Synchrotron X-ray Microtomography Research Articles

Studies of Fractal Microstructure in Nanocarbon Polymer Composites

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.

High Throughput Automated Characterization of Enamel Microstructure using Synchrotron Tomography and Optical Flow Imaging

The remarkable damage-tolerance of enamel has been attributed to its hierarchical microstructure and the organized bands of decussated rods. A thorough characterization of the microscale rod evolution within the enamel is needed to elucidate this complex structure. While prior efforts in this area have made use of single particle tracking to track a single rod evolution to various degrees of success, such a process can be both computationally and labor intensive, limited to the evolution path of a single rod, and is therefore prone to error from potentially tracking outliers. Particle image velocimetry (PIV) is a well-established algorithm to derive field information from image sequences for processes that are time-dependent, such as fluid flows and structural deformation. In this work, we demonstrate the use of PIV in extracting the full-field microstructural distribution of rods within the enamel. Enamel samples from a wild African lion were analyzed using high-energy synchrotron X-ray micro-tomography. Results from the PIV analysis provide sufficient full-field information to reconstruct the growth of individual rods that can potentially enable rapid analysis of complex microstructures from high resolution synchrotron datasets. Such information can serve as a template for designing damage-tolerant bioinspired structures for advanced manufacturing. Statement of SignificanceThorough characterization and analysis of biological microstructures (viz. dental enamel) allows us to understand the basis of their excellent mechanical properties. Prior efforts have successfully replicated these microstructures via single particle tracking, but the process is computationally and labor intensive. In this work, optical flow imaging algorithms were used to extract full-field microstructural distribution of enamel rods from synchrotron X-ray computed tomography datasets, and a field method was used to reconstruct the growth of individual rods. Such high throughput information allows for the rapid production/prototyping and advanced manufacturing of damage-tolerant bioinspired structures for specific engineering applications. Furthermore, the algorithms used herein are freely available and open source to broaden the availability of the proposed workflow to the general scientific community.

Multi-Scale Cu-Cr Composites Using Elemental Powder Blending in Laser Powder-Bed Fusion

Cu-Cr-based alloys are good candidates for thermo-electrical applications because of their excellent combination of mechanical, thermal, and electrical properties. However, tailoring their microstructure via traditional processes such as sintering and casting remains a challenging task. Herein, we introduce a strategy to fabricate multiscale Cu-25Cr composites. This is achieved through in-situ alloying from elemental powder blending in laser powder-bed fusion. The process is monitored layer-by-layer using synchrotron X-ray microtomography. We show that by changing the melt-pool size and its overlap, one can produce multiscale Cu-Cr composites with coarse (∼50µm) and fine Cr-spheroids (<500 nm) while controlling their spatial distribution. Coarse Cr particles are preferentially located at the melt pool boundaries while fine spherical Cr particles are distributed in the melt pool interior. Spatial variations in mechanical properties are revealed using nanoindentation mapping. This strategy opens new opportunities to optimize multiscale metal matrix composite through the manipulation of the scanning strategy.

Oxygen Vacancy and Bandgap Simultaneous Modulation to Achieve High Lithiophilicity and Mechanical Strength of Lithium Metal Anodes.

Metal oxides with conversion and alloying mechanisms are more competitive in suppressing lithium dendrites. However, it is difficult to simultaneously regulate the conversion and alloying reactions. Herein, conversion and alloying reactions are regulated by modulation of the zinc oxide bandgap and oxygen vacancies. State-of-the-art advanced characterization techniques from a microcosmic to a macrocosmic viewpoint, including neutron diffraction, synchrotron X-ray absorption spectroscopy, synchrotron X-ray microtomography, nanoindentation, and ultrasonic C-scan demonstrated the electrochemical gain benefit from plentiful oxygen vacancies and low bandgaps due to doping strategies. In addition, high mechanical strength 3D morphology and abundant mesopores assist in the uniform distribution of lithium ions. Consequently, the best-performed ZnO-2 offers impressive electrochemical properties, including symmetric Li cells with 2000h and full cells with 81% capacity retention after 600 cycles. In addition to providing a promising strategy for improving the lithiophilicity and mechanical strength of metal oxide anodes, this work also sheds light on lithium metal batteries for practical applications.

The hidden world of fossil larvae: description and morphological insights of an immature scorpionfly (Mecoptera: Panorpidae) from the Baltic amber

Abstract So far, there has been no information of the pre-imaginal stages in the well-preserved fossil record of the Mecoptera. The first and well-preserved mecopteran larva was discovered in Eocene Baltic amber. The application of synchrotron X-ray microtomography enabled the reconstruction of the body structure with high accuracy, providing a comprehensive set of morphological data that classical stereoscopic microscopy could not capture. The larva is eruciform, with distinct segmentation of the body. All the most important morphological structures are documented, including the chaetotaxy system. Shape of antenna and annulated processes on the abdominal segments point to the third/four stage of development. There is no doubt that the larva belongs to Panorpidae, the most abundant family of extant Mecoptera. The morphological characters point to the closest affinity to larvae of Cerapanorpa and Panorpa but the fossil larva cannot be assigned to any extant genus of Panorpidae. Based on the results of synchrotron X-ray microtomography, it is possible to discuss the assignement of this larva to a lower systematic level than the family, and draw conclusions about the nature of the habitat preferences of Eocene panorpid.

The pore structure and water absorption in Portland/slag blended hardened cement paste determined by synchrotron X-ray microtomography and neutron radiography.

The pore structures of hardened Portland/slag cement pastes (>75 wt% slag content), and the initial capillary absorption of moisture through these pores, were monitored using ex situ synchrotron X-ray computerised microtomography and in situ quantitative neutron radiography. The pore structure becomes more constricted as the cement hydrates and its microstructure develops. This mechanism was effective even at a slag content as high as 90 wt% in the cementitious blend, where the lowest total porosity and a significant pore refinement were identified at extended curing ages (360 d). By combining this information with neutron radiographic imaging, and directly quantifying both depth and mass of water uptake, it was observed that 90 wt% slag cement outperformed the 75 wt% slag blend at 90 days in terms of resistance to capillary water uptake, although the higher-slag blend had not yet developed such a refined microstructure at 28 days of curing. The assumptions associated with the "sharp front model" for water ingress do not hold true for highly substituted slag cement pastes. Testing transport properties at 28 days may not give a true indication of the performance of these materials in service in the long term.

4D structural changes and pore network model of biomass during pyrolysis

Biochar is an engineered carbon-rich substance used for soil improvement, environmental management, and other diverse applications. To date, the understanding of how biomass affects biochar microstructure has been limited due to the complexity of analysis involved in tracing the changes in the physical structure of biomass as it undergoes thermochemical conversion. In this study, we used synchrotron x-ray micro-tomography to visualize changes in the internal structure of biochar from diverse feedstock (miscanthus straw pellets, wheat straw pellets, oilseed rape straw pellets, and rice husk) during pyrolysis by collecting a sequence of 3D scans at 50 °C intervals during progressive heating from 50 °C to 800 °C. The results show a strong dependence of biochar porosity on feedstock as well as pyrolysis temperature, with observed porosity in the range of 7.41–60.56%. Our results show that the porosity, total surface area, pore volume, and equivalent diameter of the largest pore increases with increasing pyrolysis temperature up to about 550 °C. The most dramatic development of pore structure occurred in the temperature range of 350–450 °C. This understanding is pivotal for optimizing biochar’s properties for specific applications in soil improvement, environmental management, and beyond. By elucidating the nuanced variations in biochar’s physical characteristics across different production temperatures and feedstocks, this research advances the practical application of biochar, offering significant benefits in agricultural, environmental, and engineering contexts.

In situ observations of the damage behavior of the metastable β‐titanium alloy Ti5321 using synchrotron X-ray microtomography

In situ X-ray synchrotron microtomography was used to quantify the evolution of damage in the titanium alloy Ti5321 with bimodal microstructure. The results show that voids nucleate in the equiaxed primary α grains and α plates or at α/β interfaces. There exists an approximate linear relationship between volume of voids and local strain of several largest voids. The low growth rate and delay of coalescence of voids are attributed to the dispersed distribution of the α phase in the bimodal microstructure. There are no micro-cracks formed in the interior of the sample until fracture. The deep dimples in the fracture surface indicate ductile fracture. The damage mechanism of Ti5321 is discussed with the help of post-mortem SEM. To clarify the difference in damage mechanism between metastable β and α + β titanium alloys, Ti64 is also in situ tensile tested.

Deconsolidation of carbon fiber-reinforced PEKK laminates: 3D real-time in situ observation with synchrotron X-ray microtomography

Deconsolidation of carbon-fiber reinforced thermoplastic laminate occurs while (pre)heating the materials during their forming processes. Pores nucleate, grow and lead to degradations of mechanical properties. Here, a new experimental device was developed and installed inside a synchrotron beamline (dedicated to fast X-ray microtomography). Pore nucleation and growth was observed in 3D, real-time and in situ while heating Carbon/PEKK laminate samples. The time evolution of sample deconsolidation strain, porosity, as well as number, size and morphology of pores was assessed. Nucleation and growth is observed above the glass transition temperature and enhanced with initial moisture content. Drastic deconsolidation when approaching melting temperature is thought to be driven by internal stress in the laminate. The data provided may be used as input for modeling purposes or for validation of existing models.

Elucidating links between the mechanical performance of flax fibres and their structural defects

Single flax fibres develop morphological deformations, called kink-bands, which are considered to be areas of weakness. The correlation between the occurrence of kink-bands, fibre extraction method and fibre mechanical properties still needs to be clarified. To this end, an extensive multi-scale statistical study was conducted on 96 elementary fibres extracted from four distinct batches processed with different scutching and combing conditions. First, kink-bands were observed and quantified through polarized light microscopy (PLM), scanning electron microscopy (SEM) and synchrotron X-ray microtomography. PLM quantification demonstrated that uncombed fibres have more cortical residues and larger surface kink-bands with many small internal porosities. Then, the mechanical characteristics of each PLM-quantified single fibre were measured by tensile tests. A larger number of kink-bands was observed for the most intensively combed batch, 18.2 kink-bands/mm, as well as a surprisingly low average kink-band area, of the order of 158 µm² per kink-band. In addition, the same batch had a higher tensile strength and modulus than the other three batches with a negative Stearman correlation of − 0.64 and − 0.78 with the proportion of defects, respectively. Finally, 74% of the fibres in this intensively combed batch, had a ‘Type I’ linear elastic behaviour, highlighting a significant change of behaviour in comparison to the uncombed batch, attributed to local reorientation and pre-stretching. The results suggest that changes in kink-bands structure are principally responsible for these evolutions; due to both new distribution of pores in kink-bands regions and reduction in kink-band size possibly induced by local cellulose realignment.

Early developmental stages of a Lower Ordovician marrellid from Morocco suggest simple ontogenetic niche differentiation in early euarthropods

Early developmental stages of euarthropods are exceptionally rare in the fossil record. This hampers our understanding of the biology, phylogeny, and development of this extremely diverse metazoan group. Herein, we use classical paleontological methods in combination with synchrotron X-ray microtomography to explore the morphology in ca. 480 million-year-old early developmental stages of the Lower Ordovician Fezouata Shale marrellid euarthropod. These stages range between 3.8 and 5.3 mm in length and are characterized by three distinct pairs of gently curved spines that projects from the head shield. The first pair of cephalic appendages are represented by uniramous antenullae of a sensory function. The second pair of cephalic appendages is robust, and had an anchoring or stabilizing function. The third cephalic appendage pair is composed of long cylindrical podomeres and was used for walking. The trunk appendages are biramous and consist of an endopod and a lamellate exopod. Two anterior trunk endopods are composed of long slender podomeres and were used for walking, while the more posterior trunk endopods bear robust endites and associated setae and were used for food gathering. The trunk of the earliest developmental stages is composed of thirteen segments, in contrast to more than 22 segments in the adult trunk. The similar appendage morphology and differentiation along the body is evident in adult individuals of the Fezouata marrellid, suggesting these different developmental stages shared similar methods of locomotion and food processing. Given that adults and juveniles are often preserved in the same or nearby sites, the niche differentiation between these life stages would be the result of the absolute smaller appendage size in immature stages compared to larger adults, effectively differentiating the size of food resources consumed by each. In addition, the delicate setae present in the posterior trunk appendages of early developmental stages might have been used to capture smaller food particles. This simple mode of ontogenetic niche differentiation might have been common in the early diverging euarthropod groups.

Structure-aware guided filtering for a ring artifact correction in synchrotron x-ray microtomography.

Synchrotron-based x-ray microtomography (S-µCT) is a powerful non-invasive three-dimensional (3D) imaging technique used for visualizing the internal structure of objects with micron-scale spatial resolution. However, in practical applications, ring artifacts often occur in S-µCT, which significantly degrades image quality and hinders interpretation. In this study, we propose a ring artifact correction method based on guided image filtering (GIF). The method first extracts structural prior from the input S-µCT images and then uses it as the guidance image to correct the ring artifacts. Finally, GIF with a self-guidance image is employed to further enhance image quality. Extensive comparisons and analyses on simulations and real data experiments demonstrate that the proposed method is capable of effectively correcting ring artifacts, accompanied by low-dose noise suppression and sparse-view artifact reduction. These findings suggest that the proposed method has great potential to promote the wider applications of S-µCT in the future.

The damage mechanism of the metastable β-titanium alloy Ti5321 with specific microtexture using synchrotron X-ray microtomography

In order to investigate damage mechanism of metastable β-titanium alloy Ti5321 with bimodal microstructure and specific microtexture, in situ tensile test was performed facilitating with synchrotron X-ray microtomography. The damage evolution of metastable β-titanium alloy Ti5321 can be predicted in three dimensions by proper micromechanics-based modelling methods, the Rice and Tracey model and Huang model. Through comparisons of the Rice and Tracey model and Huang model validated using the values of stress triaxiality calculated from experimental data and Finite Element (FE) simulations, the prediction accuracy of growth rates of voids can be enhanced. The results also show that the void growth is strongly related to microtexture of α plates. It is found that the growth path of largest voids is along α plates which have their c-axes with similar inclination angle of ∼45° from rolling direction (RD). Electron backscatter diffraction (EBSD) was also used to reveal the damage mechanism. This result is important enlightenment for study of damage mechanism of metastable β-titanium alloys.

Structural formation during bread baking in a combined microwave-convective oven determined by sub-second in-situ synchrotron X-ray microtomography

A new concept has been developed for characterizing the real-time evolution of the three-dimensional pore and lamella microstructure of bread during baking using synchrotron X-ray microtomography (SRµCT). A commercial, combined microwave-convective oven was modified and installed at the TOMCAT synchrotron tomography beamline at the Swiss Light Source (SLS), to capture the 3D dough-to-bread structural development in-situ at the micrometer scale with an acquisition time of 400 ms. This allowed characterization and quantitative comparison of three baking technologies: (1) convective heating, (2) microwave heating, and (3) a combination of convective and microwave heating. A workflow for automatic batchwise image processing and analysis of 3D bread structures (1530 analyzed volumes in total) was established for porosity, individual pore volume, elongation, coordination number and local wall thickness, which allowed for evaluation of the impact of baking technology on the bread structure evolution. The results showed that the porosity, mean pore volume and mean coordination number increase with time and that the mean local cell wall thickness decreases with time. Small and more isolated pores are connecting with larger and already more connected pores as function of time. Clear dependencies are established during the whole baking process between the mean pore volume and porosity, and between the mean local wall thickness and the mean coordination number. This technique opens new opportunities for understanding the mechanisms governing the structural changes during baking and discern the parameters controlling the final bread quality.

4D imaging and quantification of the effect of a Phosphate-Based treatment on building materials by means of synchrotron X-ray Microtomography: New insights into the dynamic of the consolidation process

Diammonium hydrogen phosphate (DAP) solutions are used as consolidants for carbonate stone materials through the crystallization whithin the original matrix of newly formed crystalline phases. However, the formation mechanism of the new phases within the stone microstructure, and their effects on the porous system, strongly depend on the DAP molarity, the treatment method, and the stone microstructure. In this study, we obtained real-time quantitative information on the structural evolutions induced by the treatment process on the Noto limestone, a porous carbonate stone used as a building stone since antiquity, by synchrotron X-ray Microtomography. With the aid of 4D image analysis, microstructural modifications in terms of porosity, interconnection, and pore size distribution have been demonstrated in different stadia of the consolidation process, and the influence of molarity was asserted. This study paves the way for a deeper understanding of consolidation mechanisms and the effects induced overtime on the 3D microstructural features of porous materials by inorganic treatment.

Christelenkidae, a new extinct family based on a new taxon from Eocene Baltic amber (Diptera: Acalyptratae), with X-ray synchrotron microtomography imaging of its structures

A new family of DipteraAcalyptratae, Christelenkidae Roháček fam. nov., is established for Christelenka multiplex Roháček gen. et sp. nov., an unusual extinct taxon described from a unique male specimen preserved in Baltic amber (Mid-late Eocene, ca 48–34 Ma). Apart from detailed examination by light microscopy and photography, the holotype of the new species has also been studied by means of X-ray synchrotron microtomography with the aim of obtaining additional morphological data for consideration of its relationships. Because of a very peculiar combination of morphological characters, the new family is tentatively considered a separate lineage of Acalyptratae having no apparent sister-group relationship with any of the known families. Its probable relationships to some families of Opomyzoidea and Ephydroidea are discussed.

Examination of embolisms in maple and birch saplings utilising microCT

We demonstrate the application of synchrotron x-ray microtomography (microCT) to non-invasively examine the internal structure of a maple and birch sapling. We show that, through the use of standard image analysis techniques, embolised vessels can be extracted from reconstructed slices of the stem. By combining these thresholded images with connectivity analysis, we map out the embolisms within the sapling in three dimensions and evaluate the size distribution, showing that large embolisms over 0.005mm3 in volume compose the majority of the saplings' total embolised volume. Finally we evaluate the radial distribution of embolisms, showing that in maple fewer embolisms are present towards the cambium, while birch has a more uniform distribution.

Influence of Fe-rich phases and precipitates on the mechanical behaviour of Al-Cu-Mn-Fe-Sc-Zr alloys studied by synchrotron X-ray and neutron

A multiscale methodology using scanning and transmission electron microscope, synchrotron X-ray nano-tomography and micro-tomography, small angle neutron scattering, and in situ synchrotron X-ray diffraction has been used, to reveal the effect of Fe-rich phases and precipitates on the mechanical behaviour of an Al-Cu-Mn-Fe-Sc-Zr alloy. The α-Al grains size is reduced from 185.1 μm (0 MPa) and 114.3 μm (75 MPa) by applied pressure. Moreover, it has been demonstrated that suitable heat treatments modify the 3D morphology of Fe-rich phases from interconnected to a disaggregated structure that improves the mechanical properties of the alloy. The size and morphology evolution of fine precipitates under different ageing temperature and time are revealed. At ageing temperature of 160 °C, the precipitates change from GP zones to θ' (around 75 nm in length) with ageing time increasing from 1 h to 24 h; the Vickers hardness increases from 72.0 HV to 110.7HV. The high ductility of the Sc, Zr modified Al-Cu alloy is related to the complex shape and the loss of interconnectivity of the Fe-rich particles due to the heat treatment. The evolution of the crystal lattice strains in α-Al, and β-Fe calculated during tensile test using in-situ synchrotron X-ray diffraction corroborates the influence of the microstructure in the ductility of the modified alloy.

New Cretaceous crickets of the subfamilies Nemobiinae and Podoscirtinae (Orthoptera, Grylloidea: Trigonidiidae, Oecanthidae) attest the antiquity of these clades

AbstractFossils are more and more used in phylogenetic evolutionary studies either for clade calibration, or as terminals in a dataset including morphological characters. The strength of these methodological advances relies however on the quality and completeness of the fossil record. For crickets (Insecta, Orthoptera, Gryllidea), few ancient (pre-Cenozoic) well-preserved fossils are known, except for isolated wings often classified in purely fossil groups and a few fossils found in Cretaceous amber. Here, we present two remarkable fossils from mid-Cretaceous amber of France, that were imaged using X-ray synchrotron microtomography and exhibit an exquisite preservation allowing description with a precision similar to that of extant taxa.Palaeonemobius occidentalisLaurent and Desutter-Grandcolas,gen. nov., sp. nov.andPicogryllus carentonensisJosse and Desutter-Grandcolas,gen. nov., sp. nov.are the oldest representatives of the Nemobiinae and Podoscirtinae subfamilies of the Trigonidiidae and Oecanthidae families respectively.P. carentonensisJosse and Desutter-Grandcolas,gen. nov., sp. nov.is also the smallest adult male with a full stridulatory apparatus ever documented in crickets (body length 3.3 mm), and the first taxon of the cricket clade for which male genitalia can be partly described. We discuss the significance of Cretaceous fossils of crickets for future evolutionary studies of this clade.

Spherical alveolar shapes in live mouse lungs

Understanding how the alveolar mechanics work in live lungs is essential for comprehending how the lung behaves during breathing. Due to the lack of appropriate imaging tools, previous research has suggested that alveolar morphologies are polyhedral rather than spherical based on a 2D examination of alveoli in fixed lungs. Here, we directly observe high-resolution 3D alveoli in live mice lungs utilizing synchrotron x-ray microtomography to show spherical alveolar morphologies from the live lungs. Our measurements from x-ray microtomography show high sphericity, low packing density, big alveolar size, and low osmotic pressure, indicating that spherical alveolar morphologies are natural in living lungs. The alveolar packing fraction is quite low in live lungs, where the spherical alveoli would behave like free bubbles, while the confinement of alveolar clusters in fixed lungs would lead to significant morphological deformations of the alveoli appearing polyhedral. Direct observations of the spherical alveolar shapes will help understand and treat lung disease and ventilation.