Search Results (38)

This work investigates the impact of sample size on the measurement of non-wetting/wetting interfacial areas in porous media by X-ray microtomography (XMT). Standard-sized small columns and significantly larger columns, both packed with sand, were imaged using the same industrial XMT system (IMT). Additional small columns were imaged using synchrotron XMT (SMT) to evaluate the comparability between the different systems. The mean bulk densities and porosities for all three imaged sets are statistically identical, indicating that column preparations were robust. The mean non-wetting/wetting interfacial areas measured for the large columns for the low and moderate NAPL saturations (S_n), were 11.3 cm⁻¹ (S_n = 0.13) and 15.3 cm⁻¹ (S_n = 0.22), respectively. The mean interfacial areas measured at the moderate S_n for the two small columns imaged by IMT (16.7 cm⁻¹, S_n = 0.24) and imaged by SMT (16.9 cm⁻¹, S_n = 0.21) are consistent with those of the larger column. In addition, the mean interfacial area measured at the lower S_n for the two small columns imaged by SMT (9.4 cm⁻¹, S_n = 0.12) is consistent with that of the larger column. The results indicate that the small imaged volumes typically used for XMT are sufficient to establish REV conditions for measurement of fluid–fluid interfacial areas in this sand. Full article

We investigate 3D-printed composite materials composed of a photosensitive polylactic acid (PLA) resin blended with 10% starch and fabricated by Digital Light Processing. We synthesize the 3D-printed composites by incorporating a post-processing stage involving thermomoulding at various temperatures ranging from 50 °C to 150 °C. The composition, structure, and thermal and mechanical performance of the 3D-printed composites are evaluated using infrared spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), synchrotron X-ray microtomography and tensile testing assisted with digital image correlation. Our results indicate that post-treatment influences the mechanical behaviour of the composites, leading to a moderate increase in stiffness while the tensile strength remains slightly reduced compared with the reference condition, particularly when moulding temperatures reach 100 °C. Our 3D printing approach combined with the photosensitive/starch blend provides a cost-effective alternative for obtaining 3D-printed biosourced components, maintaining technical performance at a reasonable cost. Full article

Laboratory-scale cryogenic X-ray microtomography was employed for the first time to investigate the early structural evolution of polyurethane (PU) foams. This method enables ex situ studying the internal morphology of the frozen reactive mixture at various times before cell impingement. In this work, the precision of the method was evaluated by studying the early bubble formation and growth under different blowing agents and catalyst contents. It was detected that tripling the catalyst weight content doubled cell nucleation density, from 8.9 × 10⁵ to 1.8 × 10⁶ cells cm⁻³. Yet, doubling the water content has lesser impact on nucleation but leads to fast speeds of cell growth and, in turn, lower relative density at equal reaction times. Overall, it is demonstrated that laboratory cryogenic microtomography can be used to democratise the 3D investigation of the internal structure of foams which was until now only possible in synchrotron facilities. In addition, this method can help elucidate the mechanisms of nucleation and degeneration via directly measuring the density of bubbles and distance between them in the reactive mixture. Finally, this methodology could be extended to recent laboratory nanotomography systems utilizing X-ray tubes with nanometric spot sizes, thereby enabling the confident identification of nucleation events. Full article

This study examined the impact of fluid type and grain diameter on the interfacial area between different pairs of non-wetting and wetting fluids in natural porous media. Synchrotron X-ray microtomography was used to obtain high-resolution, three-dimensional images of multi-phase porous media systems. Multiple porous media, comprising a range of physical and geochemical properties, were used in this study. The four pairs of non-wetting/wetting fluids used were dense OIL/water, light OIL/water, air/dense OIL, and air/water. Images were obtained over a broad range of wetting phase saturation and for both wetting phase drainage and imbibition conditions. The results showed that for each fluid pair, the total (capillary + film) interfacial area increased with decreasing wetting fluid saturation. Interfacial areas were similar among all fluid pairs for a given porous medium. They were also similar for drainage and imbibition conditions. The maximum specific interfacial area (A_m) was shown to correlate well with inverse median grain diameter. The physical properties of the porous medium appear to have a greater influence on the magnitude of specific total interfacial area for a given saturation than fluid properties or wetting phase history. Full article

In this study, we examined how printing temperature affects the microstructure and mechanical properties of polylactic acid (PLA) composite reinforced with iron oxide i.e., magnetite manufactured using a material extrusion technique. The composite was printed at temperatures from 185 °C to 215 °C. Microstructure analysis via synchrotron radiation X-ray microtomography revealed changes in both iron oxide and porosity contents within the printed structures. Mechanical testing results demonstrated a limited effect of the printing temperature on tensile performance. Finite element computation is considered to predict the elasticity behavior of the printed composite by converting 3D images into 3D structural meshes. When implementing a two-phase model, the predictions show a leading role of the iron oxide content, and an overestimation of the stiffness of the composite. A three-phase model demonstrates a better matching of the experimental results suggesting a limited load transfer across the PLA-iron oxide interface with Young’s moduli in the interphase zone as small as 10% of PLA Young’s modulus. Magnetic actuation demonstrates that experiments on PLA-iron oxide plates reveal a pronounced thickness-dependent limitation, with the maximum deflection observed in thin strips of 0.4 mm. Full article

Residual stresses and internal strains in 3D printing can lead to issues such as cracking, warping, and delamination—challenges that are amplified when using functional composite materials like magnetic PLA filaments. This study investigates the thermo-mechanical strain evolution during fused filament fabrication (FFF) of magnetite-filled PLA using an integrated methodology combining strain gauge sensors, high-resolution infrared thermal imaging, and synchrotron X-ray microtomography. Printing parameters, including nozzle temperature (190–220 °C), build platform temperature (30–100 °C), printing speed (30–60 mm/s), and cooling strategy (fan on/off) were systematically varied to evaluate their influence. Results reveal steep thermal gradients along the build direction (up to −1 °C/µm), residual strain magnitudes reaching 0.1 µε, and enhanced viscoelastic creep at elevated platform temperatures. The addition of magnetic particles modifies heat distribution and strain evolution, leading to strong sensitivity to process conditions. These findings provide valuable insight into the complex thermo-mechanical interactions governing the structural integrity of magnetically functionalized PLA composites in additive manufacturing. Full article

One type of pore fundamental to water dynamics is the intra-aggregate pore, which holds water vital for plant and root system development, mainly in finer-textured soils such as clays. The distribution of intra-aggregate pores also influences the redistribution of water. Thus, it is important to study the dynamics of the intra-aggregate pore network under processes such as wetting and drying cycles (WDC). Changes in these pore types can play essential roles in organic matter protection, water movement, microbial activity, and aggregate stability. To date, there are few studies analyzing the impact of WDC on intra-aggregate pore dynamics. This study aims to provide results in this regard, analyzing changes in the pore architecture of a subtropical Oxisol under no-tillage (NT), conventional tillage (CT), and forest (F) after WDC application. Three-dimensional X-Ray microtomography images of soil aggregate samples (2–4 mm) subjected to 0 and 12 WDC were analyzed. The results showed that WDC did not affect (p > 0.05) the imaged porosity, number of pores, fractal dimension, tortuosity, and pore connectivity for the different soil management types. To analyze the permeability and hydraulic conductivity of the soil pore system, the most voluminous pore (MVP) was examined. No differences were observed in the imaged porosity, fraction of aggregate occupied by the MVP, connectivity, tortuosity, hydraulic radius, permeability, and hydraulic conductivity between 0 and 12 WDC for the MVP. Comparing soil management types after 12 WDCs, for example, F samples became more porous than CT and NT samples. In contrast, the pore system of NT had a lower fractal dimension and was more tortuous than that of CT and F samples. Our results show that for highly weathered soils such as the Brazilian Oxisol studied, the intra-aggregate pore network proved resistant to changes with WDC, regardless of the type of management adopted. Full article

This study presents a multi-analytical investigation of the wooden components from Khufu’s Second Solar Boat, one of the valuable archaeological discoveries in ancient Egypt. The research integrates advanced imaging and analytical techniques to identify wood species, assess deterioration patterns, and characterize the fungal and bacterial biodeteriogens. The initial visual examination documented the state of preservation at the time of discovery. Subsequently, the identification of the wood species was carried out. The deterioration status was assessed using a variety of tools, including scanning electron microscopy (SEM) and high-resolution synchrotron radiation computed microtomography (SR-μCT) for morphological alterations, X-ray diffraction (XRD) for crystallinity changes and Fourier-transform infrared spectroscopy (FTIR) to assess chemical degradation indexes of wood. Moreover, molecular techniques were used to identify and characterize the presence of biodeterioration agents. Results indicate that ancient craftsmen used cedar wood for the boat construction. The analysed samples exhibited advanced biotic and abiotic degradation, as evidenced by microbiological assessments, XRD measurements of cellulose crystallinity, FTIR indices, SEM micrographs and SR-μCT data. These results provide crucial insights into the long-term degradation processes of archaeological wood in arid environments, enhancing our understanding of ancient Egyptian woodworking practices and informing future conservation strategies for similar artifacts. Full article

The in situ study of fractal microstructure in nanocarbon polymers is an actual task for their application and for the improvement in their functional properties. This article presents a visualization of the bulk structural features of the composites using pulsed acoustic microscopy and synchrotron X-ray microtomography. This article presents details of fractal structure formation using carbon particles of different sizes and shapes—exfoliated graphite, carbon platelets and nanotubes. Individual structural elements of the composite, i.e., conglomerations of the particles in the air capsule as well as their distribution in the composite volume, were observed at the micro- and nanoscale. We have considered the influence of particle architecture on the fractal formation and elastic properties of the composite. Acoustic and X-ray imaging results were compared to validate the carbon agglomeration. Full article

This work emphasizes an innovative approach utilizing 3D imaging technology based on synchrotron radiation to assess the microstructure of second-phase iron particles and the porous structure within 3D-printed PLA/magnetic iron composites at different printing angles. The study examines how these observations relate to the material’s ductility when processed using fused filament fabrication. In particular, this study examines the impact of one processing parameter, specifically the printing angle, on the microstructure and mechanical behaviour of a polylactic acid (PLA)–iron (PLI) composite designed for magnetic actuation. Fused filament fabrication is employed to produce PLI tensile specimens, with varied printing angles to create different layups. X-ray microtomography is utilized to analyse the microstructure, while tensile mechanical properties are evaluated for all composites, with findings discussed in relation to printing angle conditions. Scanning Electron Microscopy is used to examine the fractography of broken specimens. Results indicate that the printing angle significantly influences the tensile properties and mechanical anisotropy of 3D-printed PLI composites, with an optimal 45°/45° layup enhancing tensile performance. These findings suggest that 3D-printed PLI composites offer a cost-efficient means of producing bio-sourced, light-adaptive materials with intricate magnetic actuation capabilities. By quantifying the modulation of mechanical properties based on printing parameters that influence microstructural arrangement, the research sheds light on a novel aspect of composite material characterization. Full article

Phase-contrast X-ray imaging is becoming increasingly considered since its first applications, which occurred almost 30 years ago. Particular emphasis was placed on studies that use this technique to investigate soft tissues, which cannot otherwise be investigated at a high resolution and in a three-dimensional manner, using conventional absorption-based settings. Indeed, its consistency and discrimination power in low absorbing samples, unified to being a not destructive analysis, are pushing interests on its utilization from researchers of different specializations, from botany, through zoology, to human physio-pathology research. In this regard, a challenging method for 3D imaging and quantitative analysis of collagenous tissues has spread in recent years: it is based on the unique characteristics of synchrotron radiation phase-contrast microTomography (PhC-microCT). In this review, the focus has been placed on the research based on the exploitation of synchrotron PhC-microCT for the investigation of collagenous tissue physio-pathologies from solely human samples. Collagen tissues’ elasto-mechanic role bonds it to the morphology of the site it is extracted from, which could weaken the results coming from animal experimentations. Encouraging outcomes proved this technique to be suitable to access and quantify human collagenous tissues and persuaded different researchers to approach it. A brief mention was also dedicated to the results obtained on collagenous tissues using new and promising high-resolution phase-contrast tomographic laboratory-based setups, which will certainly represent the real step forward in the diffusion of this relatively young imaging technique. Full article

Solid dosage forms such as tablets are extensively used in drug administration for their simplicity and large-scale manufacturing capabilities. High-resolution X-ray tomography is one of the most valuable non-destructive techniques to investigate the internal structure of the tablets for drug product development as well as for a cost effective production process. In this work, we review the recent developments in high-resolution X-ray microtomography and its application towards different tablet characterizations. The increased availability of powerful laboratory instrumentation, as well as the advent of high brilliance and coherent 3rd generation synchrotron light sources, combined with advanced data processing techniques, are driving the application of X-ray microtomography forward as an indispensable tool in the pharmaceutical industry. Full article

Mayaro virus (MAYV) is an emerging arthropod-borne virus endemic in Latin America and the causative agent of arthritogenic febrile disease. Mayaro fever is poorly understood; thus, we established an in vivo model of infection in susceptible type-I interferon receptor-deficient mice (IFNAR−/−) to characterize the disease. MAYV inoculations in the hind paws of IFNAR−/− mice result in visible paw inflammation, evolve into a disseminated infection and involve the activation of immune responses and inflammation. The histological analysis of inflamed paws indicated edema at the dermis and between muscle fibers and ligaments. Paw edema affected multiple tissues and was associated with MAYV replication, the local production of CXCL1 and the recruitment of granulocytes and mononuclear leukocytes to muscle. We developed a semi-automated X-ray microtomography method to visualize both soft tissue and bone, allowing for the quantification of MAYV-induced paw edema in 3D with a voxel size of 69 µm³. The results confirmed early edema onset and spreading through multiple tissues in inoculated paws. In conclusion, we detailed features of MAYV-induced systemic disease and the manifestation of paw edema in a mouse model extensively used to study infection with alphaviruses. The participation of lymphocytes and neutrophils and expression of CXCL1 are key features in both systemic and local manifestations of MAYV disease. Full article

Wheat (Triticum aestivum L.) is one of the most important crops as it provides 20% of calories and proteins to the human population. To overcome the increasing demand in wheat grain production, there is a need for a higher grain yield, and this can be achieved in particular through an increase in the grain weight. Moreover, grain shape is an important trait regarding the milling performance. Both the final grain weight and shape would benefit from a comprehensive knowledge of the morphological and anatomical determinism of wheat grain growth. Synchrotron-based phase-contrast X-ray microtomography (X-ray µCT) was used to study the 3D anatomy of the growing wheat grain during the first developmental stages. Coupled with 3D reconstruction, this method revealed changes in the grain shape and new cellular features. The study focused on a particular tissue, the pericarp, which has been hypothesized to be involved in the control of grain development. We showed considerable spatio-temporal diversity in cell shape and orientations, and in tissue porosity associated with stomata detection. These results highlight the growth-related features rarely studied in cereal grains, which may contribute significantly to the final grain weight and shape. Full article

An improved understanding of an ovary’s structures is highly desirable to support advances in folliculogenesis knowledge and reproductive medicine, with particular attention to fertility preservation options for prepubertal girls with malignant tumors. Although currently the golden standard for structural analysis is provided by combining histological sections, staining, and visible 2D microscopic inspection, synchrotron radiation phase-contrast microtomography is becoming a new challenge for three-dimensional studies at micrometric resolution. To this aim, the proper use of contrast agents can improve the visualization of internal structures in ovary tissues, which normally present a low radiopacity. In this study, we report a comparison of four staining protocols, based on iodine or tungsten containing agents, applied to bovine ovarian tissues fixed in Bouin’s solution. The microtomography (microCT) analyses at two synchrotron facilities under different set-ups were performed at different energies in order to maximize the image contrast. While tungsten-based agents allow large structures to be well identified, Iodine ones better highlight smaller features, especially when acquired above the K-edge energy of the specific metal. Further scans performed at lower energy where the setup was optimized for overall quality and sensitivity from phase-contrast still provided highly resolved visualization of follicular and intrafollicular structures at different maturation stages, independent of the staining protocol. The analyses were complemented by X-ray Fluorescence mapping on 2D sections, showing that the tungsten-based agent has a higher penetration in this type of tissues. Full article