Ion Beam Scanning Electron Microscopy Research Articles

Electro-Chemo-Mechanical Evolution at the Garnet Solid Electrolyte-Cathode Interface.

Solid-state batteries promise higher energy density and improved safety compared with lithium-ion batteries. However, electro-chemomechanical instabilities at the solid electrolyte interface with the cathode and the anode hinder their large scale implementation. Here, we focus on resolving electro-chemo-mechanical instability mechanisms and their onset conditions between a state-of-the-art cathode, LiNi0.6Mn0.2Co0.2O2 (NMC622), and the garnet Li7La3Zr2O12 (LLZO) solid electrolyte. We used thin-film NMC622 on LLZO pellets to place the interfacial region within the detection depth of the X-ray characterization techniques. The experimental probes of the near-interface region included in operando X-ray absorption spectroscopy and ex situ focused ion beam scanning electron microscopy. Electrochemical degradation was not observable during cycling at room temperature with 4.3 V versus Li/Li+ charge voltage cutoff, or with stepwise potentiostatic hold up to 4.1 V versus Li/Li+. In contrast, secondary phases including reduced transition metal species (Ni2+, Co2+) were found after cycling up to 4.3 V versus Li/Li+ at 80 °C and during potentiostatic hold at 4.3 V versus Li/Li+ (Ni2+). Intergranular cracks between NMC622 grains and delamination at the NMC622|LLZO interface occurred readily after the first charge. These interface reaction products and mechanical failure lowered the capacity and cell efficiency due to partial loss of the NMC622 phase, partial loss of contact at the interface, and a higher polarization resistance. Electrochemical instability between delithiated NMC622 and LLZO could be mitigated by using a low charge voltage cutoff or cycling at lower temperature. Ways to engineer the mechanical properties to avoid crack deflection and delamination at the interface are also discussed for enhancing mechanical stability.

Three-dimensional structural analyses of the oxygen electrodes in solid oxide electrolysis cells

Solid oxide electrolysis cells (SOECs) have garnered interest as efficient devices for production of clean fuel such as hydrogen gas. However, the industrialization of SOEC technology has encountered significant challenges, such as unsatisfactory performance and insufficient durability. In this study, we aimed to improve the electrochemical performance and stability of the SOEC air electrode by modifying it at various annealing temperatures (900, 1000, and 1100 °C). Electrochemical testing revealed that the SOEC cell with the electrode annealed at 1000 °C for 1 h exhibited the highest current density of 0.88 A/cm2 at 750 °C and 1.3 V, which is 1.76-times higher than that of the cell with the unoptimized electrode annealed at 900 °C. Three-dimensional microstructural analyses using Focused Ion Beam-Scanning Electron Microscope (FIB-SEM) confirmed that the optimized cell is the most porous with sufficient pore surface area, thereby facilitating electrochemical reactions and gas transport, and preventing delamination of the air electrode resulting from lower oxygen partial pressure difference between the barrier layer and air/electrode interface. Side reactions at the interface, including the generation of resistant SrZrO3, are concurrently avoided. These findings demonstrate the potential of the modified SOEC air electrode for improving electrochemical performance and stability.

Gamma‐ray‐induced modification of poly(ethylene terephthalate) and polypropylene solid materials with halogen‐containing olefins for X‐ray CT image contrast enhancement

AbstractIt is known that X‐ray CT of organic polymer materials usually provides low‐contrast images because of the low X‐ray absorption of these materials. In this paper, we describe a new method to enhance the contrast of X‐ray CT images of organic polymer materials. We demonstrate that gamma‐ray irradiation of poly (ethylene terephthalate) (PET) fibers in dichloromethane containing 2‐bromoethyl methacrylate, 2‐chloroethyl methacrylate, or 4‐bromostyrene results in the grafting of halogen‐containing oligomeric chains onto the PET fibers. Focused ion beam scanning electron microscopy (FIB‐SEM) and time‐of‐flight secondary ion mass spectrometry (TOF‐SIMS) analyses revealed a homogeneous distribution of bromine atoms within the 2‐bromoethyl methacrylate‐modified PET fibers, not only on the surface. This uniform incorporation translated to a significant improvement in X‐ray CT image contrast compared with pristine fibers. Similar treatment of polypropylene pellets also enhanced the contrast of their X‐ray CT images. This is a new simple and effective method to enhance the X‐ray CT image contrast and potentially applicable to various polymer materials including polymer composites and porous polymer materials, readily allowing the observation of their 3D microstructures finely.

Combining ternary, ionic liquid-based, polymer electrolytes with a single-ion conducting polymer-based interlayer for lithium metal batteries

Among the many approaches to improve the performance of lithium-metal batteries, ternary polyethylene oxide/ionic liquid/lithium salt electrolytes offer several advantages such as low flammability, high conductivity (vs. polyethylene oxide/lithium salt electrolytes) and, to a large extent, limiting the growth of dendrites at moderate currents. However, they suffer from relatively low mechanical strength for lithium metal confinement. Besides, the lithium transport numbers are very low, which is conducive to lithium depletion during plating at high current densities at the lithium/electrolyte interface. Thus, we show here that the combination of a ternary solid polymer electrolyte with a single-ion polymer-based conducting interlayer allows for a significant improvement of the cyclability of the lithium metal anode. This results in a strong improvement of the electrochemical performance of lithium-metal batteries using solid polymer electrolytes at 80 °C, with an 85% capacity retention after 350 cycles (vs. 60% after 62 cycles for the uncoated anode). This is attributed, via focused ion beam-scanning electron microscopy and X-ray photoelectron spectroscopy, to a denser lithium deposit, better contact with the electrolyte and a reduced reactivity of electrolyte species with the interlayer.

Porosity and Organic Content in the Tuscaloosa Marine Shale: Insights from Focused Ion Beam-Scanning Electron Microscopy Characterization

Porosity and Organic Content in the Tuscaloosa Marine Shale: Insights from Focused Ion Beam-Scanning Electron Microscopy Characterization

Microstructural BIB-SEM investigation of Upper Cretaceous Jordanian carbonate-rich oil shales bearing type II-S kerogen

AbstractIn this study, we use Broad Ion Beam polishing and Scanning Electron Microscopy (BIB-SEM) to characterize the microstructure of selected core samples of immature Upper Cretaceous carbonate-rich oil shales from Jordan and to link the observations to porosity and compositional and geochemical data. The aim of this study is to understand the distribution of pore space, primary organic matter, and organic sulfur on a sub-micron scale, particularly in carbonate- and silicate-dominated layers. The thermal maturity of these marine carbonate mudstone samples of pelagic origin was found to be influenced by the elevated sulfur contents in these Type II-S kerogen source rocks. This was confirmed through both organic geochemistry and BIB-SEM observations, which revealed high sulfur content. Porosity in the carbonate mudstone exists within foraminifera, and aggregates of microfossil fragments. Initially, these voids provided significant inter- and intra-particle porosity which were later filled by organic matter during diagenesis. This ‘mobile’ organic matter is interpreted as microscopic bitumen, which exists as a solid or highly viscous fluid at surface conditions. It is likely a residue of low-temperature (“early”) bitumen generation. By examining the samples before and after dichloromethane (DCM) extraction and subsequent BIB-SEM analyses, we observed that the specimens contained a significant amount of soluble organic matter (SOM), mostly present in the micropores associated with calcite. The microscopic solid bitumen is observed to remain stable even under various conditions, such as in vacuum oven conditions of 105 °C (24 h), or exposure to ultra-high vacuum, broad ion beam (heat > 70 °C) and an electron beam of 15 keV. This suggests that the solid bitumen acts as a solid at elevated temperatures and confining pressures (85 °C and 250 MPa), and its presence can lead to the buildup of significant fluid overpressures. Our observations indicate that the pores associated with calcite provide high storage capacity in the shales during the early stages of hydrocarbon generation. In contrast, it suggests that siliciclastic-rich samples are more prone to hydrofracturing as the (early) generated hydrocarbons cannot be expelled easily. These findings highlight the complex distribution and behavior of pore space, organic matter, and sulfur in shales, shedding light on their potential for hydrocarbon generation and storage. Graphical abstract

Characterizing PEM fuel cell catalyst layer properties from high resolution three-dimensional digital images, part I: A numerical procedure for the ionomer distribution reconstruction

In this work, a numerical approach is presented to reconstruct the ionomer three-dimensional distribution in the microstructure of the cathode catalyst layer (CCL) of a polymer electrolyte membrane fuel cell (PEMFC) from a 3D segmented image of the CCL obtained by focused ion beam-scanning electron microscopy (FIB-SEM). Three forms of ionomer are distinguished: the ionomer filaments, the coating ionomer and the inter-carbon grains ionomer. The ionomer filaments are identified by applying a filtering procedure to the size distribution in the segmented solid phase obtained via a maximum sphere inscription algorithm. The coating ionomer is reconstructed via a filtering procedure of the curvature distribution computed over the interface between the two segmented phases from the consideration that concave regions are preferential ionomer accumulation zones during the drying step of the CCL fabrication procedure. This procedure of coating controlled by the local curvature is applied until a desired value of coverage is reached. In a last step, catalyst nanoparticles, also not visible in the FIB-SEM image, are reconstructed in the image.

CryoET of β-amyloid and tau within postmortem Alzheimer’s disease brain

A defining pathological feature of most neurodegenerative diseases is the assembly of proteins into amyloid that form disease-specific structures1. In Alzheimer’s disease, this is characterized by the deposition of β-amyloid and tau with disease-specific conformations. The in situ structure of amyloid in the human brain is unknown. Here, using cryo-fluorescence microscopy-targeted cryo-sectioning, cryo-focused ion beam-scanning electron microscopy lift-out and cryo-electron tomography, we determined in-tissue architectures of β-amyloid and tau pathology in a postmortem Alzheimer’s disease donor brain. β-amyloid plaques contained a mixture of fibrils, some of which were branched, and protofilaments, arranged in parallel arrays and lattice-like structures. Extracellular vesicles and cuboidal particles defined the non-amyloid constituents of β-amyloid plaques. By contrast, tau inclusions formed parallel clusters of unbranched filaments. Subtomogram averaging a cluster of 136 tau filaments in a single tomogram revealed the polypeptide backbone conformation and filament polarity orientation of paired helical filaments within tissue. Filaments within most clusters were similar to each other, but were different between clusters, showing amyloid heterogeneity that is spatially organized by subcellular location. The in situ structural approaches outlined here for human donor tissues have applications to a broad range of neurodegenerative diseases.

Augmentation of Polymer-FeCO3 Microlayers on Carbon Steel for Enhanced Corrosion Protection in Hydrodynamic CO2 Corrosion Environments.

Carbon dioxide (CO2) internal corrosion of carbon steel pipelines is a significant challenge and is typically managed by adding corrosion inhibitors. In certain operational conditions, a natural protective layer of iron carbonate (FeCO3) can form on the internal walls of the pipeline, offering inhibition efficiency comparable to that of standard surfactant inhibitors. However, incomplete coverage of the FeCO3 layer on carbon steel can sometimes trigger localized corrosion. Our previous research demonstrated that poly(allylamine hydrochloride) (PAH) can work synergistically with FeCO3 when the corrosion product partially covers X65 carbon steel surfaces in an aqueous CO2 corrosion environment. In this study, we utilize rotating cylinder electrode (RCE) tests along with electrochemical measurements to investigate the FeCO3-PAH hybrid structure in a dynamic environment. We characterize the general and localized corrosion behavior as well as the surface properties of both naturally formed FeCO3 and FeCO3-PAH hybrid layers using interferometry and focused ion beam scanning electron microscopy.

Characterizing PEM fuel cell catalyst layer properties from high resolution three-dimensional digital images, Part II: Oxygen effective diffusion and proton effective conductivity tensors

The oxygen effective diffusion and proton effective conductivity tensors of a cathode catalyst layer (CCL) are computed using a two-scale approach on CCL microstructure three-dimensional images obtained by focused ion beam-scanning electron microscopy (FIB-SEM) after reconstruction of the ionomer distribution. The results show that the obtained tensors are not isotropic. It is also found that some off-diagonal components are not negligible in the case of the proton effective conductivity tensor. The simulations confirm that Knudsen diffusion has a significant impact on oxygen diffusion. The results are comparable to those obtained in previous works on synthetic images as regards the oxygen effective diffusion through-plane component but differ as regards the proton conductivity through-plane component. Contrary to previous works using synthetic images which tend to underestimate the proton conductivity, they are globally in better agreement with experimental data. The results also show that the effective proton conductivity is heterogeneous at the scale of the computational domains typically considered in several previous works due to the variability in the ionomer distribution at this scale. The impact of liquid water in the primary pores on the proton transport is explored and found to have a significant impact.

Lipid droplet dynamics are essential for the development of the malaria parasite Plasmodium falciparum.

Lipid droplets (LDs) are organelles that are central to lipid and energy homeostasis across all eukaryotes. In the malaria-causing parasite Plasmodium falciparum the roles of LDs in lipid acquisition from its host cells and their metabolism are poorly understood, despite the high demand for lipids in parasite membrane synthesis. We systematically characterised LD size, composition and dynamics across the disease-causing blood infection. Applying split fluorescence emission analysis and three-dimensional (3D) focused ion beam-scanning electron microscopy (FIB-SEM), we observed a decrease in LD size in late schizont stages. LD contraction likely signifies a switch from lipid accumulation to lipid utilisation in preparation for parasite egress from host red blood cells. We demonstrate connections between LDs and several parasite organelles, pointing to potential functional interactions. Chemical inhibition of triacylglyerol (TAG) synthesis or breakdown revealed essential LD functions for schizogony and in counteracting lipid toxicity. The dynamics of lipid synthesis, storage and utilisation in P. falciparum LDs might provide a target for new anti-malarial intervention strategies.

Mesoscale characterization of osseointegration around an additively manufactured genistein-coated implant

Given the hierarchical nature of bone and bone interfaces, osseointegration, namely the formation of a direct bone-implant contact, is best evaluated using a multiscale approach. However, a trade-off exists between field of view and spatial resolution, making it challenging to image large volumes with high resolution. In this study, we combine established electron microscopy techniques to probe bone-implant interfaces at the microscale and nanoscale with plasma focused ion beam-scanning electron microscopy (PFIB-SEM) tomography to evaluate osseointegration at the mesoscale. This characterization workflow is demonstrated for bone response to an additively manufactured Ti-6Al-4V implant which combines engineered porosity to facilitate bone ingrowth and surface functionalization via genistein, a phytoestrogen, to counteract bone loss in osteoporosis. SEM demonstrated new bone formation at the implant site, including in the internal implant pores. At the nanoscale, scanning transmission electron microscopy and energy-dispersive X-ray spectroscopy confirmed the gradual nature of the bone-implant interface. By leveraging mesoscale analysis with PFIB-SEM tomography that captures large volumes of bone-implant interface with nearly nanoscale resolution, the presence of mineral ellipsoids varying in size and orientation was revealed. In addition, a well-developed lacuno-canalicular network and mineralization fronts directed both towards the implant and away from it were highlighted.

Anomalous temperature dependence mechanism of the electrochemical dissolution efficiency of iron-based materials

In tests of typical iron-based materials, it has been found that the dissolution efficiency at low temperature is greater than that at ambient temperature. By utilizing sputtering X-ray photoelectron spectroscopy (sputtering XPS) and focused ion beam scanning electron microscopy (FIB-SEM), it was found that this abnormal phenomenon is rooted in a thinner passive film and lower valence oxides formed on the surface at low temperature. Transmission electron microscopy (TEM) analysis supported these conclusions at the microscopic level. First-principles calculations further revealed that lower valence oxides of iron are more conductive than higher valence oxides.

Quantitative atlas of collagen hydrogels reveals mesenchymal cancer cell traction adaptation to the matrix nanoarchitecture

Collagen-based hydrogels are commonly used in mechanobiology to mimic the extracellular matrix. A quantitative analysis of the influence of collagen concentration and properties on the structure and mechanics of the hydrogels is essential for tailored design adjustments for specific in vitro conditions. We combined focused ion beam scanning electron microscopy and rheology to provide a detailed quantitative atlas of the mechanical and nanoscale three-dimensional structural alterations that occur when manipulating different hydrogel's physicochemistry. Moreover, we study the effects of such alterations on the phenotype of breast cancer cells and their mechanical interactions with the extracellular matrix. Regardless of the microenvironment's pore size, porosity or mechanical properties, cancer cells are able to reach a stable mesenchymal-like morphology. Additionally, employing 3D traction force microscopy, a positive correlation between cellular tractions and ECM mechanics is observed up to a critical threshold, beyond which tractions plateau. This suggests that cancer cells in a stable mesenchymal state calibrate their mechanical interactions with the ECM to keep their migration and invasiveness capacities unaltered. Statement of significanceThe paper presents a thorough study on the mechanical microenvironment in breast cancer cells during their interaction with collagen based hydrogels of different compositions. The hydrogels’ microstructure were obtained using state-of-the-art 3D microscopy, namely focused ion beam-scanning electron microscope (FIB-SEM). FIB-SEM was originally applied in this work to reconstruct complex fibered collagen microstructures within the nanometer range, to obtain key microarchitectural parameters. The mechanical microenvironment of cells was recovered using Traction Force Microscopy (TFM). The obtained results suggest that cells calibrate tractions such that they depend on mechanical, microstructural and physicochemical characteristics of the hydrogels, hence revealing a steric hindrance. We hypothesize that cancer cells studied in this paper tune their mechanical state to keep their migration and invasiveness capacities unaltered.

Colouring mechanism and firing technology of white porcelain from the Sui Dynasty (581–618) from the Xiangzhou kiln, Anyang, China

The Xiangzhou kiln was one of the first significant kilns in China to fire white porcelain and as well as the earliest one to adopt the technique of Make-up clay. It plays a very important role in the history of Chinese ceramics. Here we utilize ten pieces of Sui (581–618) white porcelain from the Xiangzhou kiln as the research objects. The chemical composition, micro-morphology, firing temperature, firing atmosphere, micro-area composition and other characteristics of white porcelain glaze were tested by energy dispersive X-ray fluorescence spectroscopy (EDXRF), laser Raman spectroscopy (LRS), optical microscope (OM), thermal dilatometer (TD), focused ion beam scanning electron microscope combined with X-ray energy spectrometer (SEM-EDS), X-ray photoelectron spectroscopy (XPS) and spectrophotometer (UV–Vis–NIR). Finally, the firing technology and colouring mechanism of the Xiangzhou white porcelain are revealed. Our study demonstrates that the relatively high content of Fe2O3 and TiO2 in the white porcelain glaze of the Xiangzhou kiln results in a milky white glaze with a slight greenish tinge. The high content of CaO and K2O in the glaze and the almost entirely glass phase of glaze layer lead to the fine grain, good transparency and gloss. Most of the white porcelain of the Xiangzhou kiln is fired at high temperature under reducing atmosphere. The Xiangzhou kiln white porcelain glaze belongs to the crystalline glaze, glaze disorderly distribution of some calcium feldspar precipitation crystals and a very small amount of quartz, calcite residual crystals, glaze bubbles are larger, the distribution of relatively dispersed. The overall colour effect of the Xiangzhou kiln white porcelain results from the combined action of the chemical colour of the body and glaze, along with structural colour.

Quantitative 3D electron microscopy characterization of mitochondrial structure, mitophagy, and organelle interactions in murine atrial fibrillation

Atrial fibrillation (AF) is the most common clinical arrhythmia, however there is limited understanding of its pathophysiology including the cellular and ultrastructural changes rendered by the irregular rhythm, which limits pharmacological therapy development. Prior work has demonstrated the importance of reactive oxygen species (ROS) and mitochondrial dysfunction in the development of AF. Mitochondrial structure, interactions with other organelles such as sarcoplasmic reticulum (SR) and T-tubules (TT), and degradation of dysfunctional mitochondria via mitophagy are important processes to understand ultrastructural changes due to AF. However, most analysis of mitochondrial structure and interactome in AF has been limited to two-dimensional (2D) modalities such as transmission electron microscopy (EM), which does not fully visualize the morphological evolution of the mitochondria during mitophagy. Herein, we utilize focused ion beam-scanning electron microscopy (FIB-SEM) and perform reconstruction of three-dimensional (3D) EM from murine left atrial samples and measure the interactions of mitochondria with SR and TT. We developed a novel 3D quantitative analysis of FIB-SEM in a murine model of AF to quantify mitophagy stage, mitophagosome size in cardiomyocytes, and mitochondrial structural remodeling when compared with control mice. We show that in our murine model of spontaneous and continuous AF due to persistent late sodium current, left atrial cardiomyocytes have heterogenous mitochondria, with a significant number which are enlarged with increased elongation and structural complexity. Mitophagosomes in AF cardiomyocytes are located at Z-lines where they neighbor large, elongated mitochondria. Mitochondria in AF cardiomyocytes show increased organelle interaction, with 5X greater contact area with SR and are 4X as likely to interact with TT when compared to control. We show that mitophagy in AF cardiomyocytes involves 2.5X larger mitophagosomes that carry increased organelle contents. In conclusion, when oxidative stress overcomes compensatory mechanisms, mitophagy in AF faces a challenge of degrading bulky complex mitochondria, which may result in increased SR and TT contacts, perhaps allowing for mitochondrial Ca2+ maintenance and antioxidant production.

Physicochemical investigation on the hard carbon interface in ionic liquid electrolyte

An investigation of the solid electrolyte interphase (SEI) on hard carbon (HC) anodes in aprotic sodium batteries was carried out by post-mortem analyses. Electrodes cycled in 1-ethyl-3-methylimidazolium bis(fluorosulfonyl)imide (EMIFSI), and N-trimethyl-N-butylammonium bis(fluorosulfonyl)imide (N1114FSI) ionic liquid electrolytes have been collected and studied: benchmark electrodes cycled in commercial organic solutions were examined for comparison purpose. The SEI composition and morphology of post-mortem HC electrodes were analyzed by X-ray Photoelectron Spectroscopy (XPS) and focused ion beam scanning electron microscopy (FIB-SEM) analysis. Overall, the HC electrodes cycled in carbonate-based electrolyte have shown thicker SEI mainly composed of organic compounds, whereas in ILs electrolytes they have shown thinner layer richer in inorganic species, such as NaF, Na2CO3, N-containing species, and “small” sulfide-based compounds, these improving the SEI interfacial properties towards the Na+ migration kinetics. Focusing on ILs based cell formulations, anodes cycled in the EMIFSI-based electrolyte shows several cracks on its surface.

The Microstructural Reconstruction of Variously Sintered Ni-SDC Cermets Using Focused Ion Beam Scanning Electron Microscopy Nanotomography.

This work focuses in-depth on the quantitative relationships between primary first-order microstructural parameters (i.e., volume fractions of various phases and particle size distribution) with the more complex second-order topological features (i.e., connectivity of phases, three-phase boundary length (TPBL), interfacial areas, or tortuosity). As a suitable model material, a cermet nickel/samaria-doped ceria (Ni-SDC) is used as an anode in a solid oxide fuel cell (SOFC). A microstructure description of nano-sized Ni-SDC cermets, fabricated at various sintering conditions from 1100 °C to 1400 °C, was performed using FIB-SEM nanotomography. The samples were serially sectioned employing a fully automated slicing procedure with active drift correction algorithms and an auto-focusing routine to obtain a series of low-loss BSE images. Advanced image processing algorithms were developed and applied directly to image data volume. The microstructural-topological relationships are crucial for the microstructure optimisation and, thus, the improvement of the corresponding electrode performance. Since all grains of individual phases (Ni, SDC, or pores) did not percolate, special attention was given to the visualisation of the so-called active TPBL. Based on the determined microstructure characteristics of the prepared Ni-SDC cermets, including simulations of gas flow and pressure drop, thermal treatment at 1200 °C was recognised as the most appropriate sintering temperature.

Identification of solid phase speciation of trace elements in dust dry deposition using focused ion beam and selected area electron diffraction

BackgroundFew studies have been conducted to identify solid phase speciation of trace elements within the interior of airborne particles, although the adverse effects of ambient particles are closely related to the speciation of toxic elements and therefore the identification of chemical binding sites and solid phase associations is essential for assessing the impacts of trace elements in ambient air on environmental quality and human health. ObjectiveA combined use of focused ion beam scanning electron microscopy (FIB-SEM) and selected area electron diffraction (SAED) patterns from transmission electron microscopy (TEM) was applied with an energy dispersive X-ray spectroscopy (EDS) to investigate the solid phase speciation of trace elements within the interior of dust dry deposition obtained from an urban area. ResultsThe study results using the high-resolution microscopic techniques for the characterization of nano- and micron-sized particles revealed lead chromate for Pb and Cr6+, barite for Ba, rutile for Ti, and calcite, gypsum, and quicklime for Ca within the carbon matrix, implying their traffic-related sources. Fe oxides were observed for Fe, Mn, Ni, and Cr3+, with cerianite and Fe-La alloys for rare earth elements (REEs). ConclusionsThree types of anthropogenic sources were inferred based on the morphology and texture of the solid phases, as well as their primary usage: traffic road marking paints for Pb, Cr6+, Ba, and Ti, cement materials for Ca, and industrial activities for Fe, Mn, Ni, Cr3+, and REEs. The presence of submicron-sized toxic metal-bearing particles in dust dry deposition indicated that the toxic metals (i.e., Pb, Cr6+) can penetrate into the respiratory system along with the nanoparticles. The study results demonstrate that the solid phase speciation of trace elements detected using FIB-SEM and TEM-SAED can be effectively utilized for the identification of sources and the assessment of chemical toxicity of atmospheric dust.

Editors’ Choice—Visualizing the Impact of the Composite Cathode Microstructure and Porosity on Solid-State Battery Performance

The kinetics of composite cathodes for solid-state batteries (SSBs) relies heavily on their microstructure. Spatial distribution of the different phases, porosity, interface areas, and tortuosity factors are important descriptors that need accurate quantification for models to predict the electrochemistry and mechanics of SSBs. In this study, high-resolution focused ion beam-scanning electron microscopy tomography was used to investigate the microstructure of cathodes composed of a nickel-rich cathode active material (NCM) and a thiophosphate-based inorganic solid electrolyte (ISE). The influence of the ISE particle size on the microstructure of the cathode was visualized by 3D reconstruction and charge transport simulation. By comparison of experimentally determined and simulated conductivities of composite cathodes with different ISE particle sizes, the electrode charge transport kinetics is evaluated. Porosity is shown to have a major influence on the cell kinetics and the evaluation of the active mass of electrochemically active particles reveals a higher fraction of connected NCM particles in electrode composites utilizing smaller ISE particles. The results highlight the importance of homogeneous and optimized microstructures for high performance SSBs, securing fast ion and electron transport.