High-resolution Micro-computed Tomography Research Articles

(Energy Technology Division Graduate Student Award sponsored by BioLogic) In-Situ, Non-Destructive, 3D Neutron Imaging of Lithium Plating Following Extreme Fast-Charging of Full-Cell Lithium-Ion Batteries

One of the primary challenges impeding extreme fast-charging (XFC) of current lithium-ion batteries (LIBs) for electric vehicles (EVs) within 10–15 minutes is the deposition of Li metal on graphite known as “Li plating”.1-2 After Li plates, it either re-intercalates into the graphite electrode or is stripped off during battery discharging to form “active Li”or becomes electronically disconnected resulting in “dead Li.” Previous studies have indicated that dead Li is the main contributor to the XFC-related capacity loss of LIBs. However, mechanistic understanding of the 3D morphological behavior and spatial heterogeneities of dead Li; and how they differ from those of plated and active Li during the XFC is not well understood.3-4 Here, we present an in-situ, non-destructive 3D characterization of the morphological behavior and spatial heterogeneities of plated, dead, and active Li on graphite electrodes in full-cell LIBs using high-resolution neutron micro-computed tomography. We performed neutron µCT5 (pixel size: ~ 5.74 µm; effective spatial resolution: ~10-15 µm) at the ICON beamline6 at the Swiss Spallation Neutron Source at the Paul Scherrer Institute. We imaged two batteries in the charged and discharged states: (1) after 4 cycles of 1C charging and (2) after 6 cycles of 6C charging.Our results show that Li plates at and around the edges of the graphite electrodes, indicating that graphite edges and the areas around these edges are the most susceptible to Li plating. However, certain edges and areas around these edges formed dead Li whereas others formed active Li, suggesting 3D spatial heterogeneities in the formation of dead and active Li at both 1C and 6C. Mainly, we discuss these heterogeneities at four regions: (1) near the Cu CC, (2) in the middle of the graphite electrode, (3) near the graphite-separator interface, and (4) in the separator. Specifically, we found that Li near the Cu CC remains active whereas most of the plated Li at the graphite-separator interface and in the separator becomes dead at both 1C and 6C.Morphologically, we observed porous nature of plated and dead Li at both 1C and 6C. Our 3D visualizations noticeably show nodules of varying densities of metallic Li. However, we observed different 3D behavior of Li plating at 1C and 6C. For example, tip-like Li deposits were seen laterally closer to the center of the graphite electrode, near the graphite-separator interface, and into the separator at 6C. In contrast, at 1C, no tip-like Li deposits were observed near the graphite-separator interface and into the separator. Based on our findings, we concluded that higher XFC-charging rate and cycling number (6 cycles of 6C charging) cause the formation of tip-like Li deposits as compared to the relatively slower XFC-charging rate and cycling number (4 cycles of 1C charging). We believe that insights derived from this work will guide the design of thick graphite electrodes with minimized-plating for fast-charged EVs.

Integrating μCT imaging of core plugs and transfer learning for automated reservoir rock characterization and tomofacies identification

Traditional methods of core characterization are time-consuming and require the considerable effort of a large number of experts. At the same time, it is quite difficult to readily detect small but important elements in reservoir rocks, especially inside the core volume, that can have a strong impact on assessing reservoir potential and hydrodynamic properties. This research explores the integration of high-resolution micro-computed tomography (μCT) imaging and transfer learning for the automated characterization of reservoir rocks and tomofacies identification. The study involved collecting and marking a dataset containing 66,560 μCT images of 130 standard core plugs containing all major reservoir rock types. Using this dataset of 2D μCT images of core plugs, we applied convolutional neural networks (CNNs) pre-trained on ImageNet and fine-tuned them for rock classification tasks. Applying a transfer learning approach, we trained seven ResNet-50 models, which were able to identify and classify reservoir rock features in μCT images. These features included basic characteristics such as rock type, general texture, the presence of fractures and sulfidization that are common for all reservoir rocks. Further, depending on a specific rock type, individual features such as grain size, individual sedimentological texture and the presence of organic matter zones in the sample could be determined by the specialized model. The results show an average classification accuracy of over 94%, indicating the effectiveness of transfer learning in enhancing rock characterization. The obtained models demonstrated high validation rates and were organized into a workflow for automated rock feature characterization. A case study conducted on a carbonate core from a real oilfield provided a practical demonstration of the automated system's work, whose predictions were validated by traditional analyses such as X-ray diffraction and thin-section petrography. The produced models demonstrated the ability for rapid detection of subtle details that might otherwise have been missed during manual inspection. In addition, the concept of tomofacies resulting from the integration of μCT images and machine learning predictions has proven useful in highlighting different reservoir zones, allowing us to understand their heterogeneity and the ability to separate rock sections despite their apparent monotony. These findings suggest that the integration of μCT imaging and transfer learning is a promising approach for improving the automation and accuracy of reservoir rock characterization. The developed technique represents a significant advance in reservoir characterization, offering rapid and accurate identification of rock properties that can improve exploration and development strategies.

High-Resolution Iodine-Enhanced Micro-Computed Tomography of Intact Human Hearts for Detailed Coronary Microvasculature Analyses.

Identifying the detailed anatomies of the coronary microvasculature remains an area of research; one needs to develop methods for non-destructive, high-resolution, three-dimensional imaging of these vessels for computational modeling. Currently employed Micro-Computed Tomography (Micro-CT) protocols for vasa vasorum analyses require organ dissection and, in most cases, non-clearable contrast agents. Here, we describe a method developed for a non-destructive, economical means to achieve high-resolution images of the human coronary microvasculature without organ dissection. Formalin-fixed human hearts were cannulated using venogram balloon catheters, which were then fixed into the specimen's aortic root. The canulated hearts, protected by a polyethylene bag, were placed in radiolucent containers filled with insulating polyurethane foam to reduce movement. For vasculature staining, iodine potassium iodide (IKI, Lugol's solution; 6.3% Potassium Iodide, 4.1% Iodide) was injected. Contrast distributions were monitored using a North Star Imaging X3000 micro-CT scanner with low-radiation settings, followed by high-radiation scanning (3600 rad, 60 kV, 900 mA) for the final high-resolution imaging. We successfully imaged four intact human hearts presenting with chronic total coronary occlusions of the right coronary artery. This imaging enabled detailed analyses of the vasa vasorum surrounding stenosed and occluded segments. After imaging, the hearts were cleared of iodine and excess polyurethane foam and returned to their initial formalin-fixed state for indefinite storage. Conclusions: the described methodologies allow for the non-destructive, high-resolution micro-CT imaging of coronary microvasculature in intact human hearts, paving the way for detailed computational 3D microvascular reconstructions with a macrovascular context.

High-resolution three-dimensional micro-computed tomography assessment of micro-architectural patterns in non-adults with cribra orbitalia: Correlation between macro- and micro-scale bone features.

Skeletal porous lesions such as cribra orbitalia (CO) have long been of interest to bioanthropologists worldwide, mainly due to their high prevalence in osteological material. Previous studies considered CO as an external morphological manifestation, and therefore, research has mainly focused on visible (macroscopic) CO patterns. However, the understanding of CO-induced micro-scale bone changes is still scarce. Therefore, we performed high-resolution micro-computed tomography imaging to investigate three-dimensional CO-induced micro-architectural patterns in non-adults, with a particular focus on the correlation between macroscopic and micro-architectural orbital features. Cortical and trabecular micro-architectural changes in the orbital roof were analyzed in non-adults younger than 15 years, using orbital roof samples with and without macroscopic traces of CO (n = 28). A widely accepted five-grade macroscopic CO scoring system was applied to analyze CO severity. Areas affected with CO (area 1) and areas without macroscopic CO traces (area 2) were analyzed separately. The conducted high-resolution analysis showed that cortical and trabecular micro-architecture varied with CO presence, lesion severity (CO grade), and the analyzed area. Inter-grade comparisons suggested that most of the analyzed micro-architectural parameters were not significantly different between adjacent CO grades. Based on the micro-architectural evaluation of areas 1 and 2, the porous lesions were much more extensive than revealed by gross examination. In addition, micro-architectural differences were particularly pronounced in younger non-adults. In summary, our pilot study suggests that the macroscopic examination of CO reflects only the tip of the iceberg, as the micro-architectural changes seem to be much larger than macroscopically identified. RESEARCH HIGHLIGHTS: Cribra orbitalia (CO) represents orbital porous lesions. A high-resolution microscopic assessment of CO-induced changes in non-adults was done by micro-computed tomography. The microarchitecture was affected by CO presence, CO grade, area, and age.

Subchondral Bone Osteocyte Lacunae Morphology in End-Stage Osteoarthritis of the Human Tibial Plateau.

Subchondral bone remodeling, mediated by osteocytes within the lacuno-canalicular network, plays a crucial role in osteoarthritis (OA) progression. Following cell death, lacunae preserve integrity, offering insights into bone remodeling mechanisms. Limited and controversial data on osteocyte lacuna morphology in OA result from small sample sizes and two-dimensional (2D) techniques that have been used thus far. This study aimed to quantify three-dimensional (3D) osteocyte lacunar characteristics at well-defined tibial plateau locations, known to be differently affected by OA. Specifically, 11 tibial plateaus were obtained from end-stage knee-OA patients with varus deformity. Each plateau provided one sample from the less affected lateral compartment and two samples from the medial compartment, at minimum and maximum bone volume fraction (BV/TV) locations. High-resolution desktop micro-computed tomography (micro-CT) at 0.7μm voxel resolution imaged the 33 samples. Lacuna number density (Lc.N/BV) and lacuna volume density (Lc.TV/BV) were significantly lower (p < 0.02) in samples from the medial side with maximum BV/TV compared to lateral side samples. In the medial compartment at maximum local BV/TV, mean lacuna volume (Lc.V), total lacuna volume (Lc.TV), and Lc.TV/BV were significantly (p < 0.001) lower than in the region with minimum BV/TV. Lc.N/BV was also significantly lower (p < 0.02) at the maximum local BV/TV location compared to the region with minimum BV/TV. Our findings suggest that subchondral bone lacunae adapt to the changing loads in end-stage OA.

Nondestructive internal disorders detection of ‘Braeburn’ apple fruit by X-ray dark-field imaging and machine learning

'Braeburn' apples are susceptible to internal browning disorders when stored under controlled atmosphere (CA) conditions with unfavorable gas compositions. The progression of CA-related disorders in apple tissues is dynamic, noting a decrease in porosity during early storage due to cellular breakdown and pore flooding, and an increase in porosity in later stages due to structural collapse and cavity formation. Utilizing grating-based X-ray dark-field radiography, which leverages X-ray small-angle scattering to detect microstructural changes below the pixel scale, this study assesses the technique's efficacy in identifying internal disorders in 'Braeburn' apples at both early and later stages. A machine learning approach was applied to compare the diagnostic capabilities of dark-field imaging with those of X-ray absorption radiography at identical image resolutions. Results indicate that for early-stage disordered fruit detection, X-ray dark field radiography is 10 % more accurate than absorption radiography, regardless of the machine learning classifiers that were applied. In the later stage of browning, dark-field imaging performs similarly to absorption imaging. High-resolution micro-computed tomography scans suggested that the distinct detection performance of dark-field imaging may be attributed to the more pronounced microstructural differences between healthy and early-stage defective tissues than those between healthy and later-stage defective tissues. The insights from this work will guide the application of X-ray dark-field systems in fruit quality assurance, particularly in detecting internal disorders.

Abstract 1007: A Novel Heterogeneous Murine Aortic Model Derived From Micro-computed Tomography

Introduction: Strength and structural stability of the aorta primarily comes from collagen that is mostly found in the media layer of the aorta along with elastin. The risk of life-threatening aortic rupture increases in cases of aortic aneurysm diseases due to local deformation and weakening of the aortic wall. How does local structure affect how the aorta responds to stress? We hypothesize that material and geometric heterogeneity affect the local biomechanics of the aortic wall and that the local responses to stress are not necessarily the same as the global response. Our goal is to develop a novel finite element model (FEM) of collagen and elastin behavior in murine aorta derived from high-resolution micro-computed tomography (microCT). This model will allow us to study how the aorta deforms to blood pressure at the local level. Approach: The collagen and elastin from 100 vertical slices of microCT scans of a murine aorta were segmented, smoothed and meshed to create 3D models for FEM and the aortic ring was divided into 8 sections of varying geometry and composition. Local stress-strain relationships were extracted from uniaxial loading conditions. Simulations were conducted where the stiffness of collagen was set equal to (1X) or made stiffer than elastin by a factor of 10 (10X) or 100 (100X). The average Young’s modulus, E, for each section was calculated and used as parameters for FEM of the aortic ring to investigate the global mechanical behavior of the aortic wall. Results/Conclusions: The strains generated in the radial direction are greater than the strains in the hoop direction in each of the 8 heterogeneous sections of the aortic ring. There was significant variability in the E values in the 10X and 100X systems. FEM of a materially uniform aortic ring yielded smaller maximum principal logarithmic strains compared to a ring that was materially heterogeneous. This study provides evidence that local structure and material distribution are important in aortic biomechanics. Pathogenesis of aneurysmal disease is dependent on collagen and elastin turnover. Aneurysm rupture results from mechanical failure: peak wall stress exceeds local tissue strength. This novel method will allow for development of a complex aortic fracture model to study aortic pathologies.

Optimal Intermittent Administration Interval of Abaloparatide for Bone Morphogenetic Protein-Induced Bone Formation in a Rat Spinal Fusion Model.

Both bone morphogenetic protein 2 (BMP-2) and abaloparatide are used to promote bone formation. However, there is no consensus about their optimal administration. We investigated the optimal administration theory for the pairing of BMP-2 and abaloparatide in a rat spinal fusion model. Group I was only implanted in carriers and saline. Carriers with 3 µg of recombinant human BMP-2 (rhBMP-2) were implanted in other groups. Abaloparatide injections were administered three times a week for group III (for a total amount of 120 µg/kg in a week) and six times a week for group IV (for a total amount of 120 µg/kg in a week) after surgery. They were euthanized 8 weeks after the surgery, and we explanted their spines at that time. We assessed them using manual palpation tests, radiography, high-resolution micro-computed tomography (micro-CT), and histological analysis. We also analyzed serum bone metabolism markers. The fusion rate in Groups III and IV was higher than in Group I, referring to the manual palpation tests. Groups III and IV recorded greater radiographic scores than those in Groups I and II, too. Micro-CT analysis showed that Tbs. Sp in Groups III and IV was significantly lower than in Group I. Tb. N in Group IV was significantly higher than in Group I. Serum marker analysis showed that bone formation markers were higher in Groups III and IV than in Group I. On the other hand, bone resorption markers were lower in Group IV than in Group I. A histological analysis showed enhanced trabecular bone osteogenesis in Group IV. Frequent administration of abaloparatide may be suitable for the thickening of trabecular bone structure and the enhancement of osteogenesis in a rat spinal fusion model using BMP-2 in insufficient doses.

Characterisation of pore structure of bulk wheat mixed with dockage using X-ray micro-computed tomography and deep learning

Characterisation of pore structure inside grain bulks is essential for predicting the airflow resistance during grain drying and aeration. Herein, the 3D pore network of wheat mixed with different percentages of canola and dockage was characterised. The characterised parameters include pore size, throat length, coordination number, airpath length, and tortuosity. To simulate the grain storage condition, the loaded wheat mixtures were cured using wax at 110 °C. The images of the waxed wheat mixtures were produced by using a high-resolution X-ray micro-computed tomography (μCT) system at a resolution of 50 μm per pixel. The computed space distribution was based on the 3D medial axis analysis of each image stack using Dragonfly 4.1 software. The pore space was segmented using a deep-learning model with 90.1–98.0% accuracy. A watershed-based image algorithm was used to generate the pore network from the segmented pore space. The pore structure parameters were extracted from the pore network of each wheat mixture. Most pores were classified as mesopores (>99%) in a range from 62.5 to 4000 μm, with less than 1% classified as micropores (1–62.5 μm). The mean pore size of clean bulk wheat was 648 ± 403 μm with a mean throat length of 1115 ± 611 μm. In the mixtures with 10% canola, 5 and 10% wheat dockage, the mean pore size was reduced by 10%, 29%, and 17%, respectively, from clean wheat. Adding canola and dockage generally influenced the connectivity in the pore microstructure with changes in bulk porosity, tortuosity, airpath number, and length.

Investigation of gradient properties for cement mortar interfacial transition zones and their effects on mechanical characteristics using micro-CT

The interfacial transition zone (ITZ) in cement-based composites with aggregates is widely recognized as the most vulnerable component, greatly affecting their physical and mechanical properties. In this study, the effect of the ITZ characteristics on the mechanical behavior of cement mortar using its actual microstructure was investigated with image-based numerical approaches in this study. The volumetric information of the ITZ of the mortar sample was obtained and characterized from high-resolution synchrotron micro-computed tomography (micro-CT) images. The mechanical properties of the mortar were evaluated using the finite element method, based on the components characteristics represented by grayscale information of the micro-CT images. It was found that the adhesion between the aggregates and binder was well replicated in the simulation with the multiple-phase model, based on the gradient characteristics and properties of the ITZ. Considering the ITZ thickness according to the aggregates size, a more realistic crack propagation trend can be observed. The obtained results confirmed the significant influence of the ITZ thickness and phase distribution characteristics on the mechanical properties of cement mortars, emphasizing the importance of considering ITZ phases for accurate material analysis.

Using X-ray computed tomography and pore-scale numerical modeling to study the role of heterogeneous rock surface wettability on hydrogen-brine two-phase flow in underground hydrogen storage

Underground hydrogen storage (UHS) is receiving increasing attention to address the challenges in hydrogen storage. A crucial aspect of UHS is understanding the transport of hydrogen in subsurface porous media. In this work, hydrogen core flooding experiments were conducted in a sandstone sample and then the pore-scale distribution of hydrogen and brine was visualized using high-resolution X-ray micro-computed tomography (micro-CT). After CT image processing, we measured the surface contact angles (CAs) on rock surfaces and found that the measured CAs followed a log-normal distribution. To investigate the influence of rock surface wettability on the transport properties in the hydrogen-brine-sandstone system, the lattice Boltzmann (LB) method was used to simulate two-phase flows with different surface CA distributions; hydrogen-brine relative permeability and capillary pressure curves through the primary drainage, imbibition, and secondary drainage processes were obtained by LB simulations. X-ray CT scanning showed that hydrogen resided in both large pores and small pores and pore throats after the primary drainage process (i.e., hydrogen displacing brine), whereas after the imbibition process (i.e., brine displacing hydrogen) hydrogen stayed primarily in large pores where the capillary pressure barriers were low. The LB two-phase flow modeling illustrated that water’s relative permeability increased whereas hydrogen’s relative permeability decreased when the core flooding moved from primary drainage to imbibition; in contrast, when the core flooding moved from imbibition to secondary drainage, water’s relative permeability decreased whereas hydrogen’s relative permeability increased. Decreasing the surface CA increased the capillary pressure and reduced the hydrogen residual rate, which indicates high hydrogen retrievability and thus is favorable for UHS practice. The change in CA’s standard deviation did not cause noticeable changes in water’s relative permeability curves, whereas it resulted in noticeable changes in hydrogen’s relative permeability curves. This work is the first study that utilizes X-ray micro-CT scanning and pore-scale multiphase flow modeling to quantitatively and comprehensively investigate hydrogen-brine two-phase flow properties under different rock surface wettability distributions. The research findings from this study will advance the understanding of hydrogen transport in an underground storage system and provide essential data for large-scale field studies in UHS.

Low-velocity impact responses of UHMWPE fiber/epoxy laminates with plasma treatment and polypyrrole grafting

The physical–chemical method with plasma treatment and polypyrrole grafting was used to improve the low velocity impact resistance of the ultra-high molecular weight polyethylene (UHMWPE) fiber/epoxy laminates. The experimental impact force–time curves and impact force-central displacement curves were recorded. The microscopic void distribution of impact region was quantitatively counted by high-resolution X-ray micro-computed tomography (μCT). Then the residual compressive strengths for the laminates after low velocity impact were explored. Experimental results showed that the impact resistance and residual strength of the laminates treated by the combined plasma treatment and polypyrrole grafting were significantly improved by comparing with the plasma treatment alone, and the void fraction also reduced remarkably. In addition, the impact resistance with single physical plasma treatment method was more affected by the mixture ratio of nitrogen and oxygen.

Influence of microarchitecture on stressed volume and mechanical fatigue behaviour of equine subchondral bone

Fractures of the equine metacarpophalangeal (MCP) joint are among the most common and fatal injuries experienced by racehorses. These bone injuries are a direct result of repetitive, high intensity loading of the skeleton during racing and training and there is consensus that they represent a mechanical fatigue phenomenon. Existing work has found the fatigue life of bone to be strongly determined by bone microarchitecture and the resulting stressed volume (i.e., the volume of bone stressed above assumed yield). The purpose of this study was to quantify the influence of bone microarchitecture on the mechanical fatigue behaviour of equine subchondral bone from the MCP joint across a wide variety of sample types. Forty-eight subchondral bone samples were prepared from the third metacarpal (MC3) and proximal phalanx (P1) of 8 horses and subsequently imaged using high resolution micro-computed tomography (μCT) to quantify microarchitectural features of interest, including bone volume fraction, tissue mineral density, pore size, pore spacing, and pore number. Samples were cyclically loaded in compression to a stress of 70 MPa, and fatigue life was defined as the number of cycles until failure. Finite element models were created from the μCT images and used to quantify stressed volume. Based on the expected log point-wise predictive density, stressed volume was a strong predictor of fatigue life in both the MC3 and P1. A regional analysis indicated fatigue life was more strongly associated with bone volume fraction in the superficial (r2 = 0.32, p < 0.001) and middle (r2 = 0.70, p < 0.001) regions of the subchondral bone, indicating the prominent role that the cortical plate played in the fatigue resistance of equine subchondral bone. By improving our understanding of the variance in fatigue life measurements, this research helps clarify the underlying mechanisms of the mechanical fatigue process and provides a basic understanding of subchondral bone injuries in the equine fetlock joint.

Xylem-dwelling pathogen unaffected by local xylem vessel network properties in grapevines (Vitis spp.).

Xylella fastidiosa (Xf) is the xylem-dwelling bacterium associated with Pierce's disease (PD), which causes mortality in agriculturally important species, such as grapevine (Vitis vinifera). The development of PD symptoms in grapevines depends on the ability of Xf to produce cell-wall-degrading enzymes to break up intervessel pit membranes and systematically spread through the xylem vessel network. Our objective here was to investigate whether PD resistance could be mechanistically linked to xylem vessel network local connectivity. We used high-resolution X-ray micro-computed tomography (microCT) imaging to identify and describe the type, area and spatial distribution of intervessel connections for six different grapevine genotypes from three genetic backgrounds, with varying resistance to PD (four PD resistant and two PD susceptible). Our results suggest that PD resistance is unlikely to derive from local xylem network connectivity. The intervessel pit area (Ai) varied from 0.07 ± 0.01 mm2 mm-3 in Lenoir to 0.17 ± 0.03 mm2 mm-3 in Blanc do Bois, both PD resistant. Intervessel contact fraction (Cp) was not statically significant, but the two PD-susceptible genotypes, Syrah (0.056 ± 0.015) and Chardonnay (0.041 ± 0.013), were among the most highly connected vessel networks. Neither Ai nor Cp explained differences in PD resistance among the six genotypes. Bayesian re-analysis of our data shows moderate evidence against the effects of the traits analysed: Ai (BF01 = 4.88), mean vessel density (4.86), relay diameter (4.30), relay density (3.31) and solitary vessel proportion (3.19). Our results show that radial and tangential xylem network connectivity is highly conserved within the six different Vitis genotypes we sampled. The way that Xf traverses the vessel network may limit the importance of local network properties to its spread and may confer greater importance on host biochemical responses.

3D visualization of oil-abundant limon flavedo layer under drying

This study investigated the transformations of lemon flavedo tissues during freeze-drying based on high-resolution X-ray micro-computed tomography (μ-CT) and confocal laser scanning microscopy (CLSM). Contrast-enhanced segmentation, traversal statistic algorithmic analysis, and 3D visualization of lemon peel texture are studied. To avoid pseudo-imaging caused by precipitation of contrast enhancer, low concentration cesium iodide was used to improve X-ray contrast and decrease enlarged inter-cellular region. X-ray μ-CT showed the precipitation of contrast enhancers at the intercellular boundary after freeze-drying. The grayscale thresholding method was presented as the most suitable segmentation method for detecting cell walls due to the high noise level caused by low contrast enhancer concentration in the reconstructed images. The faster water loss at the primary drying stage caused the disintegration of oil glands and induced high porosity of 0.7 % in fresh to 0.84 % in 0.5 h freeze-dried. The results suggest that noise filtering based on voxel statistics provides an efficient approach for the inter and intra-cellular microstructural analysis of excessively watery plant tissues with low contrast enhancer concentration.

Updated cranial and mandibular description of the Late Cretaceous (Maastrichtian) baenid turtle Saxochelys gilberti based on micro-computed tomography scans and new information on the holotype-shell association

Saxochelys gilberti is a baenid turtle from the Late Cretaceous Hell Creek Formation of the United States of America known from cranial, shell, and other postcranial material. Baenid turtles are taxonomically diverse and common fossil elements within Late Cretaceous through Eocene faunas. Detailed anatomical knowledge is critical to understanding the systematics and morphological evolution of the group. This is particularly important as baenids represent an important group of continental vertebrates that survived the mass extinction event associated with the Cretaceous/Paleogene boundary. High-resolution micro-computed tomography scanning of the holotype skull reveals additional anatomical details for the already well-known Saxochelys gilberti. This includes the revision of some anatomical statements from the original description, but also detailed knowledge on internal anatomical features of the braincase and the description of a well-preserved axis (cervical vertebra 2). Our new detailed description and previous work on the shell and postcrania make Saxochelys one of the best-described, nearly complete baenid turtles, which are often only known from either isolated shell or cranial material. A revised phylogenetic analysis confirms the position of Saxochelys gilberti as a derived baenid (Eubaeninae) more closely related to Baena arenosa than to Eubaena cephalica.

On the characteristics of natural hydraulic dampers: An image-based approach to study the fluid flow behaviour inside the human meniscal tissue

The meniscal tissue is a layered material with varying properties influenced by collagen content and arrangement. Understanding the relationship between structure and properties is crucial for disease management, treatment development, and biomaterial design. The internal layer of the meniscus is softer and more deformable than the outer layers, thanks to interconnected collagen channels that guide fluid flow. To investigate these relationships, we propose an integrated approach that combines Computational Fluid Dynamics (CFD) with Image Analysis (CFD-IA). We analyze fluid flow in the internal architecture of the human meniscus across a range of inlet velocities (0.1 mm/s to 1.6 m/s) using high-resolution 3D micro-computed tomography scans. Statistical correlations are observed between architectural parameters (tortuosity, connectivity, porosity, pore size) and fluid flow parameters (Re number distribution, permeability). Some channels exhibit Re values of 1400 at an inlet velocity of 1.6 m/s, and a transition from Darcy’s regime to a non-Darcian regime occurs around an inlet velocity of 0.02 m/s. Location-dependent permeability ranges from 20-32 Darcy. Regression modelling reveals a strong correlation between fluid velocity and tortuosity at high inlet velocities, as well as with channel diameter at low inlet velocities. At higher inlet velocities, flow paths deviate more from the preferential direction, resulting in a decrease in the concentration parameter by an average of 0.4. This research provides valuable insights into the fluid flow behaviour within the meniscus and its structural influences. 3D models and image stack are available to download at https://doi.org/10.5281/zenodo.10401592. Statement of significanceThe meniscus is a highly porous soft tissue with remarkable properties of load transfer and energy absorption. We give insight on the mechanism of energy absorption from high resolution uCT scans, never presented before, and a new method which combine CFD and image. The structure is similar to a sandwich structure with a stiff outside layer and a soft internal layer made of collagen channels oriented in a preferential direction guiding the fluid flow, enabling it to accommodate deformation and dissipate energy, making it a potentially optimized damping system. We investigate architectural/ fluid flow parameters- fluid regimes relationship, which is of interest of the readers working on designing suitable biomimetic systems that can be adopted for replacement.

Assessment of Mechanically Induced Changes in Helical Fiber Microstructure Using Diffusion Tensor Imaging.

Noninvasive methods to detect microstructural changes in collagen-based fibrous tissues are necessary to differentiate healthy from damaged tissues in vivo but are sparse. Diffusion Tensor Imaging (DTI) is a noninvasive imaging technique used to quantitatively infer tissue microstructure with previous work primarily focused in neuroimaging applications. Yet, it is still unclear how DTI metrics relate to fiber microstructure and function in musculoskeletal tissues such as ligament and tendon, in part because of the high heterogeneity inherent to such tissues. To address this limitation, we assessed the ability of DTI to detect microstructural changes caused by mechanical loading in tissue-mimicking helical fiber constructs of known structure. Using high-resolution optical and micro-computed tomography imaging, we found that static and fatigue loading resulted in decreased sample diameter and a re-alignment of the macro-scale fiber twist angle similar with the direction of loading. However, DTI and micro-computed tomography measurements suggest microstructural differences in the effect of static versus fatigue loading that were not apparent at the bulk level. Specifically, static load resulted in an increase in diffusion anisotropy and a decrease in radial diffusivity suggesting radially uniform fiber compaction. In contrast, fatigue loads resulted in increased diffusivity in all directions and a change in the alignment of the principal diffusion direction away from the constructs' main axis suggesting fiber compaction and microstructural disruptions in fiber architecture. These results provide quantitative evidence of the ability of DTI to detect mechanically induced changes in tissue microstructure that are not apparent at the bulk level, thus confirming its potential as a noninvasive measure of microstructure in helically architected collagen-based tissues, such as ligaments and tendons.

Clustering characteristics of Fe-rich intermetallics in high vacuum die cast AlSiMgMn alloys with high resolution μ-CT inspection

The AlSiMgMn alloys with different Fe and Mn contents were prepared with high vacuum die casting (HVDC) process. The Fe-rich intermetallics in the surface layer and center of the alloys were inspected with high-resolution 3D X-ray micro-computed tomography (μ-CT), and the growth mechanism of the primary Fe-rich phase was analyzed through their different 3D morphographies. By combining Bisecting K-means and DBSCAN (Density-Based Spatial Clustering of Applications with Noise) methods, the intermetallic clusters in the surface layer and center were quantified. The results show that the primary Fe-rich intermetallics were characterized as hexahedron and octagonal dendrite shapes with large size while the eutectic Fe-rich intermetallics were polyhedron and Chinese-script shapes. When Fe and Mn contents of the alloys were lower, the intermetallic clusters in the surface layer were with less cluster number and larger intermetallic distances showing uniform distribution whereas the clusters in the center were more and had shorter distances. In the case of alloys with higher Fe and Mn contents, the intermetallics showed clustering distribution in both the surface layer and center. The mechanism for the intermetallic cluster formation in the surface layer and center was further discussed.

3D Progression of Dead Li on Graphite Electrodes during Extended Fast Charging

Long charging times of commercial lithium-ion batteries (LIBs) constitute one of the critical remaining bottlenecks in the widespread deployment of electric vehicles (EVs). Therefore, there is a global push towards extreme fast charging (XFC)1in 10–15 minutes for 80% of the pack capacity. However, existing LIBs cannot achieve these XFC goals without significant capacity fade during cycling over battery lifetime.2 One of the key XFC degradation mechanisms is “Li plating,” which occurs when Li metal forms on the graphite electrode due the liquid electrolyte and solid-phase (graphite) mass transport limitations and sluggish charge-transfer kinetics of the Li intercalation reaction.3 This is mostly attributed to the formation of dead Li,4 which is the irreversibly plated Li that has become electronically disconnected from the graphite electrode. Since dead Li constitutes most of the XFC-related capacity loss, it is extremely important to unravel the link between its morphological evolution/progression, and battery capacity fade during extended XFC cycling.In this work, we report non-destructive, in-situ three-dimensional (3D) characterization of dead Li on graphite electrodes in full-cell LIBs during extended XFC using high-resolution (pixel size: ~ 7.8 µm; effective spatial resolution: ~25-30 µm) neutron micro-computed tomography (µCT). Specifically, we imaged batteries in the discharged state at the following cycle numbers at 6C charging rate: 10, 25, 50, and 150 cycles. Neutron µCT is promising for in-situ 3D Li detection on graphite electrodes because it provides strong contrast between Li and C (~ 71.87: 5.55 barns5). To leverage high-resolution neutron µCT for this work, we designed a custom neutron-friendly LIB coin-cell that provided exceptional neutron transmission at the graphite-separator-electrolyte interface as well as standard XFC performance at 6C between 3.0 and 4.1 V. We performed these imaging experiments at the MARS (CG-1D) beamline6 at the High Flux Isotope Reactor, Oak Ridge National Laboratory.Our results reveal 3D evolution of dead Li morphology from isolated plated deposits on only one edge of the graphite electrode after 25 cycles at 6C charging, to increasingly mossy-like covering the entire circumference of the graphite electrode after 150 cycles. Based on our imaging data, we did not observe any dead Li after only 10 XFC cycles. However, we noticed that dead Li started to nucleate around a partial edge of the graphite electrode after 25 XFC cycles, and then grew to the other edges after 50 XFC cycles, eventually forming a complete ring after 150 XFC cycles. At 150 XFC cycles, we also observed the dead Li ring outgrowths away from the edges of the graphite electrode onto the separator. In the extended XFC-cycled samples, 50 and 150 XFC cycles, we found significant dried out salt deposits on the separator, spacers, spring, and casing, which may be due to other parasitic reactions occurring at increased XFC cycling. Lastly, we determined quantitative relationships between the amount of dead Li in 3D, XFC cycling number, and XFC-related capacity loss of the battery.In conclusion, this work contributed to the advanced understanding of the 3D progression of dead Li and its relationship with XFC-related capacity loss on graphite electrodes during extended XFC cycling. We believe insights from this work will help develop improved 3D graphite electrode architectures that will minimize Li plating during repeated XFC cycling in fast-charged LIBs.