Search

The effects of isothermal annealing on the self-assembled nanostructures of spinel manganese oxide ZnMnGaO4 were investigated using transmission electron microscopy and x-ray diffraction. The checkerboard nanostructures and zigzag nanostructures (named "Sierra" nanostructures) coexisted owing to the chemical phase separation of Mn3+ and Ga3+ ions by isothermal annealing at 575 °C. It was observed that the checkerboard nanostructures were dominant in short-time annealing and that the volume fraction of the Sierra nanostructures became more prominent as the annealing period increase. The interdiffusion of Mn3+ and Ga3+ is indicated to play an important role in gaining the total energy of the system by the reduction in the local strain caused by the formation of nanostructures. These results provide further insights into the fabrication of distinct types of nanostructures in complex transition-metal compounds. [ABSTRACT FROM AUTHOR]

The effects of isothermal annealing on the self-assembled nanostructures of spinel manganese oxide ZnMnGaO4 were investigated using transmission electron microscopy and x-ray diffraction. The checkerboard nanostructures and zigzag nanostructures (named "Sierra" nanostructures) coexisted owing to the chemical phase separation of Mn3+ and Ga3+ ions by isothermal annealing at 575 °C. It was observed that the checkerboard nanostructures were dominant in short-time annealing and that the volume fraction of the Sierra nanostructures became more prominent as the annealing period increase. The interdiffusion of Mn3+ and Ga3+ is indicated to play an important role in gaining the total energy of the system by the reduction in the local strain caused by the formation of nanostructures. These results provide further insights into the fabrication of distinct types of nanostructures in complex transition-metal compounds. [ABSTRACT FROM AUTHOR]

The article focuses on the growing demand for high-performance computing (HPC) driven by artificial intelligence and machine learning, leading to complex packaging challenges. Topics include the rise of heterogeneous integration and chiplet architectures, the application of 3D x-ray microscopy for nondestructive failure analysis, and the integration of AI models to enhance fault detection and process validation.

The importance of comprehensive multiscale characterisation in advancing our understanding of engineering materials is undeniable but remains a challenging pursuit. Combining complimentary microstructure characterisation techniques, including transmission electron microscopy, electron backscatter diffraction and dark-field X-ray microscopy (DFXM), the formation of deformation microstructures is investigated in presence of shearable and non-shearable hardening precipitates in an industrial aluminium alloy (AA) 2024 (Al–Cu–Mg family). The alloy was used in naturally aged T3 (with shearable co-clusters and Guinier–Preston–Bagaryatsky (GPB) zones) and peak-hardened T8 (with non-shearable S-phase precipitates) states. After cold rolling with thickness reductions varying from 25 to 60% (or corresponding von Mises strain from 0.33 to 1.06), the T8 state revealed a higher sub-boundary density with slightly smaller mean disorientation angle, as compared to those in the T3 state. At a von Mises strain of 0.33, the T8 state exhibited higher long-range orientation gradients, as compared to the T3 state, for higher strain orientation gradients in T3 surpass those in T8 state. With DFXM, distinct 3D substructures are shown, revealing ellipsoidal sub-grains in the T8 state and pancake-like sub-grains in the T3 state. Moreover, the stored energy induced by cold rolling is higher for the T8 state. These results indicate different deformation microstructures, formed in the same AA2024 but hardened by shearable and non-shearable precipitates. [ABSTRACT FROM AUTHOR]

This paper presents the authentication analysis of a bronze bust of Napoleon I, attributed to the Italian artist Renzo Colombo (1856–1885) based on his signature and other casting and molding inscriptions. The bust was made using the lost wax technique and artificially patinated in the Pinédo variant workshop. This study combined historiographical research (using the specialized literature) with data from auction catalogs. These were compared with photographs of the entire bust and close-up images of key areas, including anthropomorphic features, clothing, inscriptions, and structural and ornamental details. The condition of the bust and its historical and chemical characteristics were assessed through direct analysis with magnifying tools and indirect analysis using scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX). [ABSTRACT FROM AUTHOR]

The surface quality of the substrate has an important effect on the quality of the growth film. The roughness, uniformity, adhesion residue and oxide layer of the substrate are the evaluation criteria of its surface performance. In this paper, an in-situ thermal treatment method to remove the natural oxides on GaSb (001) substrates for epitaxial growth of CdZnTe films by close-spaced sublimation method was reported. By controlling the temperature and time of the thermal treatment, a clean and smooth substrate state is obtained. The effect of thermal treatment on the morphology and composition of GaSb substrate was analyzed by atomic force microscopy and X-ray photoelectron spectroscopy. The crystal quality of CdZnTe epitaxial film grown on GaSb substrate after thermal treatment was evaluated by double crystal X-ray curve. In order to further study the properties and epitaxial formation mechanism of the micro-defects near the heterogeneous interface, TEM analysis of CdZnTe/GaSb cross section was also carried out. After 180 s thermal treatment at 600 ℃, the GaSb substrate can obtain a clean and relatively flat surface after most of the oxide is removed from the substrate surface, thus improving the crystallization quality of CdZnTe epitaxial film. The full width of half maximum of double crystal X-ray curve is 94″, which approached the crystalline quality of bulk CdZnTe crystal ever reported. [ABSTRACT FROM AUTHOR]

This paper presents the first effort to unravel and quantify the strengthening of a shale induced by nanoparticle injection from the perspectives of cross-scale and multi-constituent mechanical properties. After being subject to injection of pure water and an aqueous suspension of carbon black nanoparticle of ~ 50 nm in diameter under a differential pressure of 850 kPa, the shale specimens were characterized by big data nanoindentation (BDNi) to probe the mechanical properties of both individual constituents at the microscale and the bulk rock at the macroscale, leading to comparatively assessing the effects of injecting pure water and aqueous nanoparticle suspension on the mechanical properties. Microstructural characterization by electron microscopy and X-ray computed tomography validates the successful injection of nanoparticles into the microcracks and micropores of the rock. While the nanoparticles can infiltrate to depths of up to 100 s μm in zones with densely populated microcracks, the maximum depths of injection in crack-free zones are only 2–5 μm. Moreover, the injected nanoparticles mostly act as inert fillers in the interconnected micropores and microcracks but can seldom enter the isolated micropores. Comparison of the BDNi results from pure water versus nanoparticle-injected specimens shows that the Young's modulus of the clay matrix experiences the highest increase by 23.1%, while the counterpart of non-porous quartz the lowest by 12.8%. Overall, the bulk shale's Young's modulus increases by 21.5%. Such data are consistent with the microcharacterization results that the injected nanoparticles mainly remain in the micropores and microcracks within the clay matrix. Owing to their hydrophobic nature, the carbon black nanoparticles have little effect on the rock's hardness. The findings can shed light on the practical applications of nanoparticle injection for improved wellbore stability in shale formations. [ABSTRACT FROM AUTHOR]

Iron redistribution in the intestine after total body irradiation is an established phenomenon. However, in the literature, there are no reports about the use of X-ray fluorescence microscopy or equivalent techniques to generate semi-quantitative 2D maps of iron in sectioned intestine samples from irradiated mice. In this work, we used X-ray fluorescence microscopy (XFM) to map the elemental content of iron as well as phosphorus, sulfur, calcium, copper and zinc in tissue sections of the small intestine from eight-week-old BALB/c male mice that developed gastrointestinal acute radiation syndrome (GI-ARS) in response to exposure to 8 Gray of gamma rays. Seven days after irradiation, we found that the majority of the iron is localized as hot spots in the intercellular regions of the area surrounding crypts and stretching between the outer perimeter of the intestine and the surface cell layer of villi. In addition, this study represents our current efforts to develop elemental cell classifiers that could be used for the automated generation of regions of interest for analyses of X-ray fluorescence maps. Once developed, such a tool will be instrumental for studies of effects of radiation and other toxicants on the elemental content in cells and tissues. While XFM studies cannot be conducted on living organisms, it is possible to envision future scenarios where XFM imaging of single cells sloughed from the human (or rodent) intestine could be used to follow up on the progression of GI-ARS. [ABSTRACT FROM AUTHOR]

In this work, we present a new defect localization capability on wafer-level chip-scale packages with small-scale Cu pillars using advanced 3D X-ray microscopy. In comparison with conventional microcomputed tomography (micro-CT) flat-panel technology, the synchrotron-based optically enhanced 3D X-ray microscopy can detect very small defects with submicron resolutions. Three case studies on actual failures (one from the assembly process and two from reliability testing) will be discussed to demonstrate this powerful defect localization technique. Using the tool has helped speed up the failure analysis process by locating the defects nondestructively in a matter of hours instead of days or weeks as needed with destructive physical failure analysis. [ABSTRACT FROM AUTHOR]

This paper presents advanced workflows that combine 3D X-ray microscopy (XRM), nanoscale tomography, and deep learning (DL) to generate a detailed visualization of the interior of electronic devices and assemblies to enable the study of internal components for failure analysis (FA). Newly developed techniques, such as the integration of DL-based algorithms for 3D image reconstruction to improve scan quality through increased contrast and denoising, are also discussed in this article. In addition, a DL-based tool called DeepScout is presented. DeepScout uses 3D XRM scans in targeted regions of interest as training data for upscaling high-resolution in a low-resolution dataset, of a wider field of view, using a neural network model. Ultimately, these workflows can be run independently or complementary to other multiscale correlative microscopy evaluations, e.g., electron microscopy, and they will provide valuable insights into the inner workings of electronic packages and integrated circuits at multiple length scales, from macroscopic features on electronic devices (i.e., hundreds of mm) to microscopic details in electronic components (in the tens of nm). Understanding advanced electronic systems through X-ray imaging and machine learning—perhaps complemented with some additional correlative microscopy investigations—can speed development time, increase cost efficiency, and simplify FA and quality inspection of printed circuit boards (PCBs) and electronic devices assembled with new emerging technologies. [ABSTRACT FROM AUTHOR]

The Cu-24Zn-6Al-4Mn-3Fe alloy is mainly used for the manufacture of sliding bushings in the agricultural sector due to its high mechanical properties in the cast state. Understanding how the casting thermal parameters affect the microstructure and impact the properties of alloys is fundamental to optimizing manufacturing processes and improving performance during their application. In this study, the Cu-24Zn-6Al-4Mn-3Fe alloy was unidirectionally solidified under non-steady heat flow conditions using a water-cooled graphite base for heat exchange. Seven points were monitored along the longitudinal region of this ingot, and the data to obtain the solidification variables were extracted using an acquisition system. The cooling rates varied from 4.50 °C/s to 0.22 °C/s from the closest to the furthest position from the heat extraction point. The microstructure was analyzed via optical microscopy, scanning electron microscopy and X-ray diffraction in order to characterize the phases and intermetallic elements present in the material. The mechanical properties were evaluated through hardness and microhardness tests throughout longitudinal extension of the solidified part. The results showed an increase in hardness and microhardness with a decrease in the cooling rate, which may be related to the increase in size and the κ phase fraction with a decrease in the cooling rate, as analyzed via optical microscopy and scanning electron microscopy. Furthermore, in all positions, there was no significant change in the amount of the α phase retained, with the matrix being mainly composed of the β phase and a small content of approximately 2% of the α phase. [ABSTRACT FROM AUTHOR]

To prevent zinc (Zn) dendrite formation and improve electrochemical stability, it is essential to understand Zn dendrite growth, particularly in terms of morphology and relation with the solid electrolyte interface (SEI) film. In this study, we employ in-situ scanning transmission X-ray microscopy (STXM) and spectro-ptychography to monitor the morphology evolution of Zn dendrites and to identify their chemical composition and distribution on the Zn surface during the stripping/plating progress. Our findings reveal that in 50 mM ZnSO4, the initiation of moss/whisker dendrites is chemically controlled, while their continued growth over extended cycles is kinetically governed. The presence of a dense and stable SEI film is critical for inhibiting the formation and growth of Zn dendrites. By adding 50 mM lithium chloride (LiCl) as an electrolyte additive, we successfully construct a dense and stable SEI film composed of Li2S2O7 and Li2CO3, which significantly improves cycling performance. Moreover, the symmetric cell achieves a prolonged cycle life of up to 3900 h with the incorporation of 5% 12-crown-4 additives. This work offers a strategy for in-situ observation and analysis of Zn dendrite formation mechanisms and provides an effective approach for designing high-performance Zn-ion batteries. Understanding the evolution of Zn dendrites during cycling is crucial for development of Zn batteries. Here, authors employ in situ scanning transmission X-ray microscopy to identify the chemical origins of Zn dendrite formation and propose an electrolyte additive strategy to prolong cycle life. [ABSTRACT FROM AUTHOR]

The efficient excitation of spin waves is a key challenge in the realization of magnonic devices. We demonstrate current-driven generation of spin waves in antiferromagnetically coupled magnetic vortices. We use time-resolved x-ray microscopy to directly image the emission of spin waves upon the application of alternating currents flowing directly through the magnetic stack. Micromagnetic simulations allow us to identify the current-driven Oersted field as the main origin of excitation, in contrast to spin-transfer torques. In our case, these internal Oersted fields have an orders of magnitude higher spin-wave excitation efficiency than commonly used stripline antennas. For magnetostrictive materials, we furthermore demonstrate that the direction of magnon propagation can be steered by increasing the excitation amplitude, which modifies the underlying magnetization profile through an additional anisotropy. The demonstrated methods allow for the efficient and tunable excitation of spin waves, marking a substantial advance concerning the design of magnonic devices. [ABSTRACT FROM AUTHOR]

Lithium dendrite growth in inorganic solid-state electrolytes acts as a main stumbling block for the commercial development of all-solid-state lithium batteries. Indeed, Li dendrites often lead to solid-state electrolyte fractures, undermining device integrity and safety. Despite the significance of these issues, the mechanisms driving the solid-state electrolyte fracture process at the microscopic level remain poorly understood. Here, via operando optical and ex situ dark field X-ray microscopy measurements of LiSn∣single-crystal Li6.5La3Zr1.5Ta0.5O12∣LiSn symmetric cells, we provide insights into solid-state electrolyte strain patterns and lattice orientation changes associated with dendrite growth. We report the observation of dislocations in the immediate vicinity of dendrite tips, including one instance where a dislocation is anchored directly to a tip. This latter occurrence in single-crystalline ceramics suggests an interplay between dendrite proliferation and dislocation formation. We speculate that the mechanical stress induced by dendrite expansion triggers dislocation generation. These dislocations seem to influence the fracture process, potentially affecting the directional growth and branching observed in lithium dendrites. Lithium dendrite growth in solid-state electrolytes is a significant challenge for next-generation battery development. Here, authors used dark-field X-ray microscopy to investigate dislocations near dendrite tips, suggesting that stress-induced dislocation may influence dendrite branching and material fracture. [ABSTRACT FROM AUTHOR]

Copper(I) thiocyanate (CuSCN) is considered an efficient HTL of low cost and with high stability in perovskite solar cells (PSCs). However, the diethyl sulfide solvent used for CuSCN preparation is known to cause damage to the underlying perovskite layer in n-i-p PSCs. Antisolvent treatment of CuSCN during spin-coating can effectively minimize interfacial interactions. However, the effects of antisolvent treatment are not sufficiently understood. In this study, the effects of five different antisolvents were investigated. Scanning electron microscopy and X-ray diffraction analyses showed that the antisolvent treatment improved the crystallinity of the CuSCN layer on the perovskite layer and reduced damage to the perovskite layer. However, X-ray and ultraviolet photoelectron spectroscopy analyses showed that antisolvent treatment did not affect the chemical bonds or electronic structures of CuSCN. As a result, the power conversion efficiency of the PSCs was increased from 14.72% for untreated CuSCN to 15.86% for ethyl-acetate-treated CuSCN. [ABSTRACT FROM AUTHOR]

Scanning transmission electron microscopy (STEM) and X-ray photoelectron spectroscopy analyses were combined to clarify the ultraviolet light-induced surface changes of WO3 in air. Identical-location STEM (IL-STEM) analysis showed that the WO3 particle surface was covered with an amorphous thin film after ultraviolet irradiation in air. X-ray photoelectron spectroscopy analysis showed that hydrocarbon decomposition and the formation of carboxyl/hydroxyl species occurred. These results suggested that the amorphous thin films consisted of photocatalytic oxidative species of hydrocarbon. The IL-STEM analysis could detect small light-induced changes. This technique will be useful for the microscopic characterization of photocatalysis or photoinduced hydrophilic conversion. [ABSTRACT FROM AUTHOR]

The paper presents the results of studying the structure and phase state of tungsten and tungsten-copper alloy after pulsed action of compression plasma flows and irradiation with helium ions. The compression plasma flows were used to modify the surface layer of tungsten, as well as to create an alloy based on tungsten and copper. Using scanning electron microscopy and X-ray structural analysis, the formation of radiation defects on the tungsten surface was detected in the form of local areas of exfoliation and destruction, which begin to form at helium ion irradiation doses of 2 × 1017 cm−2. It is shown that preliminary plasma treatment of the surface in the melting mode leads to the complete disappearance of surface radiation defects up to a dose of 2 × 1017 cm−2, which may be associated with the formation of a fine-crystalline grain structure, the intergranular boundaries of which serve as effective sinks for primary radiation defects. [ABSTRACT FROM AUTHOR]

Imaging with multiple modalities can maximise the information gained from the analysis of a single sample. probes for optical fluorescence and X-ray fluorescence microscopy based on brominated 4-amino-1,8-naphthalimide and BODIPY scaffolds have been successfully designed and synthesised. Herein we show that these prototype probes, based on each of these scaffolds, can be imaged in two different cancer cell lines, and that the respective optical fluorescence and X-ray fluorescence signals are well correlated in these images. [ABSTRACT FROM AUTHOR]

The structure of four-layer coatings with a total thickness of 9 mm made of high-speed molybdenum steel S2-9-2 (W2Mo9Al) was studied. The coatings were obtained on a substrate of 41CrMo4 (30CrMnSi) steel by plasma cladding using a powder wire in a mixture of argon and nitrogen. The structure of the coating was studied by electron microscopy and energy-dispersive x-ray spectroscopy (EDS) on sample sections. It is shown that the microhardness of the deposited layer varies in the range of 5.2 – 6.6 GPa. This is due to the formation of an inhomogeneous structure in the deposited layer consisting of grains of an iron-based solid solution, at the joints and along the boundaries of which are inclusions of eutectic enriched mainly with Mo, Cr, and W. Grain sizes vary between 5 and 20 μm. A sub-grain structure is observed in the grain volume, indicating substructural hardening of the deposited layer. The sizes of the sub-grains vary between 1.5 and 2.5 μm. The layer of the alloy S2-9-2 deposited on 41CrMo steel exhibits a framework-like structure. The main alloying elements of the clad layer are Fe, Mo, Cr, W, and Al. [ABSTRACT FROM AUTHOR]

Automated mineralogy is a software addition usually seen on scanning electron microscopes designed to provide rapid insight into sample chemistry and texture in routine petrology workflows. The specific purpose of automated mineralogy is to provide mineral classifications to uniquely identified phases typically using energy dispersive spectroscopy, thus removing laborious and time‐consuming human input for routine tasks. These mineral classifications can then be applied to image data to quantify which mineral is associated with any particular texture. Automated mineralogy systems were primarily designed to generate quantitative textural analysis of particle samples to the mining industry and have remained a critical technique in this setting for the last several decades. Automated mineralogy has become more widely used in academia, and this has changed the focus of the technique, applying it to a broader range of workflows and applications. Here we show petrology examples focussing where combined geochemical and textural analysis are widely used. Critically, the use of quantitative geochemical data means that mineral classifications are based on their quantitatively measured chemistry. By making both the chemical and textural analysis quantitative, automated mineralogy can become highly flexible and provide a unique system for petrologists in both industry and academia. [ABSTRACT FROM AUTHOR]

In this study, we investigate the impact of O2 plasma treatment on the performance of Al/TaOX/Al-based resistive random-access memory (RRAM) devices, focusing on applications in neuromorphic systems. Comparative analysis using scanning electron microscopy and X-ray photoelectron spectroscopy confirmed the differences in chemical composition between O2-plasma-treated and untreated RRAM cells. Direct-current measurements showed that O2-plasma-treated RRAM cells exhibited significant improvements over untreated RRAM cells, including higher on/off ratios, improved uniformity and distribution, longer retention times, and enhanced durability. The conduction mechanism is investigated by current–voltage (I–V) curve fitting. In addition, paired-pulse facilitation (PPF) is observed using partial short-term memory. Furthermore, 3- and 4-bit weight tuning with auto-pulse-tuning algorithms was achieved to improve the controllability of the synapse weight for the neuromorphic system, maintaining retention times exceeding 103 s in the multiple states. Neuromorphic simulation with an MNIST dataset is conducted to evaluate the synaptic device. [ABSTRACT FROM AUTHOR]

This study presents a novel approach to synthesize zinc oxide (ZnO) nanoparticles using a polymer precursor method, offering precise control over particle size in the nanometer scale. Zinc oxide nanoparticles are of significant interest due to their wideranging applications in various fields such as solar cells, gas sensors, photocatalysts, and nanomedicines. The synthesized nanoparticles were thoroughly characterized using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Fourier Transform Infrared spectroscopy (FTIR). The distinct hexagonal form detected in the XRD pattern, featuring characteristic reflection planes at angles of 31.72° (100), 34.39° (002), 36.23° (101), and 47.44° (102), signifies the synthesis of ZnO possessing a hexagonal wurtzite structure. The SEM and TEM images revealed uniformly spherical particles with an average size ranging from 35 to 40 nm. Such uniform morphology and size distribution are critical for ensuring consistent performance in applications such as gas sensing and catalysis. Additionally, the FTIR spectra indicated a reduction in impurities after the synthesis process, highlighting the effectiveness of the polymer precursor method in producing high-quality ZnO nanoparticles. Heating the ZnO precursor material at 400°C for 2 hours significantly reduces impurities, suggesting conversion to ZnO nanoparticles. [ABSTRACT FROM AUTHOR]

Hard X-ray microscopes with 20–30 nm spatial resolution ranges are an advanced tool for the inspection of materials at the nanoscale. However, the limited efficiency of the focusing optics, for example, a Fresnel zone plate (ZP) lens, can significantly reduce the power of a nanoprobe. Despite several reports on ZP lenses that focus hard X-rays with 20 nm resolution – mainly constructed by zone-doubling techniques – a systematic investigation into the limiting factors has not been reported. We report the structural effects on the focusing and imaging efficiency of 20–30 nm-resolution ZPs, employing a modified beam-propagation method. The zone width and the duty cycle (zone width/ring pitch) were optimized to achieve maximum efficiency, and a comparative analysis of the zone materials was conducted. The optimized zone structures were used in the fabrication of Pt-hydrogen silsesquioxane (HSQ) ZPs. The highest focusing efficiency of the Pt-HSQ-ZP with a resolution of 30 nm was 10% at 7 keV and >5% in the range 6–10 keV, whereas the highest efficiency of the Pt-HSQ-ZP with a resolution of 20 nm was realized at 7 keV with an efficiency of 7.6%. Optical characterization conducted at X-ray beamlines demonstrated significant enhancement of the focusing and imaging efficiency in a broader range of hard X-rays from 5 keV to 10 keV, demonstrating the potential application in hard X-ray focusing and imaging.

Large macroscopic assemblies formed by a surfactant, sodium dodecylsulfate (SDS), and glycerol, can be directed to assemble in a hierarchical manner by the addition of a strong hydrogen-bond donor/acceptor, such as urea. Self-assembly in complex media is important to a range of applications, for instance in biological media, which are multi-component, to industrial formulations, where additives are present for flavour, texture, and preservation. Here, the gelation and self-assembly of sodium dodecylsulfate (SDS) in glycerol is explored in the presence of an additive, urea. Urea was chosen due to its importance both fundamentally and industrially, but also because of its ability to form strong H-bonds and interact with both glycerol and SDS. To cover the variety of length scales present in the gel-like phase, a combination of optical microscopy and small-angle X-ray scattering techniques were used to probe the micro- to nanoscale. On the microscale, the formation of a spectacular spherulite phase, even at low urea contents - 0.1 wt%, upon cooling was observed, a stark difference to the microfibrillar phase observed in the absence of urea. Interestingly, the nanostructure of the two crystalline phases were similar and showed negligible differences. This suggests that urea is not involved in the SDS/glycerol microfibril formation but instead directs the assembly of spherulites by bundling the microfibrils. These ternary systems are also probed as a function of urea content, SDS concentration, and temperature. The observations in this work highlight the importance of small molecules in the self-assembly process, which is relevant both fundamentally but also industrially, where small molecules are often added to formulations. [ABSTRACT FROM AUTHOR]

Electrical triggering of a metal-insulator transition (MIT) often results in the formation of characteristic spatial patterns such as a metallic filament percolating through an insulating matrix or an insulating barrier splitting a conducting matrix. When MIT triggering is driven by electrothermal effects, the temperature of the filament or barrier can be substantially higher than the rest of the material. Using X-ray microdiffraction and dark-field X-ray microscopy, we show that electrothermal MIT triggering leads to the development of an inhomogeneous strain profile across the switching device, even when the material does not undergo a pronounced, discontinuous structural transition coinciding with the MIT. Diffraction measurements further reveal evidence of unique features associated with MIT triggering including lattice distortions, tilting, and twinning, which indicate structural nonuniformity of both low-and high-resistance regions inside the switching device. Such lattice deformations do not occur under equilibrium, zero-voltage conditions, highlighting the qualitative difference between states achieved through increasing temperature and applying voltage in nonlinear electrothermal materials. Electrically induced strain, lattice distortions, and twinning could have important contributions in the MIT triggering process and drive the material into nonequilibrium states, providing an unconventional pathway to explore the phase space in strongly correlated electronic systems. [ABSTRACT FROM AUTHOR]

Correlative methods to characterize single entities by electrochemistry and microscopy/spectroscopy are increasingly needed to elucidate structure‐function relationships of nanomaterials. However, the technical constraints often differ depending on the characterization techniques to be applied in combination. One of the cornerstones of correlative single‐entity electrochemistry (SEE) is the substrate, which needs to achieve a high conductivity, low roughness, and electrochemical inertness. This work shows that graphitized sputtered carbon thin films constitute excellent electrodes for SEE while enabling characterization with scanning probe, optical, electron, and X‐ray microscopies. Three different correlative SEE experiments using nanoparticles, nanocubes, and 2D Ti3C2Tx MXene materials are reported to illustrate the potential of using carbon thin film substrates for SEE characterization. The advantages and unique capabilities of SEE correlative strategies are further demonstrated by showing that electrochemically oxidized Ti3C2Tx MXene display changes in chemical bonding and electrolyte ion distribution. [ABSTRACT FROM AUTHOR]

The influence of annealing at a temperature of 980°C on the microstructure, phase composition, and microhardness of the additively manufactured TiNi-based material has been investigated. TiNi billets were produced using dual-wire electron beam additive manufacturing by simultaneous deposition of titanium and nickel wires. The typical morphology of dendritic microstructure changes from the bottom to the top of the asbuilt billet and is characterized by large dendritic blocks in the bottom part and thin dendrites in the central and upper parts. According to the data of scanning electron microscopy energy-dispersive X-ray (SEM EDS) analysis and the phase diagrams, dendrites and interdendritic regions consist of a mixture of TiNi + TiNi3 and TiNi + Ti2Ni phases, respectively, but the data of X-ray analysis confirm the presence of the Ti3Ni4 phase as well. Annealing contributes to the partial dissolution of large dendrites in the bottom part of the billet, increase of the thin dendrite sizes, and smoothing of their forms. The data of SEM EDS analysis and XRD both testify that the multiphase mixture of different phases tends to transform into a single-phase TiNi structure during annealing, but this transformation is incomplete. All these factors lead to the increase of microhardness of the annealed samples from ≈5 GPa for the as-built specimen to ≈7 GPa for the 8-h annealed specimen. [ABSTRACT FROM AUTHOR]

The root cause failure investigation for a ruptured secondary superheater (SSH) tube in a heavy oil-fired boiler was undertaken. The technical investigation disclosed severe microstructural degradation in terms of intermetallic phase precipitation, creep cavities and carburization of tube's external surface. The dimensional survey revealed significant thickness reduction along periphery of fractured surface. A semi-quantitative analysis of surface deposits was performed by scanning electron microscopy and x-ray diffraction to characterize and identify the sources of corrosive deposits. The detection of low melting eutectic vandates in external deposits induced the possibility of fireside corrosion. A comparative analysis was drawn between competing mechanisms of fireside corrosion and long-term overheating to reckon the root cause of the failure. Furthermore, a microstructural evolution model for fine-grained austenitic stainless steel (SA-213 TP347 HFG) suffering simultaneously from fireside corrosion and long-term overheating was developed. The investigation was concluded with notable recommendations and protective measures against fireside corrosion for superheater tubes for boiler life extension and maintaining overall equipment reliability. [ABSTRACT FROM AUTHOR]

The three-dimensional (3D) morphology, anatomy, and in-situ chemical composition analysis of fossils are crucial for systematic paleontology and determining their phylogenetic positions. Scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS), offers valuable structural and chemical information for the analysis of fossils. However, its primary limitation is the restriction to two-dimensional surface data, which limits the exploration of fossils' 3D complexities. Conversely, 3D X-ray microscopy (3D-XRM), also known as a novel form of micro-computed tomography (micro-CT) facilitates the non-destructive 3D reconstruction of fossil specimens. Nevertheless, it lacks the capability to provide in-situ compositional data. Acknowledging the constraints inherent in these individual techniques, and in response to the evolving requirements of paleontological research, this study introduces an integrated approach that combines 3D-XRM with EDS-coupled focused ion beam scanning electron microscopy (FIB-SEM). This innovative strategy is designed to synergize the advantages of both techniques, thereby addressing challenges that conventional methods cannot. It enables the rapid identification of regions of interest (ROI) within fossil specimens at micrometer resolution. Subsequently, this method collects detailed data on both 3D structures and chemical compositions at the nanometer scale for the identified ROI. This integrated approach represents a significant advancement in paleontological and geological research methodologies, promising to meet the increasing demands of these fields. [ABSTRACT FROM AUTHOR]

Isoprothiolane is a common pesticide used to manage a variety of crop diseases. It has also been linked to carcinogenic consequences in people when exposed to certain quantities for longer spans of time. As a result, the establishment of extremely sensitive and selective method to detect isoprothiolane is crucial for ecosystem protection and food safety. Recently, perovskite quantum dots (PQDs) have received rising interest as a result of their inherent fluorescence properties and applications in variety of domains. In the current study, we successfully synthesized cesium lead bromide (CsPbBr3) PQDs by using modified ligand-assisted re-precipitation method via tip sonication treatment. A strong green fluorescence of CsPbBr3 PQDs is effectively quenched after forming complex with isoprothiolane through a static quenching effect. The optical properties, morphology, chemical compositions, and diffraction patterns of CsPbBr3 PQDs were distinguished by using fluorescence, absorption, X-ray diffraction pattern, X-ray photoelectron microscopy, and high-resolution transmission electron microscopy techniques. Under the optimal reaction conditions, CsPbBr3 PQDs exhibit wide detection range (0.025-25 μM) and low detection limit (10.12 nM) for isoprothiolane detection. Furthermore, the nanoprobe has excellent selectivity for isoprothiolane, and it can be successfully applied to detect isoprothiolane in real samples. [ABSTRACT FROM AUTHOR]

Single-crystalline layered oxide materials for lithium-ion batteries are featured by their excellent capacity retention over their polycrystalline counterparts, making them sought-after cathode candidates. Their capacity degradation, however, becomes more severe under high-voltage cycling, hindering many high-energy applications. It has long been speculated that the interplay among composition heterogeneity, lattice deformation, and redox stratification could be a driving force for the performance decay. The underlying mechanism, however, is not well-understood. In this study, we use X-ray microscopy to systematically examine single-crystalline NMC particles at the mesoscale. This technique allows us to capture detailed signals of diffraction, spectroscopy, and fluorescence, offering spatially resolved multimodal insights. Focusing on early high-voltage charging cycles, we uncover heterogeneities in valence states and lattice structures that are inherent rather than caused by electrochemical abuse. These heterogeneities are closely associated with compositional variations within individual particles. Our findings provide useful insights for refining material synthesis and processing for enhanced battery longevity and efficiency. [ABSTRACT FROM AUTHOR]

Despite the major influence of soils on climate change, carbon sequestration, pollution remediation, and food security, soil remains a largely unexplored media with an extreme complexity of microbes, minerals, and dead organic matter, most of them being actually poorly known. In particular, soil biofilms have recently attracted attention because they strongly influence biogeochemical reactions and processes. Here we review biofilms with focus on their behavior, proliferation, distribution, characterization methods, and applications. Characterization methods include optical, electron, scanning probe, and X-ray microscopy; metagenomics, metatranscriptomics, metaproteomics, metabolomics; and tracking approaches. Applications comprise pollution remediation by metal immobilization or organics degradation; and methane oxidation, carbon dioxide reduction, and carbon sequestration. Advanced methods such as DNA-stable isotope probing and meta-omics have uncovered the multiple functions of soil biofilms and their underlying molecular mechanisms. Investigations have improved our understanding of inter- and intra-kingdom interactions, and of gene transfer. Extracellular materials such as polysaccharides enhance the transport of substances and electrons flow among microorganisms. [ABSTRACT FROM AUTHOR]

The Mazarrón 2 shipwreck was found in 1994 on the beach of Playa de la Isla (Mazarrón, Murcia, Spain). This finding is extremely important because the boat and its lead cargo were still in a reasonable conservation state and, therefore, provided new data on naval construction, commercial goods, navigation routes, and the relationships between the Phoenicians and the local population in the 7th–6th century BC. Currently, the shipwreck remains underwater, protected by a metallic coffer. In the last 2 years, a Preliminary Studies Project has been carried out, supported by national and regional public institutions. This research aims to know the shipwreck's conservation state and to determine the extraction and conservation methods at the Museo Nacional de Arqueología Subacuática ARQVA (Cartagena, Spain), where the conservation and restoration treatment will be conducted. The sampling strategy and analytical study included not only wood and other materials from the shipwreck and its cargo but also the seawater and the seabed materials in the vicinity of the shipwreck. This paper presents the results of the geochemical study of the archeological site. The applied methodology included physico-chemical tests, X-ray diffraction, optical microscopy, FTIR spectroscopy, field-emission scanning electron microscopy coupled with X-ray microanalysis, and X-ray microscopy. The results indicated that, despite the wreck being buried at a shallow depth (less than 50 cm) in a marine environment with a water column of 2–2.5 m, influenced by complex coastal dynamics that favor an oxic environment, early diagenetic processes like the formation of pyrite framboids are particularly intense in the pores and internal channels of the wreck's wood, where a different dysoxic–anoxic environment prevails. These processes have been the main mechanisms to have affected the wreck and are related to the biogeochemistry of sediments. The sediments have been confirmed to be closely related to the geological context of the Mazarrón region. The conducted study found no significant evidence of pollution due to the lead cargo. [ABSTRACT FROM AUTHOR]

The article focuses on the critical role of soldering in microelectronics assembly and the impact of voids within solder balls on device performance. Topics include the challenges posed by voids, which can affect electrical resistance and mechanical stability, the importance of accurate void detection, and the various methods, including traditional and machine learning-based approaches, used for void detection in 2D x-ray images of ball grid array packages.

Ti600/TC18 dissimilar titanium alloy joints were prepared by inertia friction welding and then underwent stress-relief annealing and three-stage annealing. The microstructure and corrosion resistance of the joints were characterized through scanning electron microscopy and X-ray diffractometry, and were tested by electrochemical measurements and static immersion corrosion experiments in HCl solution with different concentrations. The results show that the microstructure becomes more refined with more grain boundaries after stress-relief annealing, while the secondary α phase is coarsened and the α phase in the grain boundaries is formed on the microstructure after three-stage annealing with fewer grain boundaries. The specimen treated by stress-relief annealing has excellent corrosion resistance due to the denser and stabler passivation film formed on the grain boundaries. When the stress-relief annealing process is defined as 650°C, 3 h, and air cooling, more grain boundaries appeared on the joint, and, as a result, it provides more nucleation sites for the formation of the passivation film, so it is endowed with a good ability to resistant corrosion. [ABSTRACT FROM AUTHOR]

The semiconductor industry is continuing the scaling down of both device and on-chip interconnect features, for performance and economic reasons. This trend has implications for the design of guard ring structures, i.e. metallic non-functional structures in the back-end-of-line (BEoL) stack designed to be efficient to stop microcracks. In this work, we present a sample design for an in situ experiment to study mechanical degradation and failure mechanisms of crack stop structures in the BEoL stack, to ensure the mechanical robustness of microchips for future technology nodes. Additional finite element method (FEM) simulations provide supplementary understanding of the crack kinetics. To examine the effects of mechanical loading on crack stop elements of the BEoL stack, a novel sample geometry for an in situ fatigue experiment using x-ray microscopy was developed. The x-ray microscope (ZEISS Xradia 800 Ultra) enables high-resolution imaging of the 3D-patterned sample structures and defects such as microcracks. The tailored sample geometry allows the application of a tensile load to a BEoL specimen by a lever mechanism. The feasibility of the sample design is shown by mode-I loading of a pure interconnect sample. Post-mortem analysis by scanning electron microscopy (SEM), confirming planar microcrack propagation from the notch through the dielectric layer with small deflections of the crack path near cone shaped copper vias. FEM simulations focusing on the stress-strain fields around a crack tip indicate the beginning of copper plasticity as major mechanism starting the redirection of cracks due to resulting material compression in front of the obstacle. [ABSTRACT FROM AUTHOR]

Background Copper oxide (Cu2O) nanoparticles (CO NPs) are in extensive use during our everyday life as antimicrobial agent, lubricant, in manufacturing electrodes of lithium ion batteries as well as for photo catalytic degradation of organic pollutants. Due to extensive and diverse use Cu2O NPs, they are likely to accumulate in the environment and to affect the live forms. Present investigation was aimed to report the biocompatibility of CO NPs in Wistar rats in sex specific manner. CO NPs, having average diameter of 14.06 nm, were synthesized by co-precipitation method and scanning electron microscopy and X ray diffraction were used for their characterization. Methods For 14 consecutive days, Wistar rats (6 weeks old) of both sexes were intraperitoneally injected with 10 mg/mL saline/Kg body weight of CO NPs, while the control groups intraperitoneally received saline solution for same duration. Behavioral tests (open field and novel object recognition), complete blood count, selected biomarkers of oxidative stress and Copper concentration in brain and liver were determined in all subjects. Results High mortality rates [male 40% and female 60%] were observed in rats exposed to CO NPs. A sever decrease in body weight was also observed in both male and female rats exposed to CO NPs. Female rats treated with CO NPs spent significantly more time with novel object as compared to control [ P  = 0.05] during second trial of novel object test. CO NPs treated female rats had higher mean corpuscular hemoglobin [ P  < 0.001] levels and Copper concentration in liver [ P  = 0.04] than control. Male rats exposed to CO NPs had significantly higher mean corpuscular volume [ P  = 0.02] and superoxide dismutase [SOD] [ P  = 0.04] in lungs than their control group. All other studied parameters non significantly varied upon comparison between CO NPs treated and untreated rats of both sex. Conclusion In conclusion, we are reporting that intraperitoneal injections of CO NPs for 14 days can disturb complete blood count and biomarkers of oxidative stress in lungs of Wistar rats. [ABSTRACT FROM AUTHOR]

Tuberculosis (TB) causes major public health problems worldwide. Fighting TB requires sustained efforts in health prevention, diagnosis and treatment. Previous literature has shown that conventional diagnostic methods like X-ray and sputum microscopy often miss early or extrapulmonary TB due to their limited sensitivity. Blood tests, while useful, lack the anatomical detail needed for precise localization of TB lesions. A possible step forward in the fight against TB could be the use of Fluorodeoxyglucose Positron Emission Tomography (FDG-PET) and Computed Tomography (CT). This meta-analysis discusses the current literature, including the methods, results and implications of using FDG-PET-CT in the early diagnosis of TB. Analysis of the studies showed that the sensitivity of FDG-PET-CT as a potential method for early detection of TB was 82.6%. [ABSTRACT FROM AUTHOR]

Al–Zn–Mg–Si alloy coatings have been developed to inhibit the corrosion of cold-rolled steel sheets by offering galvanic and barrier protection to the substrate steel. It is known that Fe deposited from the steel strip modifies the microstructure of the alloy. We cast samples of Al–Zn–Mg–Si coating alloys containing 0.4 wt% Fe and directionally solidified them using a Bridgman furnace to quantify the effect of this Fe addition between 600   ° C and 240   ° C . By applying a temperature gradient, growth is encouraged, and by then quenching the sample in coolant, the microstructure may be frozen. These samples were analysed using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) to determine the morphological effects of the Fe distribution across the experimental temperature range. However, due to the sub 1 wt% concentration of Fe, synchrotron X-ray fluorescence microscopy (XFM) was applied to quantitatively confirm the Fe distribution. Directionally solidified samples were scanned at 7.05 keV and 18.5 keV using X-ray fluorescence at the Australian Synchrotron using the Maia array detector. It was found that a mass nucleation event of the Fe-based τ6 phase occurred at 495   ° C following the nucleation of the primary α-Al phase as a result of a peritectic reaction with remaining liquid. [ABSTRACT FROM AUTHOR]

Elektrocateres rappsilberi gen. et sp. nov. is described from Bitterfeld or Saxonian amber. It is the first representative of the superfamily Cleroidea (Coleoptera) recorded in this amber, from which only 10 families of beetles were known until now. The new genus and species was studied using classical stereomicroscopy, as well as digital microscopy and synchrotron-radiation-based micro-computed tomography. The fossil is related to the rare extant monotypic genera Trichocateres Kolibáč, 2010 and Carinicateres Kolibáč, 2021 from tropical forests of Southeastern Asia. It is assumed that Elektrocateres rappsilberi gen. et sp. nov. would be predatory, hunting other arthropods on tree branches and trunks; however, its mouthparts are probably still on halfway between herbivory or fungivory and predatory. [ABSTRACT FROM AUTHOR]

Plastic foams, near-ubiquitous in everyday life and industry, show properties that depend primarily on density. Density measurement, although straightforward in principle, is not always easy. As such, while several methods are available, plastic foam industry is not yet supported with a standard technique that effectively enables to control density maps. To overcome this issue, this paper proposes Terahertz (THz) time-of-flight imaging using normal reflection measurements as a fast, relatively cheap, contactless, non-destructive and non-dangerous way to map plastic foam density, based on the expected relationship between density and refractive index. The approach is demonstrated in the case of polypropylene foams. First, the relationship between the estimated effective refractive index and the polypropylene foam density is derived by characterizing a set of carefully crafted samples having uniform density in the range 70–900 kg/m3. The obtained calibration curve subtends a linear relationship between the density and the refractive index in the range of interest. This relationship is validated against a set of test samples, whose estimated average densities are consistent with the nominal ones, with an absolute error lower than 10 kg/m3 and a percentage error on the estimate of 5%. Exploiting the calibration curve, it is possible to build quantitative images depicting the spatial distribution of the sample density. THz images are able to reveal the non-uniform density distribution of some samples, which cannot be appreciated from visual inspection. Finally, the complex spatial density pattern of a graded foam sample is characterized and quantitatively compared with the density map obtained via X-ray microscopy. The comparison confirms that the proposed THz approach successfully determines the density pattern with an accuracy and a spatial scale variability compliant with those commonly required for plastic foam density estimate. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Silicon nitride membranes were experimentally obtained as substrates for biological samples, which are examined using a microscope with an operating wavelength of 13.8 nm. The free-hanging films obtained have a size of up to 1.5 × 1.5 mm2, which makes it possible to select an area of interest for investigation on the sample on the order of tens to hundreds of microns. The mechanical strength of the membranes satisfies that the samples do not tear the membranes and withstand transportation. The results obtained are an import-substituting technology for the manufacture of Si3N4 membranes. The resulting membranes have a transparency of more than 40% in the range of the "water transparency window" (2.3–4.4 nm) and EUV (13–15 nm). The developed technology will become the basis for creating cuvettes for living biological samples for soft X-ray microscopy studies. [ABSTRACT FROM AUTHOR]

Here, we studied several Pachyrukhinae (Mammalia: Notoungulata: Typotheria: Hegetotheriidae) fossils recovered from the late Early Miocene (Santacrucian SALMA) beds of the Cura-Mallín Formation at the Laguna del Laja (Biobío Region, Chile). The specimens are referred to a new species of the genus Pachyrukhos Ameghino, 1885, P. ngenwinkul sp. nov. The holotype of this taxon is a relatively well-preserved articulated skull and mandibles, which was investigated using 3D X-ray Microscopy. The new taxon is distinguished from other Pachyrukhos species by having a p2 smaller than p3, M3 mesiodistally shorter (around 30%) than M1, and upper premolars of a rather subtriangular contour. Pachyrukhos ngenwinkul is the most common mammal and the smallest-sized (with ~2 kg of body mass) notoungulate found in the Santacrucian assemblage at the Laguna del Laja. The discovery of this new taxon improves our understanding of the Neogene pachyrukhine diversity in southern South America and highlights the potential of the Chilean Andean Cenozoic deposits in revealing a hidden diversity of extinct continental mammals. [ABSTRACT FROM AUTHOR]

The plating of lithium metal on the graphite electrode is a major degradation mechanism in lithium‐ion batteries (LIBs). It brings a significant risk of internal shortcircuit by penetration of dendritic lithium through the separator, leading to short cycle life and safety issues. Understanding how and when plating occurs is crucial for the development of mitigation strategies, e. g. tuning the electrolyte composition. Here we present an operando X‐ray tomographic microscopy (XTM) study to directly monitor the plating of lithium metal in a lithium/graphite cell. XTM enables a non‐destructive and quantitative characterization at operando conditions of lithium deposition on a graphite electrode at relevant conditions. In this work it allows us to probe the role of the electrolyte additives vinylene carbonate (VC) and lithium bis(fluorosulfonyl)imide (LiFSI) in the standard LIB electrolyte LP57 (base electrolyte without additives). The additives show overall better performances in terms of delayed onset of lithium plating which is important for the utilisation of the full capacity of graphite intercallaiton. We show that there is a transition during lithiation of the dominating mechanism, once lithium plating is initiated this rapidly becomes dominating and hinders further intercalation. For the base electrolyte a homogeneous and dense morphology of plated lithium is found, whereas a more dendritic morphology is observed in the presence of additives. During delithiation, there is a rapid stripping of some of the plated lithium followed by deintercalation. In addition, our work provides a general methodology to track the morphology of plated lithium, which is crucial for fundamental research about battery safety. [ABSTRACT FROM AUTHOR]

The aim of this study is to evaluate the effect of various disinfection protocols on the cutting efficiency and chemical composition of ProTaper, Twisted File, Twisted File Adaptive, and Hedström files. Four experimental groups (n = 10) were presoaked in either enzymatic solution or 1% sodium hypochlorite for 30 min, followed by either 5 or 15 min of ultrasonic cleaning and then autoclaved. Resin-simulated canals with a single curvature of 38–40° were prepared by each instrument system. Cutting efficiency of each instrument was analyzed by subtracting the final weight from the initial weight of the resin blocks. Chemical compositions were studied by field emission scanning electron microscopy and X-ray energy-dispersive spectrometry. The cutting efficiency of Hedström, ProTaper, and Twisted File instruments decreased compared to their control groups (p < 0.05) whereas it did not change for Twisted File Adaptive. More corrosion was detected with longer ultrasonication time. No difference was observed regarding the pre-soaking media. Disinfection protocols exerted a significant overall effect on the performance of Hedström, ProTaper, and Twisted File instruments. Corrosion, microcracks, and crevices were evident on all tested instruments after disinfection protocols applied. All disinfection protocols, regardless of the pre-soaking media used or the ultrasonic cleaning time applied, have some effect on the cutting efficiency and the surface characteristics of the files. [ABSTRACT FROM AUTHOR]

Reptilian (non‐avian) eggshell biomineralization is markedly different from avian eggshells. Despite discontinuous/variable mineralization, the reptilian eggshell (like in birds) is responsible for protective and developmental functions of the egg as part of a highly successful reproduction strategy. Using multiscale imaging and characterization methods including X‐ray and electron microscopy/tomography, a 3D overview of eggshell ultrastructure in the gekkotan Eublepharis macularius – the common leopard gecko is provided. Eggshell mineral is shown to be sensitive to aqueous preparations, where cryogenic methods are essential for accurate mineral and organic preservation. Interwoven with the mineral are underlying organic fibers involved in the formation of complex hierarchical order in the eggshell, including nucleation and growth of mineral. The calcitic mineral phase of the eggshell takes on three microstructural motifs at the shell surface: nodular scutes (≈40 µm), intermittent blunt or star‐shaped mineral rosettes (≈1 mm), and smaller mineral corollas (≈10 µm). Individual scutes have two hierarchical mineral structures – mineral nanospheres (≈500 nm) and mineral nanodomains (≈40 nm). Diverse and variable biomineralization features of reptilian eggshells likely reflect the importance of differences in ecology and physiology on egg formation, survival, and eggshell mechanics, and are likely related to hydration sensitivity, structural organic‐inorganic interactions, and mineral polymorphism. [ABSTRACT FROM AUTHOR]

2D layered materials, such as transition metal carbides or nitrides, known as MXenes, offer an ideal platform to investigate charge transfer processes in confined environment, relevant for energy conversion and storage applications. Their rich surface chemistry plays an essential role in the pseudocapacitive behavior of MXenes. However, the local distribution of surface functional groups over single flakes and within few‐ or multilayered flakes remains unclear. In this work, scanning X‐ray microscopy (SXM) is introduced with simultaneous transmission and electron yield detection, enabling multimodal nanoscale chemical imaging with bulk and surface sensitivity, respectively, of individual MXene flakes. The Ti chemical bonding environment is found to significantly vary between few‐layered hydrofluoric acid‐etched Ti3C2Tx MXenes and multilayered molten salt (MS)‐etched Ti3C2Tx MXenes. Postmortem analysis of MS‐etched Ti3C2Tx electrodes cycled in a Li‐ion battery further illustrates that simultaneous bulk and surface chemical imaging using SXM offers a method well adapted to the characterization of the electrode‐electrolyte interactions at the nanoscale. [ABSTRACT FROM AUTHOR]

Microscopy, electrochemical techniques and mechanical testing are used to investigate the effect of varying antimony additions (0.45–1.8 wt%) on the microstructure and corrosion properties of zinc-magnesium-aluminium coating alloys. Samples were produced by splat casting to produce high cooling rates similar to those seen in a continuous galvanising line. X-Ray Microscopy reveals that the Sb additions produce disk-shaped Mg3Sb2 intermetallics, subsequently reducing or eliminating the MgZn2 eutectic. Electrochemical testing in 1 wt% NaCl shows that the Mg3Sb2 phase is cathodic with respect to the bulk alloy with slower oxygen reduction kinetics. The decrease in eutectic content leads to less intense anodic activity. The combined effect is anodic and cathodic deactivation, which leads to a 43% reduction in corrosion rate as measured through LPR compared to the base alloy. This work shows that quaternary additions to ZMA coating alloys can be a potential route to improved corrosion resistance for galvanic protection. [ABSTRACT FROM AUTHOR]