The degree of mineral liberation is important for the efficiency of subsequent physical separation processes such as froth flotation. Mineral liberation studies involve determining the volumetric abundance or volumetric grade distribution of a specific mineralogical phase in a particular mineral. Currently, methodologies for assessing mineral liberation are laborious regarding sample preparation, analysis time (from weeks to months), and the need for stereological correction. These constraints can be eliminated by using X-ray CT which gives the cross-sections directly from three-dimensional data in shorter time (from ten minutes to hours) with minimal sample preparation. X-ray computed tomography (CT) is a non-destructive technique which allows three-dimensional visualisation of inner structures of an object based on the variations in density and atomic composition. Initially, it was developed as a medical tool for imaging soft tissue and bone. During the last decade, the number of X-ray CT applications in engineering and geology has steadily increased, with the improvements in performance and imaging capabilities. The aim of the present work is to apply X-ray CT technique for finely divided ore samples and to study the relationship between mineral liberation and CT results. Four different ore types were used in this study: Northparkes ore (Australia), Ernest Henry ore (Australia), Keetac ore (USA) and Cannington ore (Australia). Different settings of the desktop X-ray CT technique were applied for each particular ore sample for several ore liberation (particle size distribution) properties. Two dimensional CT images were reconstructed from the three-dimensional X-ray CT data. It was found that the settings for CT technique were a function of the ore type. Particularly in the case of Cannington (high density ore) the best setting conditions split from the rest of the ores tested. The appearance of different artifacts occurring during the analysis were studied and kept to the minimum. A functionality between mineral liberation and CT results was found. The variables affecting the most the results were the Voltage and Minimum Intensity Percentage. Contrary to the expected trends, variables having a negligible effect on the results were found to be exposure time / equivalent Al filter thickness.

The degree of mineral liberation is important for the efficiency of subsequent physical separation processes such as froth flotation. Mineral liberation studies involve determining the volumetric abundance or volumetric grade distribution of a specific mineralogical phase in a particular mineral. Currently, methodologies for assessing mineral liberation are laborious regarding sample preparation, analysis time (from weeks to months), and the need for stereological correction. These constraints can be eliminated by using X-ray CT which gives the cross-sections directly from three-dimensional data in shorter time (from ten minutes to hours) with minimal sample preparation. X-ray computed tomography (CT) is a non-destructive technique which allows three-dimensional visualisation of inner structures of an object based on the variations in density and atomic composition. Initially, it was developed as a medical tool for imaging soft tissue and bone. During the last decade, the number of X-ray CT applications in engineering and geology has steadily increased, with the improvements in performance and imaging capabilities. The aim of the present work is to apply X-ray CT technique for finely divided ore samples and to study the relationship between mineral liberation and CT results. Four different ore types were used in this study: Northparkes ore (Australia), Ernest Henry ore (Australia), Keetac ore (USA) and Cannington ore (Australia). Different settings of the desktop X-ray CT technique were applied for each particular ore sample for several ore liberation (particle size distribution) properties. Two dimensional CT images were reconstructed from the three-dimensional X-ray CT data. It was found that the settings for CT technique were a function of the ore type. Particularly in the case of Cannington (high density ore) the best setting conditions split from the rest of the ores tested. The appearance of different artifacts occurring during the analysis were studied and kept to the minimum. A functionality between mineral liberation and CT results was found. The variables affecting the most the results were the Voltage and Minimum Intensity Percentage. Contrary to the expected trends, variables having a negligible effect on the results were found to be exposure time / equivalent Al filter thickness.

The degree of mineral liberation is important for the efficiency of subsequent physical separation processes such as froth flotation. Mineral liberation studies involve determining the volumetric abundance or volumetric grade distribution of a specific mineralogical phase in a particular mineral. Currently, methodologies for assessing mineral liberation are laborious regarding sample preparation, analysis time (from weeks to months), and the need for stereological correction. These constraints can be eliminated by using X-ray CT which gives the cross-sections directly from three-dimensional data in shorter time (from ten minutes to hours) with minimal sample preparation. X-ray computed tomography (CT) is a non-destructive technique which allows three-dimensional visualisation of inner structures of an object based on the variations in density and atomic composition. Initially, it was developed as a medical tool for imaging soft tissue and bone. During the last decade, the number of X-ray CT applications in engineering and geology has steadily increased, with the improvements in performance and imaging capabilities. The aim of the present work is to apply X-ray CT technique for finely divided ore samples and to study the relationship between mineral liberation and CT results. Four different ore types were used in this study: Northparkes ore (Australia), Ernest Henry ore (Australia), Keetac ore (USA) and Cannington ore (Australia). Different settings of the desktop X-ray CT technique were applied for each particular ore sample for several ore liberation (particle size distribution) properties. Two dimensional CT images were reconstructed from the three-dimensional X-ray CT data. It was found that the settings for CT technique were a function of the ore type. Particularly in the case of Cannington (high density ore) the best setting conditions split from the rest of the ores tested. The appearance of different artifacts occurring during the analysis were studied and kept to the minimum. A functionality between mineral liberation and CT results was found. The variables affecting the most the results were the Voltage and Minimum Intensity Percentage. Contrary to the expected trends, variables having a negligible effect on the results were found to be exposure time / equivalent Al filter thickness.

The degree of mineral liberation is important for the efficiency of subsequent physical separation processes such as froth flotation. Mineral liberation studies involve determining the volumetric abundance or volumetric grade distribution of a specific mineralogical phase in a particular mineral. Currently, methodologies for assessing mineral liberation are laborious regarding sample preparation, analysis time (from weeks to months), and the need for stereological correction. These constraints can be eliminated by using X-ray CT which gives the cross-sections directly from three-dimensional data in shorter time (from ten minutes to hours) with minimal sample preparation. X-ray computed tomography (CT) is a non-destructive technique which allows three-dimensional visualisation of inner structures of an object based on the variations in density and atomic composition. Initially, it was developed as a medical tool for imaging soft tissue and bone. During the last decade, the number of X-ray CT applications in engineering and geology has steadily increased, with the improvements in performance and imaging capabilities. The aim of the present work is to apply X-ray CT technique for finely divided ore samples and to study the relationship between mineral liberation and CT results. Four different ore types were used in this study: Northparkes ore (Australia), Ernest Henry ore (Australia), Keetac ore (USA) and Cannington ore (Australia). Different settings of the desktop X-ray CT technique were applied for each particular ore sample for several ore liberation (particle size distribution) properties. Two dimensional CT images were reconstructed from the three-dimensional X-ray CT data. It was found that the settings for CT technique were a function of the ore type. Particularly in the case of Cannington (high density ore) the best setting conditions split from the rest of the ores tested. The appearance of different artifacts occurring during the analysis were studied and kept to the minimum. A functionality between mineral liberation and CT results was found. The variables affecting the most the results were the Voltage and Minimum Intensity Percentage. Contrary to the expected trends, variables having a negligible effect on the results were found to be exposure time / equivalent Al filter thickness.

Biofilms are microbial communities developing at the interface between two phases, usually solidliquid, where the micro-organisms are nested in a self-secreted polymer matrix. The biofilm mode of growth is predominant in nature (for e.g. the slimy matter forming on rocks at river bottoms, the viscous deposit in water pipes or even dental plaque) and confers a suitable environment for the development of the micro-organisms. This is particularly the case for porous media which provide favourable substrates given their significant surface to volume ratio. The multi-physical framework of biofilms in porous media is highly complex where the mechanical, chemical and biological aspects interacting at different scales are poorly understood and very partially controlled. An example is the feedback mechanism between flow, spatial distribution of the micro-organisms and the transport of nutrient (by diffusion and advection). Biofilms developing in porous media are a key process of many engineering applications, for example biofilters, soil bio-remediation, CO2 storage and medical issues like infections. Progress in this domain is substantially hindered by the limitations of experimental techniques in metrology and imaging in opaques structures. The main objective of this thesis is to propose robust and reproducible experimental methodologies for the investigation of biofilms in porous media. An experimental workbench under controlled physical and biological conditions is proposed along with a validated 3D imaging protocol based on X-ray micro-tomography (XR MT) using a novel contrast agent (barium sulfate and agarose gel) to quantify the spatial distribution of the biofilm. At first, the XR MT-based methodology is compared to a commonly used techniques for biofilm observation: one or multiple photon excitation fluorescence microscopy, here two-photon laser scanning microscopy (TPLSM). This comparison is performed on Pseudomonas Aeruginosa biofilms grown in transparent glass capillaries which allows for the use of both imaging modalities. Then, the study of uncertainty associated to different metrics namely volume, 3D surface area and thickness, is achieved via an imaging phantom and three different segmentation algorithms. The quantitative analysis show that the protocol enables a visualisation of the biofilm with an uncertainty of approximately 17% which is comparable to TPLSM (14%). The reproducibility and robustness of the XR MT-based methodology is demonstrated. The last step of this work is the achievement of a novel bioreactor elaborated by additive manufacturing and controlled by a high-performance micro-fluidic system. The experimental workbench that we have designed enables to monitor in real-time the evolution of transport properties (effective permeability), O2 concentrations and biofilm detachment by spectrophotometry, all under controlled hydrodynamical conditions. Our methodology allows to investigate the influence of biophysical parameters on the colonisation of the porous medium, for example, the influence of flow rate or nutrient concentration on the temporal development of the biofilm. In conclusion, the thesis work proposes a robust and reproducible experimental methodology for the controlled growth and 3D imaging of biofilms in porous media; while providing versatility in the control of the substrate’s micro-architecture as well as on the flow and biochemical culture conditions. To our knowledge, the scientific approach followed, along with the experimental apparatus, form the most complete methodology, at this time, for the study of biofilms in porous media.

The occurrence of hot tearing during solidification is one of the major factors influencing both the quality and productivity of aluminum castings. In order to reduce the formation of hot tears, quantitative information regarding both hot tearing formation and semi-solid deformation is essential. In this study, the mechanisms of hot tearing and semi-solid deformation have been investigated via two novel techniques: x-ray micro-tomography on material deformed in the semi-solid region, and development of a three phase microstructural model based on a geometry derived from a Voronoi diagram with rounded corners and porosity. Numerical techniques were utilized to quantify both the size evolution and orientation of internal damage relative to void growth. In order to conduct the above research, a new semi-solid tensile deformation methodology was devised which uses a two thermocouple control technique to enable accurate measurement of semi-solid tensile strength and ductility. The experimental work was conducted on the aluminum – magnesium alloy AA5182 in the as-cast and hot isostatic pressing (HIP) states. The x-ray micro-tomography technique was used to observe that semi-solid deformation is accommodated by internal damage via growth of as-cast porosity and the nucleation of new damage-based voids. As the volume fraction of damage increases, the growth of voids occurs in an orientation perpendicular to the loading direction, both through expansion within the grain boundary liquid and via coalescence between voids. The damage then localizes, causing failure. The finite element semi-solid microstructural model was used to explore the effects of fraction solid, fraction porosity, and grain size on semi-solid constitutive behaviour. The simulations revealed that increased grain size and fraction porosity lead to a reduction in flow stress for a given fraction solid. Furthermore, local strain accumulation was linked to hot tearing, since strain localizes in the liquid very early in the deformation process. Based on the model predictions, a new constitutive relationship was developed over the range 0.75 < fs < 0.95. Together, these two techniques have provided powerful new insight, such as the critical role played by as-cast porosity, on the phenomena of hot tearing and semi-solid deformation in aluminum alloys. / Applied Science, Faculty of / Materials Engineering, Department of / Graduate

Understanding the physics of water evaporation from saline porous media is important in many processes such as soil salinity, terrestrial ecosystem functioning, vegetation and crop production, biological activities in vadose zone, and CO2 sequestration. Precipitation of salt is one of the possible outcomes of the evaporation process from saline porous media which may either enhance or interrupt the desired process depending on the localization and pattern of the precipitated salt. In the present study X-ray micro tomography was used to study the 3D dynamics and patterns of salt deposition in drying porous media under different boundary conditions and the effects of salt concentration, particle size distribution and shape of grains on the precipitation patterns and dynamics at pore-scale have been investigated. Evaporation process from porous media involves preferential invasion of large pores on the surface while the fine pores remain saturated serving as the evaporation sites to supply the evaporative demand. This results in increasing salt concentration in fine pores during evaporation. Precipitation starts when salt concentration exceeds the solubility limit in the preferential evaporation sites. At the early stages, the precipitation rate increases with time until all evaporation sites at the surface reach the solubility limit and turn into the precipitation sites. This is followed by a constant rate of precipitation proportional to the evaporation rate. We show that the formation of salt crust at the surface does not immediately interrupt the evaporation process due to the porous nature of the precipitated salt investigated using the scanning electron microscopy. Also, our results confirmed the formation of discrete efflorescence at the surface of porous media due to the presence of pores with different sizes. Distribution of these fine pores on the surface directly influences the patterns of salt precipitation and thickness of the salt crust such that in the media with more fine pores, precipitated salt forms a thinner crust as the solute transferred to the surface is distributed among more evaporation sites. In contrast, in the media with fewer evaporation sites at the surface the salt crust will be more discrete but thicker. A simple equation is also proposed to estimate the evolution if the thickness of the salt crust on the surface of porous media. Our results provide new insights regarding the physics of salt precipitation and its complex dynamics in porous media during evaporation.

Results of a study of the influence of impeller speed on the strength, structure and morphology of granules produced in a type of high shear mixer granulators are reported. Calcium carbonate particles (Durcal 65) have been granulated in a Cyclomix with a capacity of 5 L. An aqueous solution of polyethylene glycol was used as the binder. The granules produced have been dried and their structure visualized using X-ray micro-tomography equipment, Nanotom, with a resolution of less than 1 μm. It is shown that the operation of the granulator at high impeller tip speeds produces granules with a higher strength and lower porosity than those produced at medium and low impeller speeds. Two different granule micro-structures and morphologies are produced at high and low impeller speeds. Structure descriptors such as phase volume fraction (as representative of porosity), chord length distribution and auto-correlation function (as indices of homogeneity of structure) are used to quantify the internal structure of granules in 3D, which in turn affects the granule strength.

A novel method for manufacturing granules with a large particle at their core, referred to as seeded granules, is presented. As an example, calcium carbonate powders (Durcal) of different grades are used as primary particles and polyethylene glycol (PEG) as liquid binder in high shear granulators of different scales (Cyclomix, manufactured by Hosokawa Micron B.V., The Netherlands). The conditions giving rise to seeded granulations are specified in the form of an operational regime map. It is found that the seeded structure is strongly dependent on the impeller speed and the primary particles size distribution. It is shown that a Stokes number of around 0.1 represents the optimal dynamic conditions in the given example for producing seeded granules, regardless of the scale of the granulator.

O objetivo do presente trabalho foi avaliar, ex vivo, a eficiência dos sistemas rotatórios ProTaper Universal Retreatment Files e Mani Retreatment Files na desobturação de raízes mesiais de molares inferiores, obturadas pela técnica de ondas contínuas de condensação, determinando-se o volume percentual de material obturador remanescente no sistema de canais radiculares, utilizando-se a microtomografia de raios-X. Um total de 18 molares inferiores portadores de dois canais radiculares mesiais que possuíam curvatura entre 25° e 35° e raio de curvatura menor que 10mm, foram preparados até o instrumento 35/.04 Mtwo. Em seguida foram obturados com guta percha e cimento endodôntico AH-Plus pela técnica de ondas contínuas de condensação e mantidos em estufa a 37°C por sete dias. Imagens microtomográficas dos dentes obturados foram realizadas utilizando o microtomógrafo SkyScan 1172 e parâmetros de 100kV e 100A, gerando imagens de tamanho de 11,88m. Em seguida, os dentes foram divididos aleatoriamente em dois grupos experimentais de acordo com o tipo de instrumento de retratamento avaliado, ProTaper Retreatment Universal Files (PR) e Mani Retreatment Files (MR). De início, a desobturação dos canais radiculares foi realizada com a utilização de brocas de largo associadas a uma gota de solvente para que então os instrumentos de cada sistema fossem utilizados até que a desobturação até o nível do comprimento real de trabalho, fosse alcançada. Após novo escaneamento, as imagens foram reconstruídas utilizando-se o software NRecon e analisadas pelo software CTAn, permitindo a obtenção dos dados quantitativos das amostras. Empregou-se o teste t de Student para determinar a ocorrência de diferença estatística entre os grupos experimentais (p < 0.05). Os volumes, inicial e final médios (mm3) de material obturador remanescente foram de 17,72 e 2,12 para o grupo PR e de 16,61 e 3,71 para o grupo MR, respectivamente. O grupo PR apresentou o menor volume percentual médio de material obturador remanescente (12,76 ± 6,93%), quando comparado ao MR (23,54 ± 10,60%), observando-se diferença estatisticamente significante. Nenhum dos dois sistemas testados, foi capaz de remover completamente o material obturador do interior dos canais radiculares. O sistema rotatório ProTaper Universal Retreatment Files mostrou-se mais eficiente que o sistema Mani Retreatment Files na desobturação de canais mesiais de molares inferiores, obturados pela técnica de ondas contínuas de condensação. As características dos sistemas rotatórios de retratamento podem interferir no volume percentual de material obturador remanescente e conseqüentemente na sua eficiência de desobturação. / The objective of this study was to evaluate, ex vivo, the efficiency of rotary ProTaper Universal Retreatment Files and Mani Retreatment Files in removal procedure of the mesial roots of mandibular molars, obturated by the technique of continuous wave of condensation, determining the volume percentage of material remaining filling in root canals, using the X-Ray micro-CT. A total of 18 mandibular molars with two root canals which had mesial curvature between 25° and 35° and the radius of curvature smaller than 10mm, were prepared by the instrument Mtwo size/taper 35/.04. They were then filled with gutta-percha and sealer Ah-Plus by the technique of continuous wave of condensation and maintained at 37°C for seven days. Micro-CT images of the teeth was carried out using the device SkyScan 1172 on 100kV and 100A as parameters, generating images size 11.88 micrometers. Then the teeth were randomly divided into two groups according to the type of instrument retreatment evaluated ProTaper Universal Retreatment Files (PR) and Mani Retreatment Files (MR). Initially, the procedure for remove the root canal obturation was performed with Largo burs associated with a drop of solvent so that the instrument of each system could be used until the complete removal procedure was reached. After re-scanning, the images were reconstructed with the software used NRecon and analyzed by CTAn software, allowing to obtain quantitative data of the samples. We used the Student t test to determine the occurrence of significant differences between experimental groups (p <0.05). The mean initial and final volumes (mm3) of the remaining filling material were 17.72 and 2.12 for the P group and 16.61 to 3.71 for group MR, respectively. The PR group had the lowest average volume percentage of remaining filling material (12.76 ± 6.93%) when compared to MR (23.54 ± 10.60%), with a statistically significant difference. Neither of the systems tested were able to completely remove the filling material inside the root canals. The rotary system ProTaper Universal Retreatment Files was more efficient than the system Mani Retreatment Files in removal procedure of mesial canals, filled with the technique of continuous wave of condensation. The characteristics of rotary retreatment system may interfere with the volume percentage of remaining filling material and consequently the efficiency of removal procedure.