京都大学 / 新制・課程博士 / 博士(農学) / 甲第24663号 / 農博第2546号 / 新制||農||1098(附属図書館) / 学位論文||R5||N5444(農学部図書室) / 京都大学大学院農学研究科森林科学専攻 / (主査)教授 杉山 淳司, 教授 藤井 義久, 教授 仲村 匡司 / 学位規則第4条第1項該当 / Doctor of Agricultural Science / Kyoto University / DFAM

The AM60 Mg alloy has been used in the automotive industry to help achieve higher fuel efficiency. However, its products, mostly fabricated via high pressure die casting process, are inherently plagued with porosity issues. The presence of porosity impairs mechanical properties, especially fatigue properties, and thus affects the product reliability. We have therefore studied the effect of porosity on the fatigue behavior of samples drawn from a prototype AM60 shock tower by conducting strain-controlled fatigue test along with X-ray computed tomography (XCT). The 3D analysis of porosity by XCT showed discrepancies from 2D metallographic characterization. Fatigue testing results showed the machined surface is the preferential site for crack initiation to occur, on which pores are revealed after specimen extraction. A large scatter in fatigue life was observed as crack initiating at a large pore situated on the surface will result in a significantly shorter fatigue life. SEM fractography showed fracture surfaces are generally flat and full of randomly orientated serration patterns but without fatigue striations. The observations and measurements of porosity and fatigue cracks made by XCT were confirmed by SEM, supporting it as a reliable characterization tool for 3D objects and has value in assisting the failure analysis by SEM. Fatigue life was found to decrease with the increase of fatigue-crack-initiating pore size. The same trend was also found between the fatigue life and the volume fraction of porosity. The pore shape and pore orientation should be taken into account when determining the pore size as they can result in the difference in pore size between 2D and 3D measurement. / Thesis / Master of Applied Science (MASc) / The AM60 Mg alloy has been used in the automotive industry to help achieve higher fuel efficiency. However, its products, mostly fabricated via high pressure die casting process, are inherently plagued with porosity issues. The presence of porosity impairs mechanical properties, especially fatigue properties, and thus affects the product reliability. We have therefore studied the effect of porosity on the fatigue behavior of samples drawn from a prototype AM60 shock tower by conducting strain-controlled fatigue test along with X-ray computed tomography (XCT). The 3D analysis of porosity by XCT showed discrepancies from 2D metallographic characterization. Fatigue testing results showed the machined surface is the preferential site for crack initiation to occur, on which pores are revealed after specimen extraction. A large scatter in fatigue life was observed as crack initiating at a large pore situated on the surface will result in a significantly shorter fatigue life. SEM fractography showed fracture surfaces are generally flat and full of randomly orientated serration patterns but without fatigue striations. The observations and measurements of porosity and fatigue cracks made by XCT were confirmed by SEM, supporting it as a reliable characterization tool for 3D objects and has value in assisting the failure analysis by SEM. Fatigue life was found to decrease with the increase of fatigue-crack-initiating pore size. The same trend was also found between the fatigue life and the volume fraction of porosity. The pore shape and pore orientation should be taken into account when determining the pore size as they can result in the difference in pore size between 2D and 3D measurement.

No description available.

Serious issues including solidification porosity, columnar grains, and large grain sizes are common during fusion-based metal additive manufacturing due to the inherent melting and solidification that occurs during printing. In recent years, a high-temperature, rapid plastic deformation technique called additive friction stir deposition (AFSD) has shown great promise in overcoming these issues. Because the deposited material stays in the solid state during printing, there are no melting and solidification events and the process can result in as-printed material that is fully-dense with equiaxed, fine grains. As AFSD is an emerging process, developing an understanding of the synergy between material deformation and the resultant microstructure evolution, especially the strain magnitude, its influence on dynamic microstructure evolution, and material flow details, is imperative for the full implementation of AFSD. Therefore, the purpose of this work is to investigate the severe plastic deformation in AFSD through complementary studies on the concurrent evolution of shape and microstructure during the deposition of dissimilar aluminum alloys. In this work, we systematically study (1) the entire deposition via dissimilar cladding along with (2) specific volumes within the deposited layer via embedded tracers printed at varied processing parameters. X-ray computed tomography and electron backscatter diffraction are employed to visualize the complex shape of the deposits and understand the microstructure progression. Investigation of dissimilar cladding of homogeneous AA2024 feed-rods onto an AA6061 substrate establishes a working understanding of the mechanisms related to material flow and microstructure evolution across the whole deposit (macroscopic shape evolution) as well as at the interface between the deposit and the substrate. Variations in tooling and rotation rate affect the interfacial features, average grain size, and depth of microstructural influence. The non-planar and asymmetric nature of AFSD on the macro-scale is revealed and a maximum boundary of deposited material is established which gives a frame of reference for the next material flow study within the deposition zone. An understanding of the mesoscopic morphological evolution and concurrent dynamic microstructure evolution of representative volumes within the deposition zone is determined by comparing depositions of hybrid feed-rods (AA6061 matrix containing an embedded tracer of AA2024). Samples were printed with and without an in-plane velocity to compare initial material feeding to steady-state deposition. Variations in initial tracer location and tool rotation rate/in-plane velocity pairs affect the final morphology, intensity of mixing, and microstructure of the deposited tracer material. The tracer material undergoes drastic mesoscopic shape evolution from millimeter-scale cylinders to long, curved micro-ribbons. There is simultaneous grain refinement in AA2024 via geometric dynamic recrystallization during initial material feeding, after which the grain size remains relatively constant at a steady-state size. The lower bound of strain is estimated based on extrusion, torsion, and shear-thinning factors. The step-by-step mesoscopic deformation and microstructure evolution is further elucidated by characterizing depositions of hybrid feed-rods with a series of embedded tracers. The AFSD tooling is stopped quickly at the end of the deposition with a quench applied to "freeze" the sample. X-ray computed tomography reveals multiple intermediate morphologies including the progression from a cylinder to a tight spiral, to a flattened spiral shape, and to a thin disc. EBSD mapping shows that a refined microstructure is formed soon after the material leaves to tool head with areas off the centerline reaching a fully recrystallized state more quickly. The findings from this work summarize the current understanding of the link between material deformation and microstructure evolution in AFSD. Hopefully these first fundamental studies on the co-evolution of material flow and grain structure during AFSD can inspire future work, especially in the area of heterogeneous multi-material printing. / Doctor of Philosophy / Additive friction stir deposition (AFSD) is a new metal 3D printing process that uses friction to heat up and deposit materials rather than using a laser to melt the material into place. This is beneficial since it avoids problems that come from melting and solidification (e.g., porosity, hot cracking, residual stresses, columnar grains). Since AFSD is such a new technology, an understanding of some of the fundamental processing science is needed in order to predict and control the performance of the resultant parts. This is because the processing of a material affects its structure (at multiple scales, for example macro-, micro-, atomic) which then affects the properties a material will exhibit which, finally, dictates the performance of the overall part. Therefore, the purpose of this work is to explore how the feed material is transformed and deposited into the final layer after printing and to link the original processing conditions to the resultant structure. To investigate the interface between the deposited layer and the substrate, we use a simple feed-rod of one aluminum alloy (AA2024) and deposit it onto a substrate of another aluminum alloy (AA6061). To look at just one small volume within the deposited layer, we use a hybrid feed-rod that is mostly AA6061 except for small cylinders of AA2024 that are placed either in the center or on the edge of the feed-rod so that we can track the AA2024. Printing these feed-rods under different processing conditions will help us understand the connection between processing and structure. Using a characterization technique called X-ray computed tomography we can visualize a 3D representation of the final position for the AA2024 material. In order to evaluate the structure on the micro-scale, a characterization technique called electron backscatter diffraction is used to show the individual grains of our metal. The main contributions of this work are as follows: 1) a lower bound of strain is estimated for AFSD, 2) various intermediate deformation steps are captured for the tracer cylinders including a progression from cylinder to multiple spiral shapes to a thin disc to long ribbons, 3) these deformation steps are linked to different microstructures, and 4) changing the tool geometry and other processing parameters significantly alters the range of shapes and microstructures developed in the deposited material. These findings bring us closer to a fully controllable system as well as sparking some interesting areas for future research because of the complex shapes we observed. These results could lead to the customization and optimization of 3D spirals, ribbons, etc. designed for a certain application.

While the structure and mechanical properties of natural cellular solids such as wood and trabecular bone have been extensively studied in the past, the structural design and underlying deformation mechanisms of natural cellular solids with very high mineral contents (> 90 wt%), which we term as natural ceramic cellular solids, are largely unexplored. Many of these natural ceramic cellular solids, despite their inherent brittle constituent biominerals (e.g., calcite or aragonite), exhibit remarkable mechanical properties, such as high stiffness and damage tolerance. In this thesis, by carefully selecting three biomineralized skeletal models with distinctly different cellular morphologies, including the honeycomb-like structure in cuttlefish bone (or cuttlebone), the stochastic open-cell structure in sea urchin spines, and the periodic open-cell structure in starfish ossicles, I systematically investigate the mechanical design strategies of these natural ceramic cellular solids. The three model systems are cuttlefish Sepia officinalis, sea urchin Heterocentrotus mammillatus, and starfish Protoreaster nodosus, respectively. By investigating the relationship between their mechanical properties and structural characteristics, this thesis reveals some novel structural design strategies for developing lightweight, tough, strong, and stiff ceramic cellular solids. The internal skeleton of S. officinalis, also known as cuttlebone, has a porosity of 93 vol% (constituent material: 90 wt% aragonite), which is a multichambered structure consisting of horizontal septa and thin vertical walls with corrugated cross-sectional profiles. Through systematic ex-situ and synchrotron-based in-situ mechanical measurements and collaborative computational modeling, we reveal that the vertical walls in the cuttlebone exhibit an optimal waviness gradient, which leads to compression-dominant deformation and asymmetric wall fracture, accomplishing both high stiffness (8.4 MN∙m/kg) and high energy absorption (4.4 kJ/kg). Moreover, the distribution of walls reduces stress concentrations within the horizontal septa, facilitating a larger chamber crushing stress and more significant densification. For the stochastic open-cell foam-like structure, also known as stereom (porosity: 60-80 vol%, constituent material: 99 wt% calcite) in H. mammillatus, we first developed a computer vision-based algorithm that allows for quantitative analysis of the cellular network of these structures at both local individual branch and node level as well as the global network level. This open-source algorithm could be used for analyzing both biological and engineering open-cell foams. I further show that the smooth, highly curved branch morphology with near-constant surface curvature in stereom results in low-stress concentration, which further leads to dispersed crack formation upon loading. Combined synchrotron in-situ analysis, electron microscopic analysis, and computational modeling further reveal that the fractured branches are efficiently jammed by the small throat openings within the cellular structure. This further leads to the formation of damage bands with densely packed fracture pieces. The continuous widening of the damage bands through progressive microfracture of branches at the boundaries contributes to the observed high plateau stress during compression, thereby contributing to its high energy absorption (17.7 kJ/kg), which is comparable and even greater than many synthetic metal- and polymer-based foams. Lastly, this thesis leads to the discovery of a unique dual-scale single-crystalline porous lattice structure (porosity: 50 vol%, constituent material: 99 wt% calcite) in the ossicles of P. nodosus. At the atomic level, the ossicle is composed of single-crystal biogenic calcite. At the lattice level, the ossicle's microstructure organizes as a diamond-triply periodic minimal surface (TPMS) structure. Moreover, the crystallographic axes at atomic and lattice levels are aligned, i.e., the c-axis of calcite is aligned with the [111] direction of the diamond-TPMS lattice. This single crystallinity co-alignment at two levels mitigates the compliance of calcite in the c-axis direction by utilizing the stiff <111> direction of the diamond-TPMS lattice. Furthermore, 3D in-situ mechanical characterizations reveal that the presence of crystal defects such as 60° and screw dislocations at the lattice level suppresses slip-like fracture along the {111} planes of the calcitic diamond-TPMS lattice upon loading, achieving an enhanced energy absorption capability. Even though the skeleton of echinoderm is made up of single-crystal calcite, the structure fractures in a conchoidal manner rather than along the clipping plane, which can continuously fracture the fragments into small pieces and enhance energy dissipation. / Doctor of Philosophy / The application of engineering ceramic cellular solids as structural components is limited by their brittleness and flaw sensitivity. In contrast, nature has evolved ceramic cellular materials such as sea sponge, sea urchin spine, and diatom shells that are simultaneously lightweight, strong, and damage-tolerant. These properties are thought to be achieved by the structure design of the component of those materials. Learning design strategies from these natural ceramic cellular solids is significant for developing lightweight bio-inspired ceramic materials with improved mechanical performance. In this thesis, I investigated mechanical design strategies from natural ceramic cellular solids in three model systems, i.e., cuttlebone from cuttlefish Sepia officinalis, spines from sea urchin Heterocentrotus mammillatus, ossicles from starfish Protoreaster nodosus. These three natural ceramic porous solids have high mineral content in the constituent materials (> 90 wt%) and have a highly porous structure (porosity: 50 vol%-93 vol%). These three model systems are selected to represent the analogs of three typical structure forms of synthetic cellular solids, i.e., honeycomb-like structures, stochastic and periodic open-cell structures, respectively. This thesis aims to establish a quantitative relationship between the 3D multiscale structure and deformation/toughening behavior for these selected natural ceramic cellular solids via a combination of different experimental and computational approaches.

Biomineral composites, consisting of intercrystalline organics and biogenic minerals, have evolved unique structural designs to fulfill mechanical and other biological functionalities. Aside from the intricate architectures at the composite level and 3D assemblies of the biomineral building blocks, the individual mineral blocks enclose intracrystalline structural features that contribute to the strengthening and toughening at the intrinsic material level. Therefore, the design strategies of biomineralized composites can be categorized into two structural levels, the individual building block level and the composite level, respectively. This dissertation aims at revealing the material design strategies at both levels for the bioinspired designs of advanced structural ceramics. At the building block level, there is a lack of comparative quantification of the mechanical properties between geological and biogenic minerals. Correspondingly, I first benchmark the mechanical property difference between biogenic and geological calcite through nanoindentation techniques. The selected biogenic calcite includes Atrina rigida prisms and Placuna placenta laths, corresponding to calcite {0001}, and {101 ̅8} planes. The natural cleavage plane {101 ̅4} of geological calcite was added to the comparative study. Under indentation load, geological calcite deforms plastically via twinning and slips under low loads, and shifts to cleavage fracture under high loads. In comparison, the P. placenta composites, composed of micro-sized single-crystal laths and extensive intercrystalline organic interfaces, exhibit better crack resistance. In contrast, the single-crystal A. rigida prisms show brittle fracture with no obvious plastic deformation. Secondly, how the internal microstructures and loading types affect the mechanical properties of individual building blocks is investigated. The prismatic building blocks are obtained from the bivalves A. rigida and Sinanodonta woodiana, where the former consists of single-crystal calcite and the latter consists of polycrystalline aragonite. The comparative investigation under different loading conditions is conducted through micro-bending and nanoindentation. The continuous mineral matrix in A. rigida prisms leads to comparable modulus under tensile and compressive loadings in the elastic regime, while the high-density intracrystalline nanoinclusions contribute to the conchoidal fracture behaviors (instead of brittle cleavage). In comparison, the interlocking grain boundaries in S. woodiana prisms correlate with easier tensile deformation (smaller tensile modulus) than compression, as well as the intergranular fracture morphologies. The third topic in the biomineral-level investigation focuses on how biomineral utilizes residual stress at the macroscopic scale. The selected model system is the spine from the sea urchin Heterocentrotus mamillatus, which has a bicontinuous porous structure and mesocrystalline texture. It is confirmed that the spine has a macroscopic stress field with residual tension in the central medulla and compression in the radiating layers. The multimodal characterizations on the spine conclude that the structural origins are not associated with the gradient distribution of the intracrystalline defects, including Mg substitution in the calcite matrix, intracrystalline organics, and amorphous calcium carbonates (ACC). It is hypothesized that the residual stress is generated due to the volume expansion during ACC crystallization at the compacted growth front. At the composite level, even though enhanced crack resistance is expected in biomineralized composites due to their hierarchical structures, the correlation between their 3D composite structures and damage/crack evolution is quite limited in the literature. I developed in-situ testing devices integrated with synchrotron-based X-ray tomography to capture the crack propagation in the materials, including the four-point bending and compression/indentation configurations. Two representative models are chosen to demonstrate the deformation of biomineralized composites under bending and compression, respectively, including the calcium carbonate-based gastropod shell (Melo diadema) and the hydroxyapatite-based fish teeth (Pogonias cromis). Also, the two composites are designed to achieve different functional requirements, i.e., enhanced fracture toughness vs. wear resistance. The comprehensive characterizations of these two composites revealed how biological structural composites are designed accordingly to their functional needs. For the crossed-lamellar M. diadema shell, directional dependence of the shell property was revealed, where the transversal direction (perpendicular to the growth line) represents both the stronger and tougher direction, but the longitudinal direction is more resistant to notches and defects. For the P. cromis teeth, the enhanced wear resistance of the near-surface enameloid originates from the intricate designs at the microscale, with c-axes of hydroxyapatite crystals and micro-sized enameloid rods coaligned with biting direction and F and Zn doping. In addition, the fracture morphologies of the fish teeth correlate with the microstructures; the enameloid exhibits corrugated fracture paths due to the interwoven fibrous building blocks, and the dentin exhibits clean planar fracture surfaces. / Doctor of Philosophy / Ceramic materials have wide applications in daily life and advanced technologies, and examples range from kitchenware (e.g., cups and plates) to spacecraft (e.g., thermal coating). These materials have indispensable applications due to their advantages of high strength and hardness, high heat and corrosion resistance, lightweight, chemical inertness, etc. Yet, intrinsic brittleness usually limits their applications. Typical ways to enhance the toughness of ceramics involve microstructure design (by refining the sizes and shapes of grains) and transformation toughening (phase transition) at the individual grain level, composite reinforcement (or ceramic matrix composites) at the composite level, and introducing residual stress to impede crack initiation and propagation. The engineering methods usually involve high energy input, chemical treatment, and usually significant waste and non-ecofriendly emissions. Therefore, learning the design strategies from biological ceramic solids constructed by organisms wound provide valuable insights into enhancing the performance of ceramics while reducing the harmful impact on the environment. In this dissertation, I investigated the mechanical design strategies from natural 3D biomineralized composites from two structural levels, i.e., building-block and composite levels, analogous to individual grains and composite reinforcement in engineering ceramics. For the building-block level research, the model systems include bivalve shells Atrina rigida, Placuna placenta, and Sinanodonta woodiana. The three bivalve shells contain different building blocks with intrinsic microstructures, corresponding to monolithic prisms with controlled nanoinclusions, diamond-shaped thin laths, and polycrystalline prisms with interlocking grains, respectively, presenting different structural designs of individual grains in ceramic materials. The sea urchin Heterocentrotus mamillatus spine represents a natural porous material with compressive residual stress on the surface, and the investigation of the structural origins aims to provide insights into the cost-effective synthesis of stressed ceramics with residual stress for engineering applications. In addition, the composite-level studies focus on the composite structures of the crossed-lamellar shell Melo diadema and the fish teeth from Pogonias cromis. These two model systems correspond to natural ceramic matrix composites with nano-scale fibrous building blocks arranged in 3D specialized for enhanced crack resistance and wear resistance, respectively. The comprehensive investigation of the deformation behaviors and mechanisms allows for a better understanding of the intricate strategies specialized for different functional requirements, which apply to bio-inspired designs in ceramic composites.

High-resolution micro computed tomography (micro-CT) offers 3D image resolution of 1 um for non-destructive evaluation of various samples. However, the micro-CT performance is limited by several factors. Primarily, scan time is extremely long, and sample dimension is restricted by the x-ray beam and the detector size. The latter is the cause for the well-known interior problem. Recent advancement in image reconstruction, spurred by the advent of compressed sensing (CS) theory in 2006 and interior tomography theory since 2007, offers great reduction in the number of views and an increment in the volume of samples, while maintaining reconstruction accuracy. Yet, for a number of reasons, traditional filtered back-projection based reconstruction methods remain the de facto standard on all manufactured scanners. This work demonstrates that CS based global and interior reconstruction methods can enhance the imaging capability of micro-CT scanners. First, CS based few-view reconstruction methods have been developed for use with data from a real micro-CT scanner. By achieving high quality few-view reconstruction, the new approach is able to reduce micro-CT scan time to up to 1/8th of the time required by the conventional protocol. Next, two new reconstruction techniques have been developed that allow accurate interior reconstruction using just a limited number of global scout views as additional information. The techniques represent a significant progress relative to the previous methods that assume a fully sampled global scan. Of the two methods, the second method uses CS techniques and does not place any restrictions on scanning geometry. Finally, analytic and iterative reconstruction methods have been developed for enlargement of the field of view for the interior scan with a small detector. The idea is that truncated projections are acquired in an offset detector geometry, and the reconstruction procedure is performed through the use of a weighting function / weighted iteration updates, and projection completion. The CS based reconstruction yields the highest image quality in the numerical simulation. Yet, some limitations of the CS based techniques are observed in case of real data with various imperfect properties. In all the studies, physical micro-CT phantoms have been designed and utilized for performance analysis. Also, important guidelines are suggested for future improvements. / Ph. D.

Lightweighting demands have been achieved by third generation (3G) Advanced High Strength Steels (AHSSs) by a means of increased strength. The challenge faced in doing so, however, is in ensuring that ductility and crashworthiness is efficiently retained. Key methods in which automotive research has been invested to achieve this strength-ductility balance is by microalloying to promote grain refinement, the introduction of precipitates, and the effective use of plasticity enhancing mechanisms. Specifically, the ability to tailor the stability of retained austenite during deformation has been crucial in manipulating the strength-to-ductility ratio of 3G AHSSs using the Transformation Induced Plasticity (TRIP) effect. On the other hand, dual phase (DP) (i.e: non-TRIP-assisted steels) continue to be most significantly manufactured due to their robust thermomechanical processing but are also compromised by their poor damage tolerance. Hence, considerable reports are available regarding the damage tolerance of DP steels, but the ability for the volume expansion associated with the austenite-to-martensite transformation to suppress damage evolution and enhance a steel’s local formability has not yet been thoroughly investigated. Nonetheless, the damage processes that lead to fracture in 3G AHSSs are complex. A full understanding of the underlying phenomena requires a careful assessment of the strain partitioning amongst phases, how the microstructure evolves with strain and how damage, in the form of voids and micro-cracks, nucleates and grows. This can only be accomplished by applying a range of methodologies, including microscopic Digital Image Correlation (µDIC), X-ray Computed Microtomography (µXCT), Electron Backscattered Diffraction (EBSD) and X-ray Diffraction (XRD), all of which can be tracked as deformation proceeds. This PhD thesis uses a novel post µDIC data processing technique to prove that a reduction in strain gradient, linked to the evolution Geometrically Necessary Dislocations (GNDs), at dissimilar phase interfaces is attainable with vanadium-microalloying and with use of the TRIP effect. A local strain gradient post µDIC data processing technique was developed and first applied on 3G DP steels to show that the microcompatibility between ferrite and martensite directly at the interface is considerably improved with vanadium-microalloying. This in turn microscopically explains this DP steel’s increased local formability/damage tolerance with vanadium micro-additions. Moreover, when applying this novel µDIC technique on two other 3G experimental steels of interest, an ultrahigh strength Quench & Partition (Q&P) steel and a continuous galvanizing line (CGL)-compatible Medium-Mn (med-Mn) steel, an even slower evolution of microstrain gradients at dissimilar phase interfaces was observed. This indicates that, although vanadium-microalloying can improve the damage tolerance of a DP steel, its ability to achieve the ultrahigh strengths is a direct result of the severe inhibition of dislocation motion at dissimilar phase boundaries. Eventually, at high strains, these local strain gradients cannot be maintained and results in premature damage nucleation. By comparison, at such high strains, distinct evidence of damage nucleation was not apparent in the 3G TRIP-assisted steels which is the result of a slow strain gradient evolution delayed by the effective use of TRIP. This finding triggered a further investigation into isolating the impact the rate of TRIP exhaustion has on damage development. By intercritically annealing this prototype med-Mn steel (0.15C-5.8Mn-1.8Al-0.71Si) with a martensitic starting microstructure, within a narrow temperature interval (from 665 to 710°C), it was possible to make significant changes in the steel’s rate of TRIP exhaustion without making considerable changes to its physical microstructure. This steel exhibits the largest true strain at fracture (ɛf = 0.61), meets U.S. Department of Energy (DoE) mechanical targets (28,809 MPa%), and shows sustained monotonic work hardening when intercritically annealed at an intermediate IA temperature of 685°C for 120s. In addition, this IA condition showed optimal damage tolerance properties as an abundance of voids nucleated during its tensile deformation, but their growth was suppressed by prolonging TRIP over a large strain range. There is reason to believe that the heterogeneous distribution of austenite and Mn throughout this 685°C IA condition compared to the other two enabled its suppressed TRIP kinetics and in turn improved damage tolerance. The impact that changes in stress-state, from a stress triaxiality of 0.33-0.89, has on microstrain partitioning, TRIP kinetics and damage evolution was tested on this med-Mn at its 685°C IA condition. With the machining of notches on tensile specimens, it was seen that a high stress triaxiality (0.74-0.89) accelerated the rate of TRIP, whereas the introduction of shear, through a misaligned notched specimen design, delayed TRIP kinetics. The change in mean stress imposed by the notches was deemed to have played an active role in TRIP exhaustion during the material’s tensile deformation. A unique electropolishing micro-speckle patterning technique was applied to show that the amount of strain that can be accommodated by the steel’s the polygonal ferrite-tempered martensitic regions are considerably impacted by external modifications in stress-state. While damages studies using different such notched tensile geometries revealed that once a critical void size is reached in this med-Mn steel, coalescence proceeds at an increasing, exponential rate up to fracture. It continues to remain a challenge to quantify the effects microstrain partitioning, TRIP kinetics and damage evolution separately, opening new avenues for future experimental and modeling investigations. / Thesis / Candidate in Philosophy / A lot of research up to now has been invested in the automotive industry to create steels that are lightweight, strong and show improved crashworthiness. The means by which this has been achieved is with the use of innovative processing routes to manufacture and implement Advanced High Strength Steels (AHSSs) in a vehicle’s body-in-white. Nonetheless, the constant global pressure to reduce greenhouse gas emissions has eventually driven research to a third-generation class of ultrahigh strength, lightweight AHSSs. These steels retain the weight savings of their second-generation counterparts but are more cost-effective to manufacture and can be adapted to current industrial line capabilities. Considerable work has been done to enable the manufacturing of 3G steels, yet the steel characteristics which underpin fracture, thereby affecting the crashworthiness of these steels, continues to be weakly understood. As such, at a microscopic scale, this thesis uses three different promising 3G AHSSs candidates to evaluate the impact their unique steel characteristics has on the ability to resist damage evolution and fracture.

Thesis (PhD)--Stellenbosch University, 2013. / ENGLISH ABSTRACT: Maize (Zea mays L.) is used for human and animal consumption in diverse forms, from specialised foods in developed countries, to staple food in developing countries. Unfortunately, maize is prone to infection by different Fusarium species that can produce harmful mycotoxins. Fusarium verticillioides is capable of asymptomatic infection, where infected kernels show no sign of fungal growth, but are contaminated with mycotoxins. If fungal contamination is not detected early on, mycotoxins can enter the food chain. Rapid and accurate methods are required to detect, identify and distinguish between pathogens to enable swift decisions regarding the fate of a batch or consignment of cereal. Near infrared (NIR) hyperspectral imaging and multivariate image analysis (MIA) were evaluated to investigate the fungal development in maize kernels over time. When plotting principal component (PC) 4 against PC5, with percentages sum of squares (%SS) 0.49% and 0.34%, three distinct clusters were apparent in the score plot and this was associated with degree of infection. Prominent peaks at 1900 nm and 2136 nm confirmed that the source of variation was due to changes in starch and protein. Variable importance plots (VIP) confirmed the peaks observed in the PCA loading line plots. Early detection of fungal contamination and activity (20 h after inoculation) was possible before visual symptoms of infection appeared. Using NIR hyperspectral imaging and MIA it was possible to differentiate between species of Fusarium associated with maize. It was additionally applied to examine the fungal growth kinetics on culture media. Partial least squares discriminant analysis (PLS-DA) prediction results showed that it was possible to discriminate between species, with F. verticillioides the least correctly predicted (between 16-47% pixels correctly predicted). For F. subglutinans 78-100% and for F. proliferatum 60-80% pixels were correctly predicted. Three prominent bands at 1166, 1380 and 1918 nm were considered to be responsible for the differences between the growth zones. Variations in the bands at 1166 and 1380 nm were correlated with the depletion of carbohydrates as the fungus grew while the band at 1918 nm was a possible indication of spore and new mycelial formation. By plotting the pixels from the individual growth zones as a function of time, it was possible to visualise the emergence and interaction of the growth zones as separate growth profiles. The microstructure of fungal infected maize kernels was studied over time using high resolution X-ray micro-computed tomography (μCT). The presence of voids and airspaces could be seen in two dimensional (2D) X-ray transmission images and in the three dimensional (3D) tomograms. Clear differences were detected between kernels imaged after 20 and 596 h of inoculation. This difference in voids as the fungus progressed showed the effect of fungal damage on the microstructure of the maize kernels. Imaging techniques are important for rapid, accurate and objective evaluation of products for quality and safety. NIR hyperspectral imaging offers rapid chemical evaluation of samples in 2D images while μCT offers 3D microstructural information. By combining these image techniques more value was added and this led to a comprehensive evaluation of Fusarium infection in maize. / AFRIKAANSE OPSOMMING: Mielies (Zea mays L.) word in verskeie vorms deur mens en dier verbruik, van gespesialiseerde voedsel in ontwikkelde lande, tot stapelvoedsel in ontwikkelende lande. Ongelukkig is mielies onderhewig aan besmetting deur verskeie Fusarium spesies wat skadelike mikotoksiene kan produseer. Fusarium verticilloioides is in staat tot asimptomatiese infeksie waar die besmette pit geen teken van fungusgroei toon nie, maar (reeds) met mikotoksiene besmet is. Indien fungusbesmetting nie vroegtydig opgespoor word nie, kan mikotoksiene die voedselketting betree. Vinnige en akkurate metodes word benodig om patogene op te spoor, te identifiseer en ook om onderskeid tussen patogene te tref om sodoende (effektiewe) besluite aangaande die gebruik van ‘n lot of besending graan te neem. Naby-infrarooi (NIR) hiperspektrale beelding en meerveranderlike beeld ontleding (MIA) is geëvalueer om fungusontwikkeling in mieliepitte oor tyd te ondersoek. Wanneer hoofkomponent (PC) 4 teenoor PC5 gestip word, met persentasies som van kwadrate (%SS) 0.49% en 0/34%, is drie afsonderlike groepein die telling grafiek waargeneem. Dit is geassosieer met die graad van besmetting. Prominente pieke by 1900 nm en 2136 nm het bevestig dat veranderinge in stysel en proteïene die bron van die variasie was. Veranderlike belangrikheidsgrafieke (VIP) het die pieke wat in die PCA beladingslyngrafieke waargeneem is, bevestig. Vroegtydige opsporing (bespeuring) van fungusbesmetting en aktiwiteit (20 h na inokulasie) was moontlik voor visuele besmettingsimptome verskyn het. Onderskeid tussen Fusarium spesies wat met mielies geassosieer word, was moontlik deur gebruik te maak van NIR hiperspektrale beelding en MIA. Dit is bykomend toegepas om fungusgroeikinetika op kwekingsmedia te bestudeer. Parsiële kleinste kwadrate diskriminantanalise (PLS-DA) voorspellingsresultate het getoon dat dit moontlik was om tussen spesies te onderskei, met F. verticillioides die minste korrek voorspel (tussen 19-47% beeldelemente korrek voorspel). Vir F. subglutinans is 78-100% en vir F. proliferatum is 60-80% beeldelemente korrek voorspel. Drie prominente bande by 1166, 1380 en 1918 nm is oorweeg as oorsaak vir die verskille tussen die groeisones. Variasies in die bande by 1166 en 1380 nm is gekorreleer met die vermindering van koolhidrate soos die fungus groei, terwyl die band by 1918 nm ‘n moontlike aanduiding van spoor en nuwe miseliale vorming is. Deur die beeldelemente van die individuele groeisones as ‘n funksie van tyd te stip, was dit moontlik om die verskyning en interaksie van die groeisones as aparte groeiprofiele te visualiseer. Hoë-resolusie X-straal mikro-berekende tomografie (μCT) is gebruik om die mikrostruktuur van fungusbesmette mieliepitte oor tyd te ondersoek. Die voorkoms van leemtes en lugruimtes kon in die twee-dimensionele (2D) X-straal transmissie beelde en in die drie-dimensionele (3D) tomogramme gesien word. Duidelike verskille is waargeneem tussen pitte wat na 20 en 596 h na inokulasie verbeeld is. Hierdie verskil in leemtes soos die fungus vorder, het die effek van fungusskade op die mikrostruktuur van mieliepitte getoon. Beeldingstegnieke is belangrik vir vinnige, akkurate en objektiewe evaluasie van produkte vir kwaliteit en veiligheid. NIR hiperspektrale beelding bied vinnige chemiese evaluering van monsters in 2D beelde, terwyl μCT 3D mikrostrukturele inligting gee. Meer waarde is toegevoeg deur hierdie beeldingstegnieke te kombineer en dit het gelei tot ‘n omvangryke evaluering van Fusarium besmetting in mielies.

A região da articulação temporomandibular (ATM) possui uma limitação na obtenção de imagens pela radiografia convencional. A tomografia computadorizada é o exame mais indicado pela alta especificidade e sensibilidade, para o diagnóstico, planejamento cirúrgico e tratamento das lesões ósseas. O objetivo deste trabalho consiste na avaliação de lesões ósseas simuladas na cabeça da mandíbula pela tomografia computadorizada. Foram utilizadas 15 mandíbulas secas, onde foram criadas lesões esféricas, com o auxílio de brocas esféricas cirúrgicas de uso odontológico com tamanhos variados (nº 1, 3, 6) na cabeça da mandíbula. As lesões foram avaliadas por meio da TC multislice (64 canais), por 2 examinadores independentemente, em 02 ocasiões distintas, utilizando 2 protocolos: axial, coronal, sagital e imagens parassagitais para visualização dos pólos (anterior, lateral, posterior, medial, superior). Posteriormente, as imagens foram comparadas com as lesões presentes na mandíbula seca (Padrão Ouro) avaliando o grau de especificidade e sensibilidade da TC. Estatística de Kappa, teste de validade e teste do Qui-Quadrado foram utilizados como métodos estatísticos. Como resultados observaram a vantagem da associação dos cortes axial, coronal e sagital com cortes parassagitais para detecção de lesões na região de cabeça de mandíbula. Para determinada localização de lesões nos pólos, os tipos de protocolos não apresentaram diferenças significativas em relação as porcentagens de concordância. Os protocolos para visualização da região de cabeça da mandíbula foram estabelecidos no intuito de melhorar a visualização da presença de alterações de cada pólo da cabeça da mandíbula. No que se refere aos pólos avaliados pelos cortes parassagitais houve melhor visualização no pólo anterior e posterior no sentido látero medial. Nos pólos superior, medial e lateral foram mais bem visualizados no sentido ântero-posterior. / There are limitations for image acquisition using conventional radiography of the temporomandibular joint (ATM) region. Computerized tomography (CT) scan is a better option due to its higher specificity and sensitivity for diagnosis, surgical planning and treatment of bone injuries. The purpose of this study is to evaluate simulated bone injuries of the head of the jaw by CT scan. Spherical lesions were created in the head of 15 dry jaws with dentist drills (sizes 1, 3, and 6). Lesions were evaluated using the CT multislice (64 bits) by 2 examiners independently, in 2 different occasions, using 2 protocols: axial, coronal, and sagittal and parasagittal images for head of the mandible visualization (anterior, lateral, posterior, medial, and superior). Images were compared with the dry jaw (gold standard) regarding the presence of injuries, evaluating the degree of specificity and sensitivity of the CT. Kappa statistics, validity tests, and chi-square tests were used as statistical methods. As a result, we observed the advantage of the association of axial, coronal and sagittal slices with parasagittal slices for detection of lesions in the region of mandibles head. For some lesions localized in polar regions, protocols did not show statistically significant differences regarding the proportion of agreement. Protocols for visualization were created to improve the visualization of lesions in each polar region of the jaws head. Regarding parassagittal slices, there was better lateromedial visualization of the anterior and posterior poles and better anteroposterior visualization of superior, medial, and lateral poles.