des défauts par endommagement ductile à chaud. Lors du matriçage, la matière est soumise à des chargements globalement compressifs, et le risque d'endommagement est par conséquent très faible. De plus, comme observé lors de la caractérisation des défauts industriels, les défauts présentent un fond lisse, similaire au fond lisse observé sur les rares porosités présentes dans le matériau industriel à l'état brut d'élaboration. Le même type de fond lisse caractérise également les porosités présentes dans le matériau modèle. Cette observation favorise l'hypothèse de défauts provenant d'un défaut préexistant dans le matériau initial (en l'occurrence à partir d'une porosité). Cette hypothèse est par ailleurs cohérente avec le comportement des porosités lors de la simulation du forgeage sur petits lopins du matériau modèle.Les résultats de cette étude montrent en effet que les porosités ont tendance à s'aplatir et à se refermer pendant la déformation plastique à chaud, sans forcément cicatriser. Les faciès de rupture d'échantillons soumis à de fortes déformations cumulées et ne donnant plus de réponse ultrasonore significative continuent en effet de présenter de petites plages à fond lisse qui témoignent d'une cicatrisation incomplète. Le traitement thermique semble en outre favoriser la réouverture des porosités non cicatrisées (zones lisses) pendant la déformation et leur élargissement (zones ductiles). / The thesis project aims to study the origin of defects detected in 7XXX aluminium alloy components for aeronautical applications.This work was conducted on two different components (A and B) produced by Aubert&Duval using 7050 aluminium alloy ingots produced by Constellium. The choice of these two components is based on a five year industrial production statistical analysis. Component A has a much higher defect rate compared to component B, even though they are produced from the same ingots.This work was conducted according to two research axis:• Thermo-mechanical axis : defects occurred during the material forming as a result of ductile hot damage• Material axis: defects resulted from a pre-existent defect in the raw material that was not closed during forming.The thermo-mechanical axis is based on numerical simulations of the component's forming processes using the Forge® 2009 software. The material axis is based on the experimental characterization of porosity in a model material with high hydrogen content and thus a higher pore density than the industrial material. Small samples of the model material were experimentally forged using an alternating compression test that was designed and developed from the industrial forging process. Theses samples were characterized to describe pore evolution during hot deformation, by the combination of two characterization techniques: High Resolution Ultrasound Control (HRUS) and Scanning Electron Microscope (SEM) observations on 2D sections and fracture surfaces. An ultrasound signal processing technique was also developed in order to quantitatively compare two different deformation states using ultrasound control.The results of the numerical simulation of A and B component stamping process showed that the detected defects could not occur by ductile hot damage. Indeed, the stamping process is purely compressive and damage risks are thus very low. Moreover, the defect experimental characterization showed the presence of smooth surface areas very similar to the surface aspect of the rare observed porosity in the raw material. The same smooth aspect characterized the porosity observed in the model material. These results lead to the hypothesis that the detected defects could occur from a pre-existent defect (porosity more precisely) in the raw material. This hypothesis is consistent with the pore behaviour during the experimental hot forging of the model material.The hot forging experiment conducted on the model material, showed that pores tend to flatten as plastic strain increases. SEM observations on rupture surfaces from the highest plastic strain showed the presence of small smooth aspect areas. These areas confirm that some pores are not completely healed during deformation even though the correspondent ultrasound signal is very low. During heat treatment, unhealed pores after deformation seem to be reopened (smooth aspect surface areas) and expanded (ductile areas).

Despite applications of foamed bitumen technology in pavement construction in various places around the world, there are still several aspects about this technology that are not clear. In addition, knowledge on foamed bitumen technology is mainly empirical and lacks scientific basis. This study addresses some of the aspects for foamed bitumen technology such as: Investigation of any effects in binder composition during the production process for foamed bitumen; assessment of the effect of bitumen source on foamed bitumen characteristics; development of a rational method to optimise foamed bitumen characteristics and conditions; evaluation of aggregate particle coating within foamed bitumen mixes; further improvements in the mix design procedure specifically the method of compaction and optimum bitumen content determination stages are suggested.  Fourier transform infrared spectroscopy techniques were used to investigate any changes in bitumen composition after the production process of foamed bitumen. Fourier transform infrared tests were done on foamed bitumen and neat bitumen specimens for two bitumens with similar penetration grades. Foamed bitumen characteristics of three bitumens were established by producing foamed bitumen at temperatures of 150ºC up to 180ºC and foamant water contents of 1, 2, 3, 4 and 5%. From the analysis of variation of foamed bitumen characteristics (maximum expansion ratio and half-life) at different temperatures a new method based on the equi-viscous bitumen temperature to optimize foamed bitumen conditions and characteristics was proposed. Rice density and surface energy concepts were used to evaluate aggregate particle coating with foamed bitumen. A granite aggregate divided into three different size fractions and three sets of foamed bitumen produced from three bitumen penetration grades were used. A gyratory laboratory compaction procedure for laterite gravels treated with foamed bitumen was established using the modified locking concept. Three laterite gravels with different chemical composition were mixed with foamed bitumen produced from one penetration bitumen grade. The resulting mixes were compacted up to 200 gyrations and the corresponding compaction curve defined in terms of height versus number of gyrations noted. In addition, the optimum moisture content requirements at the modified locking point were determined. 3D packing theory concepts, primary aggregate structure porosity and an indirect tensile strength criteria were employed to determine optimum bitumen content for foamed bitumen mixes.  Fourier infrared techniques revealed that foaming did not cause any changes in the bitumen chemistry, implying that the foamed bitumen production process may possibly be a physical process. Characterisation of foamed bitumen produced from three bitumen penetration grades showed that foamed bitumen characteristics (maximum expansion ratio and half-life) were mainly influenced by binder viscosity rather than the source. The equi-viscous temperature seemed to provide a suitable criterion at which foamed bitumen with optimum characteristics could be produced. Rice density results showed that aggregate size fraction, binder expansion ratio and viscosity influenced aggregate particle coating. For the coarser aggregate fraction, results revealed that binder coating seemed to be mainly influenced by temperature. Whilst for fine aggregate fraction the coating was mainly influenced by surface area. Surface energy results revealed that foamed bitumen exhibited better coating attributes than neat bitumen. A new laboratory compaction procedure for laterite gravels treated with foamed bitumen based on the modified locking point was developed. The modified locking point represents the state at which maximum aggregate particle interlock occurs when mixes are compacted in the field. It is based on the iii analysis of the rate of change for the gyratory compaction curve. The compaction curve in this case is defined in terms of compaction height versus number of gyrations. Gradation analysis beyond the modified locking point showed that aggregate particle breakdown occurred. Analysis of the optimum moisture at the modified locking point revealed that the moisture conditions were less than the aggregate optimum moisture conditions. It is recommended that this point be used to determine the optimal compaction characteristics of foamed bitumen mixes.  Aggregate structure porosity and an indirect tensile strength criteria can be used to determine the bitumen content that could be used in design of foamed bitumen mixes. This would reduce the amount of resources required since the bitumen content could be estimated prior to carrying out the actual laboratory work given that the aggregate grading is known. The aggregate structure can be divided (based on 3D packing theory) into oversize, primary, and secondary structures. The primary structure is mostly responsible for carrying loads whilst the secondary structure fills the voids within the primary structure and provides support to the primary structure. The aggregate size particles constituting the primary structure are deduced as a function of standard sieve sizes using the packing theory concepts. The minimum sieve size for the primary structure is proposed as 1 mm. The oversize structure consists of aggregate particles whose size is greater than the maximum size for the primary structure. The secondary structure consists of aggregate particles whose size is below the minimum size for the primary structure. The primary aggregate structure porosity can be used to establish the starting bitumen content; the bitumen content at which this porosity is 50% is chosen as the initial bitumen content. Indirect tensile strength values corresponding to 50% primary porosity are determined as well as the bitumen contents and compared against the recommended minimum values. / <p>QC 20161012</p>

Manufacturing processes are getting more and more complex with increasing demands of advanced and light weight engineering components, especially in aerospace industry. The global requirements on lower fuel consumption and emissions are increasing the demands in lowering weight of cast components. Ability to produce components in lower wall thickness will not only help to reduce the cost of production but also help to improve the efficiency of engineering systems resulting in lower fuel consumption and lesser environmental hazardous emissions. In order to produce thin-walled components, understanding of mechanism behind fluidity as it is effected by casting parameters is very important. Similarly, for complex components study of solidification morphology and its effects on castability is important to understand. The aim of this work was to investigate casting of thin-walled test geometries (less than 2mm) in aero-space grades of alloys. The casting trials were performed to investigate the fluidity as a function of casting parameters and filling system in thin-walled sections. Test geometries with different thickness were cast and evaluated in terms of filled area with respect to casting parameters, ı.e. casting temperature and shell preheat temperature. Different feeding systems were investigated to evaluate effects of filling mode on castability. Similarly for complex components where geometries are very organic in shape, solidification morphology effects the quality of castings. Process parameters, that effect the solidification morphology were identified and evaluated. In order to develop a relation between defect formation and process parameters, solidification behaviour was investigated using simulations and casting trials. Similarly the effect of factors that influence grain structure and flow related defects were studied. It was observed that fluidity is affected by the mode of geometry filling in investment casting process. The filling mode also have different effect on defect formation. A top-gated configuration is strongly affected by casting parameters where as a bottom-gated configuration is more stable and thus fluidity is not significantly affected by variation in casting parameters. Less porosity and flow-related defects were observed in the bottom-gated system as compared to top-gated system. In the study about casting defects as affected by process parameters, it was observed that shell thickness is important to avoid interdendritic shrinkage. It was observed that the increased shell thickness induces a steeper thermal gradient which is essential in order to minimize the width of the mushy zone. It was also observed that a slower cooling rate along with a steeper thermal gradient at the metal-mould interface not only helps to avoid shrinkage porosity but also increases fill-ability in thinner sections. The work presented here is focused on the optimization of process parameters, in order, for instance, to improve castability and reduce the casting defects in investment casting process. The work, however, does not focus on externally influencing the casting conditions or modifying the casting/manufacturing process. The future work towards PhD will be focused on externally improving the casting conditions and investigating other possible route of manufacturing for thin, complex components.

Orientador: Rodolfo Bruniera Anchieta / Resumo: O objetivo deste trabalho foi avaliar “in vitro” e “in silico” a integridade estrutural da interface de cimentação, o comportamento biomecânico, e a resistência de união da interface dentina/cimento de diferentes técnicas de cimentação de pinos de fibra de vidro (PFV) em canais amplos. Para tanto, foram utilizados 33 incisivos bovinos. Após o tratamento endodôntico, os espécimes foram divididos aleatoriamente em três grupos (n=11): PCN- Pino convencional cimentado em dente com conduto normal; PCA- Pino convencional cimentado em dente com conduto amplo; PAA- Pino anatômico cimentado em dente com conduto amplo. Em seguida, foram executados os preparos intrarradiculares de acordo com cada grupo com brocas pré-estabelecidas, tratamento de superfície dos PFV (WhitePost nº3 DC, FGM) e cimentação dos mesmos com o cimento resinoso autoadesivo (Rely X U200, 3M ESPE). Então, 6 espécimes de cada grupo foram submetidos ao escaneamento em um microtomógrafo de alta resolução (SkyScan 1272) para avaliação da integridade, volume e presença de bolhas na interface de cimentação. Posteriormente, com base nos dados do µCT e imagens de microscopia (n=1), dois modelos tridimensionais de cada grupo foram confeccionados para a análise de elementos finitos, sendo que o primeiro foi considerado ideal (G1, G3 e G5), sem defeitos na interface, e o segundo continha as condições encontradas pela análise de µCT(G2, G4 e G6). Após o envelhecimento em estufa por 7 meses, todos os espécimes foram submetidos a... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The objective of this study was to evaluate “in vitro” and “in silico” the structural integrity of the cementation interface, the biomechanical behavior and the bond strength of different fiberglass post cementation techniques in flared root canal. To this end, 33 bovine incisors were used. After the endodontic treatment, the specimens were randomly divided into three groups (n = 11): PCN - conventional post cemented in tooth with normal canal lumen; PCA- Conventional fiberglass post cemented in flared root canal; PAA- Fiberglass post relined with composite resin and cemented in flared root canal; Then, the intra-radicular preparations were performed according to each group with pre-established drills, surface treatment of PFV (WhitePost Nº. 3DC, FGM) and cementation with self-adhesive resin cement (Rely X U200, 3M ESPE). Then, 6 specimens from each group were submitted to scanning in a high resolution microtomograph (SkyScan 1272) to evaluate the integrity, volume and presence of bubbles at the cementation interface. Then, based on the μCT data and the microscopic images (n = 1), two three-dimensional models of each group were made to analyze finite elements, the first one being considered ideal (G1, G3 and G5), without interface defects and the second contained the conditions found by μCT analysis (G2, G4 and G6). After being stored for 7 months, all specimens were submitted to the pushout bond strength test (n = 10). Data were submitted to ANOVA with repeated measures and ... (Complete abstract click electronic access below) / Mestre