Ion Beam Scanning Electron Microscopy Research Articles

Pore development characteristics and controlling factors of Lower Cambrian Qiongzhusi shale gas reservoir in Sichuan Basin, China

Recently, the shale gas exploration of Lower Cambrian Qiongzhusi Formation in Sichuan Basin has made a great breakthrough. However, the pore characteristics and controlling factors of the shale-gas reservoir in the Qiongzhusi Formation are not clear, which hinders further exploration and development of shale gas. This paper focuses on the Qiongzhusi Formation in the Lower Cambrian of the Sichuan Basin. On the basis of mineral composition and the lithofacies types of shale-gas reservoirs in Qiongzhusi Formation were classified by microscopic observation. Additionally, focused ion beam-scanning electron microscope (FIB-SEM), advanced mineral identification and characterization system (AMICS) analysis, large-field stitching scanning electron microscope technology (MAPS) and nitrogen adsorption experiment were employed to comprehensively determine the differential characteristics and controlling factors of pore development. The results indicate that the pore types in Qiongzhusi Formation are mainly composed of interparticle pores and intercrystalline pores. The pore structure of Qiongzhusi Formation is complex. Significant differences in pore structure parameters are observed among different lithofacies. Quartz and feldspar contribute to the preservation of primary pores due to their strong compressive resistance. Clay minerals and carbonate minerals impede pore development by occluding pores. The influence of organic matter on the pore development is relatively small. According to the mineral composition and pore parameters, laminated shale is a relatively favorable reservoir facies among different lithofacies types.

Electrochemical, Microstructural and Mechanical Investigations of H2O2-Driven Degradation of Ti6Al4V

Titanium and its alloys consitute one of the main classes of materials utilized as non-biodegradable implants in the human body. The corrosion resistance of titanium is mainly due to the presence of a thin, compact and passive layer on its surface. However, this layer degrades in the presence of reactive oxygen species, such as oxygen peroxide (H2O2) [1,2]. This leads to the device degradation and the release of its constituents in the surrounding tissues, which may bring about serious health issues (peri-implantitis, osteolysis, neurotoxicity...) [3]. H2O2 is produced by the immune system during inflammatory episodes by specific enzymes, such as NADPH oxidase and superoxide dismutase [4]. It is also utilized by surgeons at high concentrations (ca. 1 M) during peri-implant tissue disinfection. Ti6Al4V (titanium grade 5, an α + β alloy) is a popular implant material because of its excellent mechanical properties. However, in recent years, Ti6Al4V with equiaxed α grains (and β phase located at the grain boundaries) was reported to undergo a significant degradation by H2O2 characterized by the growth of a thick oxide layer on the α grains and the development of porosity and cracks in the β phase [1]. Ti6Al4V could be susceptible to stress corrosion cracking (SCC) under mechanical load due to the β phase dissolution in H2O2-containing physiological solutions (Figure 1). However, no clear link has been established yet between the corrosive environment, the mechanical load and the microstructure of the Ti6Al4V alloy.This contribution will report about the influence of H2O2 concentration on the in vitro corrosion of Ti6Al4V simulating inflammation conditions (low concentration) as well as disinfection procedures (high concentrations). Results on the electrochemical behavior (monitored by impedance spectroscopy), the degraded microstructure (obtained with focused ion beam scanning electron microscopy and transmission electron microscopy) and the impact of the H2O2-driven degradation on the mechanical properties of the alloy will be presented and discussed.Acknowledgements:The authors gratefully acknowledge the financial support of the French National Research Agency (grant agreement ANR-22-CE93-0007-02) and that of the Swiss National Science Foundation (grant agreement 200021L_213161).

(Invited) Dry Process for Thick Electrode in Batteries

Due to its high operating voltage and cobalt-free chemistry, the spinel-type LiNi0.5Mn1.5O4 (LNMO) cathode material has attracted great interest as one of the few next-generation candidates capable of addressing this combination of challenges. However, severe capacity degradation and poor interphase stability have thus far impeded the practical application of LNMO. In this study, by leveraging a dry electrode coating process, we demonstrate LNMO electrodes with stable full cell operation and ultra-high loading. This excellent cycling stability is ascribed to a stable cathode-electrolyte interphase for charge transfer and ion transport, a highly distributed and interconnected electronic percolation network, and robust mechanical properties. High-quality images collected using plasma focused ion beam scanning electron microscopy (PFIB-SEM) provide additional insight into this behavior, with a complementary 2-D model illustrating how the electronic percolation network in the dry-coated electrodes more efficiently supports homogeneous electrochemical reaction pathways. These results strongly motivate that LNMO as a high voltage cobalt-free cathode chemistry combined with an energy-efficient dry electrode coating process opens the possibility for sustainable electrode manufacturing of cost-effective and high-energy-density cathode materials.

The Mg Electrode Cycling Mechanism in Simple Salt Glyme Electrolytes

The lithium-ion battery (LIB) has been at the forefront of innovations in energy storage since its commercialisation over 30 years ago. As we reach the practical specific capacity limit of current state-of-the-art materials, novel and innovative battery technologies are required to satiate the requirements of energy intensive applications such as electric vehicles. 1 The use of a lithium metal negative electrode has been proposed to increase the energy density, however the high reactivity causes poor cycling performance due to electrolyte degradation, dendrite formation and safety issues. 2 The magnesium electrode offers a solution that has double the theoretical volumetric capacity of the lithium electrode while simultaneously mitigating dendritic growth, reducing raw material costs and greatly increasing sustainability. 3,4 Previous work has shown that traditional LIB electrolytes are not compatible with magnesium metal, and the plating and stripping mechanism that underpins how magnesium electrodes cycle is poorly understood. 5 Here we explored the mechanism of magnesium plating and stripping in glyme-based electrolytes with a range of additional additives. We show that in the pure electrolyte solution, interphase formation is critical to stable cycling but that this is accompanied by significant degradation and accumulation of inactive Mg.6 We establish the three-dimensional chemical composition of Mg deposits in the different electrolyte formulations using a combination of focused ion beam-scanning electron microscopy (FIB-SEM), energy dispersive x-ray spectroscopy (EDX) and transmission electron microscopy (TEM). We use these findings to develop a mechanistic understanding that explains the electrochemical cycling performance of magnesium metal negative electrodes. In situ electrochemical quartz crystal microbalance (EQCM) measurements are used to evaluate the plating and stripping efficiency of the electrodes and to identify non-electrochemical degradation reactions between Mg and the electrolyte solutions.

Quantitative subcellular reconstruction reveals a lipid mediated inter-organelle biogenesis network.

The structures and functions of organelles in cells depend on each other but have not been systematically explored. We established stable knockout cell lines of peroxisomal, Golgi and endoplasmic reticulum genes identified in a whole-genome CRISPR knockout screen for inducers of mitochondrial biogenesis stress, showing that defects in peroxisome, Golgi and endoplasmic reticulum metabolism disrupt mitochondrial structure and function. Our quantitative total-organelle profiling approach for focussed ion beam scanning electron microscopy revealed in unprecedented detail that specific organelle dysfunctions precipitate multi-organelle biogenesis defects, impair mitochondrial morphology and reduce respiration. Multi-omics profiling showed a unified proteome response and global shifts in lipid and glycoprotein homeostasis that are elicited when organelle biogenesis is compromised, and that the resulting mitochondrial dysfunction can be rescued with precursors for ether-glycerophospholipid metabolic pathways. This work defines metabolic and morphological interactions between organelles and how their perturbation can cause disease.

MUSCLE UP: WHAT AGING LOOKS LIKE FROM THE INSIDE OUT

Abstract The Longitudinal Studies Section of the Translational Gerontology Branch of the National Institute on Aging Intramural Research Program has the mission and opportunity to examine aging physiology from the cellular to the full body functional level in model systems and human populations. This symposium presents ongoing research that targets pathologic and normative change in muscle with aging and the significance of these changes for understanding the aging process. Data come from the Baltimore Longitudinal Study of Aging (BLSA) and the Genetic and Epigenetic Signatures of Translational Aging Laboratory Testing (GESTALT) study. In nearly 500 BLSA participants aged 50+, Zenobia Moore evaluates the association between multiple epigenetic age metrics and change over 6 years in mid-femur areas of muscle and subcutaneous and intramuscular fat derived from computed tomography. Qu (Teresa) Tian investigates the relationship between skeletal muscle mitochondrial function and risk of MCI or dementia over 3.3 years in 460 initially cognitively normal BLSA participants and PET and blood biomarkers of AD in available subsamples. In 82 men and women from GESTALT, Stefano Donega examines relationships between physical activity, peak oxygen consumption and muscle oxidative capacity using p31 MR spectroscopy and gene expression, transcript usage and splicing events derived from vastus lateralis biopsies. Using volumetric Focused Ion Beam Scanning Electron Microscopy, Lisa Hartnell shares 3D images of muscle samples at the level of the mitochondrial reticulum and sarcomere from young and old healthy and frail GESTALT participants. Together, these findings highlight the value of muscle as a window on aging.

Mid-Infrared (MIR) Complex Refractive Index Spectra of Polycrystalline Copper-Nitride Films by IR-VASE Ellipsometry and Their FIB-SEM Porosity

Copper-nitride (Cu3N) semiconductor material is attracting much attention as a potential, next-generation thin-film solar light absorber in solar cells. In this communication, polycrystalline covalent Cu3N thin films were prepared using reactive-RF-magnetron-sputtering deposition, at room temperature, onto glass and silicon substrates. The very-broadband optical properties of the Cu3N thin film layers were studied by UV-MIR (0.2–40 μm) ellipsometry and optical transmission, to be able to achieve the goal of a low-cost absorber material to replace the conventional silicon. The reactive-RF-sputtered Cu3N films were also investigated by focused ion beam scanning electron microscopy and both FTIR and Raman spectroscopies. The less dense layer was found to have a value of the static refractive index of 2.304, and the denser film had a value of 2.496. The iso-absorption gap, E04, varied between approximately 1.3 and 1.8 eV and could be considered suitable as a solar light absorber.

Segmentation of cellular ultrastructures on sparsely labeled 3D electron microscopy images using deep learning.

Focused ion beam-scanning electron microscopy (FIB-SEM) images can provide a detailed view of the cellular ultrastructure of tumor cells. A deeper understanding of their organization and interactions can shed light on cancer mechanisms and progression. However, the bottleneck in the analysis is the delineation of the cellular structures to enable quantitative measurements and analysis. We mitigated this limitation using deep learning to segment cells and subcellular ultrastructure in 3D FIB-SEM images of tumor biopsies obtained from patients with metastatic breast and pancreatic cancers. The ultrastructures, such as nuclei, nucleoli, mitochondria, endosomes, and lysosomes, are relatively better defined than their surroundings and can be segmented with high accuracy using a neural network trained with sparse manual labels. Cell segmentation, on the other hand, is much more challenging due to the lack of clear boundaries separating cells in the tissue. We adopted a multi-pronged approach combining detection, boundary propagation, and tracking for cell segmentation. Specifically, a neural network was employed to detect the intracellular space; optical flow was used to propagate cell boundaries across the z-stack from the nearest ground truth image in order to facilitate the separation of individual cells; finally, the filopodium-like protrusions were tracked to the main cells by calculating the intersection over union measure for all regions detected in consecutive images along z-stack and connecting regions with maximum overlap. The proposed cell segmentation methodology resulted in an average Dice score of 0.93. For nuclei, nucleoli, and mitochondria, the segmentation achieved Dice scores of 0.99, 0.98, and 0.86, respectively. The segmentation of FIB-SEM images will enable interpretative rendering and provide quantitative image features to be associated with relevant clinical variables.

Detection of atmospheric aerosols and terrestrial nanoparticles collected in a populous city in southern Brazil.

The main objective of this study is to analyze hazardous elements in nanoparticles (NPs) (smaller than 100nm) and ultrafine particles (smaller than 1µm) in Porto Alegre City, southern Brazil using a self-made passive sampler and Sentinel-3B SYN satellite images in 32 collection points. The Aerosol Optical Thickness proportion (T550) identification was conducted using images of the Sentinel-3B SYN satellite at 634 points sampled in 2019, 2020, 2021, and 2022. Focused ion beam scanning electron microscopy analyses were performed to identify chemical elements present in NPs and ultrafine particles, followed by single-stage cascade impactor to be processed by high-resolution transmission electron microscopy. This process was coupled with energy-dispersive X-ray spectroscopy and later analysis via secondary ion mass spectrometry. Data was acquired from Sentinel-3B SYN images, normalized to a standard mean of 0.83µg/mg, at moderate spatial resolution (260m), and modeled in the Sentinel Application Platform (SNAP) software v.8.0. Statistical matrix data was generated in the JASP software (Jeffreys's Amazing Statistics Program) v.0.14.1.0 followed by a K-means cluster analysis. The results demonstrate the presence of between 1 and 100nm particles of the following chemical elements: Si, Al, K, Mg, P, and Ti. Many people go through these areas daily and may inhale or absorb these elements that can harm human health. In the Sentinel-3B SYN satellite images, the sum of squares in cluster 6 is 168,265 and in cluster 7 a total of 21,583. The use of images from the Sentinel-3B SYN satellite to obtain T550 levels is of great importance as it reveals that atmospheric pollution can move through air currents contaminating large areas on a global scale.

Bundling of collagen fibrils influences osteocyte network formation during bone modeling

Osteocytes form a cellular network by gap junctions between their cell processes. This network is important since intercellular communication via the network is essential for bone metabolism. However, the factors that influence the formation of this osteocyte network remain unknown. As the early stage of osteocyte network formation occurs on the bone surface, we observed a newly formed trabecular bone surface by orthogonal focused ion beam-scanning electron microscopy. The embedding late osteoblast processes tended to avoid bundled collagen fibrils and elongate into sparse collagen fibrils. Then, we examined whether the inhibition of bundling of collagen fibrils using a potent lysyl oxidase inhibitor, β-aminopropionitrile (BAPN) changed the cellular network of the chick calvaria. The osteocyte shape of the control group was spindle-shape, while that of the BAPN group was sphere-shaped. In addition, the osteocyte processes of the control group were elongated vertically to the long axis of the cell body, whereas the osteocyte processes of the BAPN group were elongated radially. Therefore, it was suggested that the bundling of collagen fibrils influences normal osteocyte network formation during bone modeling.

Size and shape analysis of micro- to nano-particles of quartz powders using advanced electron microscopy and laser diffraction methods

The paper deals with particle analysis and the evaluation of the shape and size distribution of micro- to nano-sized quartz particles as a key parameter for the evaluation of quality in many industrial fields, particularly for high-purity applications. Samples are analyzed by laser diffraction, the most commonly used method for determining the size of the particles; for precise measurement with the possibility of high-resolution imaging of particles, scanning electron microscopy was applied. For morphological and size analysis of electrically non-conductive micro- to nano-particles under environmentally compatible conditions of elevated gas pressure and humidity, environmental scanning electron microscopy was selected as the most suitable. Moreover, the high-end methods of focused ion beam scanning electron microscopy and serial block-face scanning electron microscopy enabled the analysis of particles in the epoxy resin volume including spatial imaging. The application of image post-processing as an important part of the electron microscopy workflow is also discussed.

Characterization for 3D pore-fracture systems in Hot-Dry-Rock samples from Gonghe Basin, China

As a new type of renewable energy, Hot-Dry-Rock (HDR) is gaining increasing attention. The physical properties of rock influenced by the pore-fracture structure are vital for the hydraulic and chemical characteristics of HDR reservoirs. However, the natural pore-fracture structure in HDR has not been sufficiently studied. To fulfill this gap, we used focused ion beam-scanning electron microscopy (FIB-SEM) to construct three-dimensional (3D) digital models for four granite samples from the deep HDR reservoir in Gonghe Basin, Qinghai Province, China, and obtained the nanoscale structure of the pores and fractures in HDR reservoir for the first time. Our analysis based on the 3D models indicates that the heat transfer area in the HDR reservoir is mainly from fractures and crack-like pores, but a large amount of small but regular pores could be neglected when heat transfer in HDR is considered. The permeability of HDR reservoirs at nanoscale varies from 9.414 nD to 0.082 mD, and the high permeability in this study is accompanied by throughgoing fractures. The variation of porosity and permeability of deep HDR at nanoscale in this study is much more severe than that of shallow granites previously studied at microscale. The performance of geothermal field is significantly influenced by the size of throats and the average size and tortuosity of the interconnected pore-fracture network in HDR. The hydraulic aperture could be 32-58% lower than the mechanical aperture of the natural fractures in HDR reservoirs, which is a vital clue for the numerical simulation associated with enhanced geothermal systems.

CDK2 inhibition disorders centrosome stoichiometry and alters cellular outcomes in aneuploid cancer cells

ABSTRACT Cyclin-dependent Kinase 2 (CDK2) inhibition prevents supernumerary centrosome clustering. This causes multipolarity, anaphase catastrophe and apoptotic death of aneuploid cancers. This study elucidated how CDK2 antagonism affected centrosome stoichiometry. Focused ion beam scanning electron microscopy (FIB-SEM) and immunofluorescent imaging were used. Studies interrogated multipolar mitosis after pharmacologic or genetic repression of CDK2. CDK2/9 antagonism with CYC065 (Fadraciclib)-treatment disordered centrosome stoichiometry in aneuploid cancer cells, preventing centrosome clustering. This caused ring-like chromosomes or multipolar cancer cells to form before onset of cell death. Intriguingly, CDK2 inhibition caused a statistically significant increase in single centrioles rather than intact centrosomes with two centrioles in cancer cells having chromosome rings or multipolarity. Statistically significant alterations in centrosome stoichiometry were undetected in other mitotic cancer cells. To confirm this pharmacodynamic effect, CDK2 but not CDK9 siRNA-mediated knockdown augmented cancer cells with chromosome ring or multipolarity formation. Notably, engineered gain of CDK2, but not CDK9 expression, reversed emergence of cancer cells with chromosome rings or multipolarity, despite CYC065-treatment. In marked contrast, CDK2 inhibition of primary human alveolar epithelial cells did not confer statistically significant increases of cells with ring-like chromosomes or multipolarity. Hence, CDK2 antagonism caused differential effects in malignant versus normal alveolar epithelial cells. Translational relevance was confirmed by CYC065-treatment of syngeneic lung cancers in mice. Mitotic figures in tumors exhibited chromosome rings or multipolarity. Thus, CDK2 inhibition preferentially disorders centrosome stoichiometry in cancer cells. Engaging this disruption is a strategy to explore against aneuploid cancers in future clinical trials.

Visualizing the Structure, Composition and Activity of Single Catalyst Particles for Olefin Polymerization and Polyolefin Decomposition.

The structural and morphological characterization of individual catalyst particles for olefin polymerization, as well as for the reverse process of polyolefin decomposition, can provide an improved understanding for how these catalyst materials operate under relevant reaction conditions. In this review, we discuss an emerging analytical toolbox of 2D and 3D chemical imaging techniques that is suitable for investigating the chemistry and reactivity of related catalyst systems. While synchrotron-based X-ray microscopy still provides unparalleled spatial resolutions in 2D and 3D, a number of laboratory-based techniques, most notably focused ion beam-scanning electron microscopy, confocal fluorescence microscopy, infrared photoinduced force microscopy and laboratory-based X-ray nano-computed tomography, have helped to significantly expand the arsenal of analytical tools available to scientists in heterogeneous catalysis and polymer science. In terms of future research, the review outlines the role and impact of in situ and operando (spectro-)microscopy experiments, involving sophisticated reactors as well as online reactant and product analysis, to obtain real-time information on the formation, decomposition, and mobility of polymer phases within single catalyst particles. Furthermore, the potential of fluorescence microscopy, X-ray microscopy and optical microscopy is highlighted for the high-throughput characterization of olefin polymerization and polyolefin decomposition catalysts. By combining these chemical imaging techniques with, for example, chemical staining methodologies, selective probe molecules as well as particle sorting approaches, representative structure-activity relationships can be derived at the level of single catalyst particles.

How sintering temperature affects the electrochemical performance of ultra-high nickel (Ni > 0.9) cathode material

The burgeoning demand for electric vehicles with extended driving ranges has propelled ongoing development efforts for ultra-high nickel (Ni > 0.9) cathode materials. Despite significant ongoing research focused on Ni-rich cathode materials, a more comprehensive foundational understanding of ultra-high nickel cathode materials is essential. In our research, we employed LiNi0.94Co0.06O2 as a model ultra-high nickel cathode material to systematically delve into the interplay between sintering temperature, structural features, and electrochemical behavior. Within a sintering temperature spectrum of 660–720 °C, we discerned that specimens produced at diminished temperatures manifest a reduced initial discharge capacity yet excel in cycling endurance. In stark contrast, their counterparts produced at augmented temperatures behave inversely. Identifying a singular sintering temperature that achieves equilibrium between initial discharge capacity and cycling performance proves elusive. Through X-ray diffraction and high-resolution transmission electron microscopy, it became evident that samples synthesized at lower temperatures exhibit pronounced lithium-nickel mixing and develop a thicker NiO layer on the surface, leading to compromised initial discharge performance and capacity. Utilizing focused ion beam scanning electron microscopy, differential capacity analysis, and in-situ X-ray diffraction, we confirm that samples synthesized at lower temperatures possess smaller particle sizes, enabling them to withstand volumetric expansion stress during cycling, resulting in enhanced cycling performance. In the realm of ultra-high nickel cathode materials, elevating the sintering temperature is a conduit to superior initial discharge efficiency and capacity. Yet, the imperative of preserving diminutive particle dimensions, as a stratagem to bolster cycling performance, stands out as a pivotal research frontier.

Local Structural Modifications in Metallic Micropillars Induced by Plasma Focused Ion Beam Processing.

A focused ion beam scanning electron microscope (FIB-SEM) is a powerful tool that is routinely used for scale imaging from the micro- to nanometer scales, micromachining, prototyping, and metrology. In spite of the significant capabilities of a FIB-SEM, there are inherent artefacts (e.g., structural defects, chemical interactions and phase changes, ion implantation, and material redeposition) that are produced due to the interaction of Ga+ or other types of ions (e.g., Xe+, Ar+, O+, etc.) with the sample. In this study, we analyzed lattice distortion and ion implantation and subsequent material redeposition in metallic micropillars which were prepared using plasma focus ion beam (PFIB) milling. We utilized non-destructive synchrotron techniques such as X-ray fluorescence (XRF) and X-ray nanodiffraction to examine the micropillars prepared using Xe+ ion energies of 10 keV and 30 keV. Our results demonstrate that higher Xe ion energy leads to higher density of implanted ions within the redeposited and milled material. The mixing of ions in the redeposited material significantly influences the lattice structure, causing deformation in regions with higher ion concentrations. Through an X-ray nanodiffraction analysis, we obtained numerical measurements of the strain fields induced in the regions, which revealed up to 0.2% lattice distortion in the ion bombardment direction.

Three-dimensional architecture of granulosa cell derived from oocyte cumulus complex, revealed by FIB-SEM

The oocyte cumulus complex is mainly composed of an oocyte, the perivitelline space, zona pellucida and numerous granulosa cells. The cumulus granulosa cells (cGCs) provide a particularly important microenvironment for oocyte development, regulating its growth, maturation and meiosis. In this study, we studied the internal structures and cell-to-cell connections of mouse cGCs using focused ion beam scanning electron microscopy (FIB-SEM). We reconstructed three-dimensional models to display characteristic connections between the oocyte and cGCs, and to illustrate various main organelles in cGCs together with their interaction relationship. A special form of cilium identified in granulosa cell was never reported in previous literature.

Ultrastructure of noise-induced cochlear synaptopathy

Acoustic overexposure can eliminate synapses between inner hair cells (IHCs) and auditory nerve fibers (ANFs), even if hair-cell function recovers. This synaptopathy has been extensively studied by confocal microscopy, however, understanding the nature and sequence of damage requires ultrastructural analysis. Here, we used focused ion-beam scanning electron microscopy to mill, image, segment and reconstruct ANF terminals in mice, 1 day and 1 week after synaptopathic exposure (8–16 kHz, 98 dB SPL). At both survivals, ANF terminals were normal in number, but 62% and 53%, respectively, lacked normal synaptic specializations. Most non-synapsing fibers (57% and 48% at 1 day and 1 week) remained in contact with an IHC and contained healthy-looking organelles. ANFs showed a transient increase in mitochondrial content (51%) and efferent innervation (34%) at 1 day. Fibers maintaining synaptic connections showed hypertrophy of pre-synaptic ribbons at both 1 day and 1 week. Non-synaptic fibers were lower in mitochondrial content and typically on the modiolar side of the IHC, where ANFs with high-thresholds and low spontaneous rates are normally found. Even 1 week post-exposure, many ANF terminals remained in IHC contact despite loss of synaptic specializations, thus, regeneration efforts at early post-exposure times should concentrate on synaptogenesis rather than neurite extension.

Solid electrolyte cracking due to lithium filament growth and concept of mechanical reinforcement – An operando study

Lithium metal solid state batteries (LMSSB) attract great interest in academia and industry due to their projected high energy density and safety. However, hard short circuits due to the penetration of lithium filaments through the solid electrolyte impede their development for practical application. Here, multi-characterization methods ranging from operando and in situ scanning electron microscopy to ex situ focused ion beam scanning electron microscopy are employed for comprehensive understanding of the cell failure. The rapid failure is attributed to coupled crack propagation and subsequent lithium filament growth during the plating process which is demonstrated in a Li6PS5Cl (lithium argyrodite) based LMSSB. Cracking initiates at current constriction spots and voids, where inhomogeneous lithium plating/stripping causes high local stress fields that trigger continuous crack propagation. Lithium filament growth finally leads to a hard short circuit. Considering the low fracture toughness of ceramic electrolytes, strengthening with Al2O3 fibers is shown to be effective in significantly improving the critical current density and cycling stability. Our results clearly show that cracks can have a detrimental effect on LMSSB and we suggest focusing on strategies to improve the fracture toughness of thiophosphate electrolytes in order to suppress lithium filament growth.

Automatic pore structure analysis in organic-rich shale using FIB-SEM and attention U-Net

The pore structure is an important factor in determining the productivity of shale, which can help us make better operational decisions. Shale formations have an extremely complex pore structure with a wide range of pore sizes, shapes, orientations, and connectivity. Advanced imaging techniques, such as focused ion beam scanning electron microscopes (FIB-SEM), contribute significantly to the analysis and understanding of complex pore networks in shale, but they are time-consuming. Developing new methods and techniques to capture the spatial distribution and connectivity of pores at various scales is essential to understanding pore structure and its impact on fluid flow. This study aims to analyze the pore characteristics of shale reservoirs by using artificial intelligence (AI) and FIB-SEM. We applied a novel attention gate (AG) model to FIB-SEM images that automatically learns to focus on target structures of varying pores’ shape and size. AG can be fully incorporated into the U-Net model with minimal computational impact. The AG improved prediction accuracy by making the U-Net model more sensitive to essential features in the input images and achieved a precision of 97%, recall of 71%, and F1 score of 81% at a confidence threshold of 1. Experimental results show that Attention U-Net outperformed in predicting the pore structures in shale samples from Longmaxi Formation, Qingshankou Formation, Cambrian Niutitang Formation, Yanchang shale oil, and Bakken shale while obtaining optimal performance without requiring multiple convolutional neural network (CNN) models. Additionally, Attention U-Net addresses some of the limitations of the Edge-Threshold Automatic Processing (ETAP) method, including the limited ability to obtain a complete description of the pore space as well as the low segmentation accuracy and sensitivity. The proposed workflow offers a promising solution for optimizing the automatic processing of microscopic images for pores and microfractures identification. Researchers and industry professionals can improve their understanding of shale properties and applications in various fields by maximizing the benefits of our workflow.