Focused Ion Beam Scanning Electron Microscopy Research Articles

Correlating Heterogeneities in Support Fragmentation to Polymer Morphology in Metallocene‐Based Propylene Polymerization Catalysis

In the field of olefin polymerization catalysis, metallocenes are heterogenized with methylaluminoxane onto silica supports to yield active catalysts. During olefin polymerization, these silica supports act as a framework to control the fragmentation stage, thereby influencing the final polymer product and preventing reactor fouling and fines formation. This study investigates the influence of different silica supports induced on the final polymer product. To study a broad range of silica supports from an industrial silica database, we utilize a hierarchical clustering method to cluster the supports based on their physical properties. From the clustering method, five supports representing the clusters and an industrial benchmark were analyzed at different polymerization stages using Focused Ion Beam Scanning Electron Microscopy (FIB‐SEM) and Micro‐computed Tomography (MicroCT). This combined FIB‐SEM/MicroCT methodology revealed differences in both fragmentation behavior and polymer morphologies based on structural features, including macropores, mesopores, spray‐dried shells, spray‐dried spheres, and denser shells. The heterogeneity and ideal fragmentation behavior was further assessed by calculating the replication factor of each support, indicating that silica materials containing macropores and spray‐dried shells have an almost ideal replication phenomenon. This multi‐scale analysis revealed new understanding of catalyst fragmentation for different supports.

Application of Advanced Microscopy Techniques to The Characterization of Mixed Matrix Membranes.

Mixed matrix membranes (MMMs) have emerged as promising materials for various separation processes due to their tunable properties, enhanced separation performance and reproducibility. In this review paper, we provide a comprehensive overview of the methodologies, challenges, and applications associated with the characterization of MMMs using two advanced imaging techniques: Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) and Transmission Electron Microscopy (TEM). We begin by outlining the principles and capabilities of FIB-SEM and TEM, emphasizing their suitability for studying the microstructure, morphology, and composition of MMMs at nanoscale resolution. Subsequently, we discuss the specific challenges and limitations encountered in the characterization of MMMs using these techniques, including sample preparation, image acquisition, and data interpretation. Furthermore, we review the diverse applications of FIB-SEM and TEM in elucidating the structure-property relationships of MMMs. Through illustrative examples, we highlight the valuable insights gained from these imaging techniques in optimizing MMMs for various separation applications. Finally, we propose future directions and emerging trends in MMM characterization, including the integration of lasers into FIB-SEM and in situ characterization techniques, to address current challenges and push the boundaries of MMM design and performance.

High-fidelity reconstruction of porous cathode microstructures from FIB-SEM data with deep learning

Accurate modeling of lithium-ion battery (LIB) electrode microstructures provides essential references for understanding degradation mechanisms and optimizing materials. Traditional segmentation methods often struggle to accurately capture the complex microstructures of porous LIB electrodes in focused ion beam scanning electron microscopy (FIB-SEM) data. In this work, we develop a deep learning model based on the Swin Transformer to segment FIB-SEM data of a lithium cobalt oxide electrode, utilizing fused secondary and backscattered electron images. The proposed approach outperforms other deep learning methods, enabling the acquirement of 3D microstructure with reduced particle elongated artifacts. Analyses of the segmented microstructures reveal improved electrode tortuosity and pore connectivity crucial for ion and electron transport, emphasizing the necessity of accurate 3D modeling for reliable battery performance predictions. These results suggest a path toward voxel-level degradation analysis through more sensible battery simulation on high-fidelity microstructure models directly twinned from real porous electrodes.

An improved convolutional architecture for quantitative characterization of pore networks in fine-grained rocks using FIB-SEM

Focused ion beam scanning electron microscope (FIB-SEM) is one of the most advanced imaging techniques for analyzing and understanding complex pore networks in shale and other fine-grained formations. However, FIB-SEM imaging tends to be time-consuming and labor-intensive and can result in biased interpretations associated with pore analysis. Recently, U-Net or its variants for image segmentation have been applied to capture microscopic pores at higher resolutions. The ‘traditional’ encoder-decoder-based approaches tend to detect very fine-scale microscopic pores poorly. This study presents an improved convolutional architecture for automatically analyzing pore structures in shale reservoirs using FIB-SEM. It does so by applying an overcomplete convolutional architecture, KiU-Net, to capture very fine-scale microscopic pores by accurately defining their edges in the input FIB-SEM images. The KiU-Net learns low and high-level features by making the model more sensitive to fine-scale microscopic pores in the input images. The purpose of this study is to demonstrate KiU-Net's capabilities by analyzing different shale formations with varying characteristics. The results indicate that KiU-Net is more accurate and efficient than other methods in predicting nanopores in the Longmaxi, Niutitang, Qingshankou, Qianjiang, and Yanchang Formations (China), Bakken shale (Canada), and coal reservoirs (China). Furthermore, KiU-Net demonstrated the advantage of requiring fewer parameters and achieving super convergence compared to the Attention U-Net technique. KiU-Net addresses the challenges of the Edge-Threshold Automatic Processing (ETAP) methods by capturing very fine-scale microscopic pores with accurate edges. This study further enhances the accuracy and efficiency of pore analysis in shales, thereby offering an improved method for understanding shale reservoir quality with the potential to improve petroleum recovery from such formations.

The impact of pore heterogeneity on pore connectivity and the controlling factors utilizing spontaneous imbibition combined with multifractal dimensions: Insight from the Longmaxi Formation in Northern Guizhou

The heterogeneity of shale pores, a crucial factor in the occurrence and migration of shale gas, exerts a significant impact on the pore connectivity. Pores exhibiting a range of structural attributes to the complexity of pore connectivity. A comprehensive study into the impact of pore heterogeneity on pore connectivity in shale is lacking. This study aims to explore the impact of pore heterogeneity on pore connectivity in shale and the primary controlling factors of pore connectivity. Shale pore connectivity, pore structures, mineral composition, and geochemical parameters were assessed using various tests, including spontaneous imbibition, adsorption, mercury intrusion capillary pressure (MICP), focus ion beam-scanning electron microscopy (FIB-SEM), sulfur and carbon analysis, vitrinite reflectivity, and X-ray diffraction (XRD). Pore heterogeneity was quantitatively analyzed using the multifractal dimensions method. Results show that the increased heterogeneity of pore structure and surface roughness facilitating the potential for increased connectivity. The presence of well-developed micro-mesopores within the organic matter, alongside numerous disconnected and independent pores, contributes to an increase in pore heterogeneity. Micro-mesopore structures have a more pronounced impact on pore heterogeneity than macropores. The heterogeneity of the pores is predominantly influenced by variations in the PV and SSA of micro-mesopores. Furthermore, the heightened heterogeneity of pore structure (D1) and surface roughness (D2) leads to a more complex pore structure with increased roughness, promoting the potential for enhanced connectivity through additional throats and facilitating the formation of secondary microfractures. Shale cores characterized by high total organic carbon (TOC) content, porosity, and clay mineral content are conducive to improved pore connectivity. Conversely, the increase of thermal evolution maturity of shale in the over-mature stage is not conducive to the increase of pore connectivity. Thermal evolution maturity, TOC content, and clay mineral are key factors that control pore heterogeneity, further affecting the connectivity of shale pores. High pore connectivity is conducive to spontaneous imbibition capacity and the formation of hydraulic microfractures, promoting the migration of shale gas.

3D microstructure reconstruction and characterization of porous materials using a cross-sectional SEM image and deep learning

Accurate assessment of the three-dimensional (3D) pore characteristics within porous materials and devices holds significant importance. Compared to high-cost experimental approaches, this study introduces an alternative method: utilizing a generative adversarial network (GAN) to reconstruct a 3D pore microstructure. Unlike some existing GAN models that require 3D images as training data, the proposed model only requires a single cross-sectional image for 3D reconstruction. Using porous ceramic electrode materials as a case study, a comparison between the GAN-generated microstructures and those reconstructed through focused ion beam-scanning electron microscopy (FIB-SEM) reveals promising consistency. The GAN-based reconstruction technique demonstrates its effectiveness by successfully characterizing pore attributes in porous ceramics, with measurements of porosity, pore size, and tortuosity factor exhibiting notable agreement with the results obtained from mercury intrusion porosimetry.

Zygospore formation in Zygnematophyceae predates several land plant traits.

Recent research on a special type of sexual reproduction and zygospore formation in Zygnematophyceae, the sister group of land plants, is summarized. Within this group, gamete fusion occurs by conjugation. Zygospore development in Mougeotia, Spirogyra and Zygnema is highlighted, which has recently been studied using Raman spectroscopy, allowing chemical imaging and detection of changes in starch and lipid accumulation. Three-dimensional reconstructions after serial block-face scanning electron microscopy (SBF-SEM) or focused ion beam SEM (FIB-SEM) made it possible to visualize and quantify cell wall and organelle changes during zygospore development. The zygospore walls undergo strong modifications starting from uniform thin cell walls to a multilayered structure. The mature cell wall is composed of a cellulosic endospore and exospore and a central mesospore built up by aromatic compounds. In Spirogyra, the exospore and endospore consist of thick layers of helicoidally arranged cellulose fibrils, which are otherwise only known from stone cells of land plants. While starch is degraded during maturation, providing building blocks for cell wall formation, lipid droplets accumulate and fill large parts of the ripe zygospores, similar to spores and seeds of land plants. Overall, data show similarities between streptophyte algae and embryophytes, suggesting that the genetic toolkit for many land plant traits already existed in their shared algal ancestor. This article is part of the theme issue 'The evolution of plant metabolism'.

Factors Controlling Differences in Morphology and Fractal Characteristics of Organic Pores of Longmaxi Shale in Southern Sichuan Basin, China

Shale gas is a prospective cleaner energy resource and the exploration and development of shale gas has made breakthroughs in many countries. Structure deformation is one of the main controlling factors of shale gas accumulation and enrichment in complex tectonic areas in southern China. In order to estimate the shale gas capacity of structurally deformed shale reservoirs, it is necessary to understand the systematic evolution of organic pores in the process of structural deformation. In particular, as the main storage space of high-over-mature marine shale reservoirs, the organic matter pore system directly affects the occurrence and migration of shale gas; however, there is a lack of systematic research on the fractal characteristics and deformation mechanism of organic pores under the background of different tectonic stresses. Therefore, to clarify the above issues, modular automated processing system (MAPS) scanning, low-pressure gas adsorption, quantitative evaluation of minerals by scanning (QEMSCAN), and focused ion beam scanning electron microscopy (FIB-SEM) were performed and interpreted with fractal and morphology analyses to investigate the deformation mechanisms and structure of organic pores from different tectonic units in Silurian Longmaxi shale. Results showed that in stress concentration areas such as around veins or high-angle fractures, the organic pore length-width ratio and the fractal dimension are higher, indicating that the pore is more obviously modified by stress. Under different tectonic backgrounds, the shale reservoir in Weiyuan suffered severe denudation and stronger tectonic compression during burial, which means that the organic pores are dominated by long strip pores and slit-shaped pores with high fractal dimension, while the pressure coefficient in Luzhou is high and the structural compression is weak, resulting in suborbicular pores and ink bottle pores with low fractal dimension. The porosity and permeability of different forms of organic pores are also obviously different; the connectivity of honeycomb pores with the smallest fractal dimension is the worst, that of suborbicular organic pores is medium, and that of long strip organic pores with the highest fractal dimension is the best. This study provides more mechanism discussion and case analysis for the microscopic heterogeneity of organic pores in shale reservoirs and also provides a new analysis perspective for the mechanism of shale gas productivity differences in different stress–strain environments.

Rapid on-site nondestructive surface corrosion characterization of sintered nanocopper paste in power electronics packaging using hyperspectral imaging

Sintered nanocopper (nanoCu) paste, exhibiting excellent electrical, thermal, and mechanical performances, offers promise for interconnections in wide bandgap (WBG) semiconductors operating at higher temperatures. However, sintered nanoCu is prone to severe corrosion in environments containing H2S, with on-site characterization methods for the composition of corrosion products currently lacking. In this study, a novel method was proposed for the rapid characterization of corrosion products during the corrosion process based on hyperspectral imaging (HSI) technology. Sintered nanoCu samples were subjected to 336 h H2S gas corrosion tests with bulk Cu as the reference, followed by correlating the corrosion element content with hyperspectral characteristic parameters. Then, the morphology and composition of corrosion products were researched using focused ion beam scanning electron microscope (FIB-SEM) and transmission electron microscope (TEM) analysis. The results showed that (1) during the corrosion process, a linear relationship was established between the Cu, O elemental atomic contents on the sample surfaces and their hyperspectral characteristic parameters. (2) The elemental atomic content of S exhibited an exponential relationship with the characteristic parameter. (3) The change rate in the spectral characteristic parameters during the corrosion process reflected the severity of corrosion, which was confirmed by comparing the thickness of the corrosion products of the sintered nanoCu and bulk Cu. This study offers a foundation for the further investigation of rapid on-site characterization of sintered nanoCu corrosion involving H2S.

Advanced multi-scale characterization of loess microstructure: Integrating μXCT and FIB-SEM for detailed fabric analysis and geotechnical implications

Loess, a Quaternary wind-blown deposit, is a problem soil that gives rise to frequent geohazards such as landslides and water-induced subsidence. The behaviour of loess is controlled by its microstructure, consisting of silt-sized skeleton particles and complex bonding structures formed by clay-sized particles. Achieving a deep understanding and precise modelling of loess behaviour necessitates comprehensive knowledge of the realistic 3D microstructure. In this paper, a correlative investigation of the 3D loess microstructure is performed using X-ray micro-computed tomography (μXCT) and focused ion beam scanning electron microscope (FIB-SEM). Details of clay structures in loess, such as clay coatings, clay bridges and clay buttresses, are visualized and characterized in 3D based on FIB-SEM images with a voxel size of 10 × 10 × 10 nm3. The clay structures exhibit a diverse degree of complexity and their impact on the mechanical properties of loess is highlighted. Statistical analysis of the skeleton particles, including size, shape and orientation, are derived from μXCT images with a voxel size of 0.7 × 0.7 × 0.7 μm3. The findings provide insights into the collapse mechanism and particle-scale modelling of loess. The combination of μXCT and FIB-SEM proves to be a powerful approach for characterizing the intricate micro-structures of loess, as well as other geomaterials.

Characterization of human trabecular bone across multiple length scales using a correlative approach combining X-ray tomography with LaserFIB and plasma FIB-SEM

Three-dimensional correlative multimodal and multiscale imaging is an emerging method for investigating the complex hierarchical structure of biological materials such as bone. This approach synthesizes images acquired across multiple length scales, for the same region of interest, to provide a comprehensive view of the material structure of a sample. Here, we develop a workflow for the structural analysis of human trabecular bone using a femtosecond laser to produce a precise grid to facilitate correlation between imaging modalities and identification of structures of interest, in this case, a single trabecula within a volume of trabecular bone. Through such image registration, high resolution X-ray microscopy imaging revealed fine architectural details, including the cement sheath and bone cell lacunae of the selected bone trabecula. The selected bone volume was exposed with a combination of manual polishing and site-specific femtosecond laser ablation and then examined with plasma focused ion beam-scanning electron microscopy. This reliable and versatile correlation approach has the potential to be applied to a variety of biological tissues and traditional engineered materials. The proposed workflow has the enhanced capability for generating highly resolved and broadly contextualized structural data for a better understanding of the architectural features of a material spanning its macroscopic to nanoscopic levels.

Volume electron microscopy reveals 3D synaptic nanoarchitecture in postmortem human prefrontal cortex.

Synaptic function is directly reflected in quantifiable ultrastructural features using electron microscopy (EM) approaches. This coupling of synaptic function and ultrastructure suggests that in vivo synaptic function can be inferred from EM analysis of ex vivo human brain tissue. To investigate this, we employed focused ion beam-scanning electron microscopy (FIB-SEM), a volume EM (VEM) approach, to generate ultrafine-resolution, three-dimensional (3D) micrographic datasets of postmortem human dorsolateral prefrontal cortex (DLPFC), a region with cytoarchitectonic characteristics distinct to human brain. Synaptic, sub-synaptic, and organelle measures were highly consistent with findings from experimental models that are free from antemortem or postmortem effects. Further, 3D neuropil reconstruction revealed a unique, ultrastructurally-complex, spiny dendritic shaft that exhibited features characteristic of heightened synaptic communication, integration, and plasticity. Altogether, our findings provide critical proof-of-concept data demonstrating that ex vivo VEM analysis is an effective approach to infer in vivo synaptic functioning in human brain.

Video frame interpolation neural network for 3D tomography across different length scales

Three-dimensional (3D) tomography is a powerful investigative tool for many scientific domains, going from materials science, to engineering, to medicine. Many factors may limit the 3D resolution, often spatially anisotropic, compromising the precision of the information retrievable. A neural network, designed for video-frame interpolation, is employed to enhance tomographic images, achieving cubic-voxel resolution. The method is applied to distinct domains: the investigation of the morphology of printed graphene nanosheets networks, obtained via focused ion beam-scanning electron microscope (FIB-SEM), magnetic resonance imaging of the human brain, and X-ray computed tomography scans of the abdomen. The accuracy of the 3D tomographic maps can be quantified through computer-vision metrics, but most importantly with the precision on the physical quantities retrievable from the reconstructions, in the case of FIB-SEM the porosity, tortuosity, and effective diffusivity. This work showcases a versatile image-augmentation strategy for optimizing 3D tomography acquisition conditions, while preserving the information content.

Tuning α precipitation via post-heat treatments in direct energy deposited metastable β Ti-5Al-5Mo-5V-3Cr alloy and its impact on mechanical properties

In this study, the strength and ductility of a direct energy deposited (DEDed) metastable β Ti-5Al-5Mo-5 V-3Cr (wt%, Ti-5553) alloy was explored by tuning the formation of various α microstructures through post-heat treatments. The microstructure of DEDed Ti-5553 with and without post-heat treatments was systematically studied using scanning electron microscopy, three-dimensional (3D) focused ion beam-scanning electron microscopy tomography, transmission electron microscopy, scanning transmission electron microscopy, and atom probe tomography. Nanoscale ω phase and O′ phase particles were observed in the as-built DEDed Ti-5553 without post-heat treatment for the first time. By altering the aging temperatures and heating rates during post-heat treatments, various microstructural evolution pathways were activated, leading to α microstructures with different sizescales, morphologies, and number densities. By fast heating and isothermal aging at 600°C for 2 hours, refined α microstructure was formed through the pseudospinodal decomposition mechanism. While slow heating (at the heating rates of 5 °C/min or 0.5 °C/min) to 600°C and isothermal aging for 2 hours, super-refined α microstructures were produced respectively, primarily via ω-assisted and O′-assisted α precipitation mechanisms. By fast heating to and isothermal aging at 700°C, fine-scaled intragranular α microstructure was formed, dramatically different in morphology and sizescale from the coarse α microstructure formed in the casted Ti-5553, which is suspected to be related to the indirect influence of nanoscale isothermal ω phase particles formed during the DED process and the excess oxygen introduced during the DED process. With fast heating to and isothermal aging at 800°C, coarse α microstructure forms through the classical nucleation and growth mechanism. Various α microstructures led to a drastic change of mechanical properties with improvements up to a 55 % increase in hardness and 92 % increase in tensile yield strength, compared with as-built DEDed Ti-5553. Our work indicates the feasibility of achieving tailored mechanical properties in DEDed metastable β-Ti alloys by tuning α microstructures through selectively activating various phase transformation mechanisms via post-heat treatments.

Chronic undernutrition impairs renal mitochondrial respiration accompanied by intense ultrastructural damage in juvenile rats

This study investigated whether chronic undernutrition alters the mitochondrial structure and function in renal proximal tubule cells, thus impairing fluid transport and homeostasis. We previously showed that chronic undernutrition downregulates the renal proximal tubules (Na++K+)ATPase, the main molecular machine responsible for fluid transport and ATP consumption. Male rats received a multifactorial deficient diet, the so-called Regional Basic Diet (RBD), mimicking those used in impoverished regions worldwide, from weaning to a juvenile age (3 months). The diet has a low content (8 %) of poor-quality proteins, low lipids, and no vitamins compared to control (CTR). We investigated citrate synthase activity, mitochondrial respiration (oxygraphy) in phosphorylating and non-phosphorylating conditions with different substrates/inhibitors, potential across the internal membrane (Δψ), and anion superoxide/H2O2 formation. The data were correlated with ultrastructural alterations evaluated using transmission electron microscopy (TEM) and focused ion beam scanning electron microscopy (FIB-SEM). Citrate synthase activity decreased (∼50 %) in RBD rats, accompanied by a similar reduction in respiration in non-phosphorylating conditions, maximum respiratory capacity, and ATP synthesis. The Δψ generation and its dissipation after carbonyl cyanide-4-(trifluoromethoxy) phenylhydrazone remained unmodified in the survival mitochondria. H2O2 production increased (∼100 %) after Complex II energization. TEM demonstrated intense matrix vacuolization and disruption of cristae junctions in a subpopulation of RBD mitochondria, which was also demonstrated in the 3D analysis of FIB-SEM tomography. In conclusion, chronic undernutrition impairs mitochondrial functions in renal proximal tubules, with profound alterations in the matrix and internal membrane ultrastructure that culminate with the compromise of ATP supply for transport processes.

Correlative Microscopy Analysis for Battery Materials

Lithium batteries (LB) are in high demand for a diverse range of applications, such as automotive industry, consumer electronics, wearable and medical devices, grid storage, etc. Each application demands a specific set of performance advantages, such as high capacity and/or energy density, long cycle life, superior electrochemical stability. Therefore, there is no one-size-fits-all for a LB chemistry and its form factor. Battery performance advantages rely on optimization of the battery components, including active materials, electrolyte, separator, binder system, and current collectors. For meaningful device optimization, electrochemical battery testing needs to be combined with a deep understanding of the material and device microstructure. Physical and chemical characterization on the material- and electrode-level is needed to establish root-cause relationships with battery performance. Properties of the interfaces between layers of the battery components often define the device characteristics. Critical information is usually buried beneath the surface of a material specimen or encapsulated in a closed-form device. Microstructural defect identification in the battery needs to be followed by a targeted defect study. Different battery form factors and chemistries make it hard to streamline root-cause analysis.Recently, a commercial focused-ion beam scanning electron microscope was developed with an integrated fs-laser mill attached to the load lock of the microscope, opening the door to new and more powerful analysis approaches in energy materials research. Applications include rapid access to deeply buried structures for high resolution imaging and analytics, large area cross-section preparation, and massive material ablation for sample preparation of structures; e.g. FIB-SEM tomography, TEM, APT, or X-ray nanoCT. Additionally, each of these methods may be correlatively guided by prior imaging, with techniques like 3D X-ray microscopy (XRM), to enable targeted analysis and preparation. The non-destructive nature of 3D XRM makes it an ideal tool for microstructural defect identification in LB. Laser mill allows researchers to combine non-destructive X-ray defect identification with electron microscopy methods for targeted defect characterization. This approach can be used for various battery types and form factors.By combining the laser mill with 3D X-ray microscopy, this platform enables comprehensive analysis of energy materials at the nanoscale. We illustrate these concepts with application examples, and use cases demonstrating the utility of the approach.

Mass Transport Regimes in a CO2R Gas Diffusion Electrode Pore with Coupled Microkinetics Model

Gas Diffusion Electrodes (GDEs) have arisen as a popular CO2 electrolyser configuration due to the improved mass transfer properties and higher current densities possible in comparison to a liquid-fed system. In this work, we aim to understand the mass transport regimes in a single liquid-filled pore of a GDE, i.e., an idealized model of the porous catalyst layer. In previous work, Butler-Volmer (BV) expressions have been used to model the CO evolution reaction and the Hydrogen Evolution Reaction (HER). In this study, we extend that in a few ways: (1) a MicroKinetic Model (MKM) of Au at the surface of the electrode is used instead of the BV expressions, (2) volume/steric effects are incorporated through the Generalized Modified Poisson-Nerst-Planck (GMPNP) equation, and (3) more reactions are considered in the electrolyte. By analyzing pores of varying sizes, following the size distribution measured by Focused Ion Beam Scanning Electron Microscopy (FIB/SEM) in a GDE from the literature, we assess conditions where concentration profiles are no longer effectively one-dimensional in the pore axis. We discuss how these three-dimensional mass transfer effects impact CO2 conversion efficiency. In such regimes, we describe why special treatment is required when calling BV expressions in macroscale pore-averaged models.This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344. LLNL release number: LLNL-ABS-858384.

Understanding the Phenomenon of High Temperature Hydrogen Attack (HTHA) Responsible for Ferrito-Pearlitic Steels Damage

This article focuses on the fine characterization of steels commonly used in the petrochemical industry damaged by the phenomenon of high temperature hydrogen attack (HTHA). The study was conducted in two steps. To begin with, a damaged 0.5-Mo pearlitic steel from the petroleum refineries, submitted to HTHA for decades, was characterized in detail using multiscale electron microscopy techniques. As part of an upstream study to better understand the onset and the growth of cavities, a brand new SA516 grade 60 low carbon–manganese steel was subsequently exposed to accelerated HTHA conditions through interrupted cycles carried out in autoclaves and then examined. Numerous cavities, plausibly filled with methane, were noticed in both materials. These cavities were mostly located at ferrite–pearlite grain boundaries along carbides and at triple grain boundaries near large carbides. The 0.5-Mo pearlitic steel showed cavities reaching significant sizes, up to 1 µm, but surprisingly no cracks were observed in the depth of the pipe. The major outcome is that 3D focused ion beam–scanning electron microscopy combined with transmission electron microscopy (TEM) analyses unveiled different natures of precipitates as well as in and nearby HTHA cavities for both 0.5-Mo and low carbon–manganese steels. Inclusions, likely AlN, but also Mo- and Cu-rich precipitates were observed in cavities of the industrial steel. These results confirmed a previous study performed on a similar industrial steel that drew a possible correlation between cavities nucleation and the intersection of transgranular inclusion-enriched plane with a grain boundary or carbides in pearlite grains (Flament in Microscopy and Microanalysis 28:1602–1604, 2022).

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.

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.