Advanced Electron Microscopy Techniques Research Articles

Advanced Electron Microscopy Characterisation of Aluminium-Oxygen Coordination in Catalyst Supports

Performance of alumina-supported catalyst systems are significantly affected by how the tetrahedral (Al-O4) and octahedral (Al-O6) coordination are mixed and blended with each other. Characterisation of aluminium-oxygen coordination is thus important to understand how catalysts interact with alumina at the microscopic level. Here we report the application of two advanced electron microscopy techniques on aluminium-oxygen coordination. The first technique is electron energy loss spectroscopy (EELS) that can reveal detailed electronic structure profile of aluminium valence band to analyse how aluminium is coordinated by oxygen. The second technique is pair distribution function (PDF) based on electron diffraction (ED), employed to measure aluminium-oxygen bond lengths associated with the coordination geometry.

Pentatwinned AuAg Nanorattles with Tailored Plasmonic Properties for Near-Infrared Applications.

Noble metal nanoparticles, particularly gold and silver nanoparticles, have garnered significant attention due to their ability to manipulate light at the nanoscale through their localized surface plasmon resonance (LSPR). While their LSPRs below 1100 nm were extensively exploited in a wide range of applications, their potential in the near-infrared (NIR) region, crucial for optical communication and sensing, remains relatively underexplored. One primary reason is likely the limited strategies available to obtain highly stable plasmonic nanoparticles with tailored optical properties in the NIR region. Herein, we synthesized AuAg nanorattles (NRTs) with tailored and narrow plasmonic responses ranging from 1000 to 3000 nm. Additionally, we performed comprehensive characterization, employing advanced electron microscopy and various spectroscopic techniques, coupled with finite difference time domain (FDTD) simulations, to elucidate their optical properties. Notably, we unveiled the main external and internal LSPR modes by combining electron energy-loss spectroscopy (EELS) with surface-enhanced Raman scattering (SERS). Furthermore, we demonstrated through surface-enhanced infrared absorption spectroscopy (SEIRA) that the NRTs can significantly enhance the infrared signals of a model molecule. This study not only reports the synthesis of plasmonic NRTs with tunable LSPRs over the entire NIR range but also demonstrates their potential for NIR sensing and optical communication.

Investigation of AlGaN UV emitting tunnel junction LED devices by off-axis electron holography

Here we use off-axis electron holography combined with advanced transmission electron microscopy techniques to understand the opto-electronic properties of AlGaN tunnel junction (TJ)-light-emitting diode (LED) devices for ultraviolet emission. Four identical AlGaN LED devices emitting at 290 nm have been grown by metal–organic chemical vapour deposition. Then Ge doped n-type regions with and without InGaN or GaN interlayers (IL) have been grown by molecular beam epitaxy onto the top Mg doped p-type layer to form a TJ and hence a high quality ohmic metal contact. Off-axis electron holography has then been used to demonstrate a reduction in the width of the TJ from 9.5 to 4.1 nm when an InGaN IL is used. As such we demonstrate that off-axis electron holography can be used to reproducibly measure nm-scale changes in electrostatic potential in highly defected and challenging materials such as AlGaN and that systematic studies of devices can be performed. The LED devices are then characterized using standard opto-electric techniques and the improvements in the performance of the LEDs are correlated with the electron holography results.

A HRTEM-EDS-SAED Study of Precipitates in Mg-Zn-Zr Alloy

In this study, aging heat treatment was performed on extruded Mg-Zn-Zr alloy. Aging was performed on as-extruded samples at 180°C for 1-2-4-8 and 24 hours. Microhardness tests were made to obtain the aging curve. Detailed transmission electron microscopy (TEM) examinations such as selected area electron diffraction (SAED), energy dispersive spectrometry (EDS), and high resolution transmission electron microscopy (HRTEM) were used to investigate the microstructure, second phases, and precipitates. Size, type, and morphologies of second phases and precipitates were studied aided by advanced transmission electron microscopy techniques. With the help of hardness test results peak aged condition was found to be 8 hour aging. TEM examinations were detailed for the 8-hour aged sample. It was observed that the precipitates responsible for age hardening were MgZn2. Moreover, the majority of these precipitates were β’1 phase.

Investigation of macro-micro mechanical behaviors and failure mechanisms in cemented tailings backfill with varying proportions of fine

This study investigates the impact of tailings characteristics, particularly fine tailings, on the efficiency and effectiveness of mining engineering backfill operations. Contrary to the common underestimation, fine tailings significantly affect the mechanical properties and failure mechanisms of Cemented Tailings Backfill (CTB). Through a series of experiments examining various particle size distributions and employing advanced Scanning Electron Microscopy (SEM) and Mercury Intrusion Porosimetry (MIP) techniques, this research clarifies the role of fine tailings in modifying the mechanical strength and failure patterns of CTB. Adding 20 % fine tailings optimally enhances both the early and long-term strength of backfill materials. With aging, adding 30 % fine tailings shows a rapid strength increase from 7d to 28d, with the 28d strength slightly lower than that of specimens with 20 % addition, but the specimens demonstrate better ductility after reaching peak strength. As the content of fine tailings increases, crack propagation in the specimens shifts from radial to axial, simplifying the fracture mode from complex to singular. Consequently, the fracture mechanism changes from ductile to brittle, and then reverts to ductile. Moreover, using particle flow simulation and moment tensor analysis to study the failure processes indicates that while increased fine particle content boosts the material's initial strength, it ultimately leads to a simpler crack network and volumetric expansion as the primary failure mode. In terms of energy conversion mechanisms, as the content of fine particles increases, the energy first increases and then decreases. During the elastic stage and the early stage of the plastic stage, the energy is mainly converted into strain energy and PB bonding energy, which affects the elasticity of the sample. In the later stage of the plastic phase, the energy is mainly converted into dissipated energy, leading to the failure of the sample.

A new bi-directional surface modification cathode based on conventional cathode La0.6Sr0.4Co0.2Fe0.8O3-δ

The commercialization of proton solid oxide fuel cells (H-SOFCs) is hindered by the lack of high active and durable cathode materials exposed to evil operation conditions. Here, this groundbreaking study addresses two critical challenges impeding the practicality of La0.6Sr0·4Co0·2Fe0·8O3-δ (LSCF), one of the most popular proton-conducting cathode materials contemporarily: inadequate temperature activity and durability issues stemming from surface Sr segregation. The research introduces a transformative solution through the creation of a novel nanofiber cathode, denoted as PrBaCo1.4Fe0·6O6-δ@LSCF, comprising a nanoscale LSCF FP host and PBCF NP guest. Advanced electron microscopy and scanning electron microscopy techniques confirm the seamless integration of the two phases, highlighting a distinctive fiber structure adorned with impregnated nanoparticles. Meanwhile, efficiently reducing oxygen vacancies within the LSCF bulk phase significantly suppresses Sr segregation. Systematic simulations based on density functional theory reveal that the incorporation of PSCF reduces the polarization energy barrier. In practical terms, electrochemical testing of a single cell supported by PBCF@LSCF shows a polarization resistance of only 0.053 Ω cm2 at 700 °C, translating to a remarkable fifty percent reduction. Furthermore, a sustained 100-h test reveals no notable decline in performance. Consequently, a novel dual modification approach is proposed for crafting cathodes tailored for SOFCs.

A morphological analysis of calcium hydroxylapatite and poly-l-lactic acid biostimulator particles.

Injectable fillers, pivotal in aesthetic medicine, have evolved significantly with recent trends favoring biostimulators like calcium hydroxylapatite (CaHA-CMC; Radiesse, Merz Aesthetics, Raleigh, NC) and poly-l-lactic acid (PLLA; Sculptra Aesthetics, Galderma, Dallas, TX). This study aims to compare the particle morphology of these two injectables and examine its potential clinical implications. Utilizing advanced light and scanning electron microscopy techniques, the physical characteristics of CaHA-CMC and PLLA particles were analyzed, including shape, size, circularity, roundness, aspect ratio, and quantity of phagocytosable particles. The findings reveal several morphological contrasts: CaHA-CMC particles exhibited a smooth, homogenous, spherical morphology with diameters predominantly ranging between 20 and 45µm, while PLLA particles varied considerably in shape and size, appearing as micro flakes ranging from 2 to 150µm in major axis length. The circularity and roundness of CaHA-CMC particles were significantly higher compared to PLLA, indicating a more uniform shape. Aspect ratio analysis further underscored these differences, with CaHA-CMC particles showing a closer resemblance to circles, unlike the more oblong PLLA particles. Quantification of the phagocytosable content of both injectables revealed a higher percentage of phagocytosable particles in PLLA. These morphological distinctions may influence the tissue response to each treatment. CaHA-CMC's uniform, spherical particles may result in reduced inflammatory cell recruitment, whereas PLLA's heterogeneous particle morphology may evoke a more pronounced inflammatory response.

Recent progresses in transmission electron microscopy studies of two-dimensional ferroelectrics

The rich potential of two-dimensional materials endows them with superior properties suitable for a wide range of applications, thereby attracting substantial interest across various fields. The ongoing trend towards device miniaturization aligns with the development of materials at progressively smaller scales, aiming to achieve higher integration density in electronics. In the realm of nano-scaling ferroelectric phenomena, numerous new two-dimensional ferroelectric materials have been predicted theoretically and subsequently validated through experimental confirmation. However, the capabilities of conventional tools, such as electrical measurements, are limited in providing a comprehensive investigation into the intrinsic origins of ferroelectricity and its interactions with structural factors. These factors include stacking, doping, functionalization, and defects. Consequently, the progress of potential applications, such as high-density memory devices, energy conversion systems, sensing technologies, catalysis, and more, is impeded. In this paper, we present a review of recent research that employs advanced transmission electron microscopy (TEM) techniques for the direct visualization and analysis of ferroelectric domains, domain walls, and other crucial features at the atomic level within two-dimensional materials. We discuss the essential interplay between structural characteristics and ferroelectric properties on the nanoscale, which facilitates understanding of the complex relationships governing their behavior. By doing so, we aim to pave the way for future innovative applications in this field.

Crystallization-driven tuneable lasing of perylene doped into the nematic liquid crystal

Versatile devices with tunable capabilities for controlling lasing wavelength and intensity are in high demand. Liquid crystals (LCs) exhibit immense potential for such applications, offering fine-tuning possibilities through external factors. On the other hand, laser technology is currently a research hotspot in optoelectronics, and also in practical applications. The recent market introduction of laser television marks a significant stride toward making such advanced technology accessible in every household. In synergy with laser pumping, the LCs unquestionably can be rediscovered. This study presents a comprehensive investigation into the crystallization phenomenon within a host-guest device, compact in size, free from moving parts, and integrating the liquid crystalline (LC) matrix doped with 3,4,9,10-tetra-(3-alcoxy-carbonyl)-perylene (THCP) dye. The focus lies in examining the influence of varying dye concentrations on multicolor fluorescence, lasing behavior, and device morphology. The systematic analysis of Random Lasing (RL) energy thresholds and the impact of DC voltage on light intensity modulation is demonstrated. Morphological changes were monitored in real-time using optical microscopy techniques, including crossed polarizer, and fluorescence imaging under 450 nm excitation. Utilizing advanced Transmission Electron Microscopy (TEM) techniques, we explore exceptional insights into our set of devices, providing novel information about the THCP crystallization process for the first time in the literature. To gain a comprehensive understanding of the crystal forming and molecular geometry we examined additionally the THCP dye, using X-ray diffraction and Raman spectroscopy. Furthermore, we showcase that varying the pumping energy enables multicolor tuning in the fabricated systems, presenting an attractive feature in the context of laser display technologies.

Visualizing Structure, Growth, and Dynamics of Li Dendrite in Batteries: From Atomic to Device Scales

AbstractThe growth of lithium (Li) dendrites, characterized by construction of internal Li substrate and surface solid electrolyte interphase (SEI), represents a significant hurdle for both liquid‐state and solid‐state Li batteries. To better understand the growth behaviors of these dendrites at atomic to device scale, advanced electron microscopy techniques have emerged as a valuable tool, providing high temporal and spatial resolutions for real‐time observations. In this review, the mechanistic aspects of growth of Li dendrites are delved first from both thermodynamic and kinetic perspectives. Then, a systematic overview of the state‐of‐the‐art in‐situ devices is provided that is developed for integration into electron microscopes, detailing the corresponding static and dynamic structures of Li dendrites. Additionally, the utilization of the non‐destructive cryogenic TEM technique is explored to classify and compare the local fine structure information of as‐formed Li deposits, which are influenced by various factors such as current density, temperature, electrolyte composition, solvents, and additives. Overall, this review article offers a comprehensive understanding of the physical origins associated with Li dendrites, spanning from atomic to device scales and encompassing both liquid and all‐solid‐state battery scenarios, then envisioning fundamental principles and strategies for optimizing batteries and overcoming the critical challenges posed by Li dendrites.

EXPLORING AMORPHOUS ALLOYS: ADVANCED ELECTRON MICROSCOPY AND CLUSTER ANALYSIS

In this study, we explored the atomic structure and orderliness of amorphous alloys through advanced electron microscopy and analytical techniques. Amorphous alloys, characterized by disordered atomic structures, exhibit promising applications in technology. The research addresses a crucial knowledge gap by investigating cluster distribution, particle arrangement, and orderliness within the amorphous matrix. High-resolution electron microscopy (HREM) images are analyzed using diverse algorithms and software tools. The study establishes a correlation between angles approaching 180 degrees and increased orderliness within clusters, highlighting the reliability of angle distribution analysis. Robust indicators, including Div (SP(B/V)) and Div (Mu(B/V)) metrics, assess and compare amorphous alloy samples. Kullback-Leibler (K-L) divergence indicates the significance of cluster ordering, validated by the S-K test. Radial Distribution Function (RDF) analysis uncovers local short-range order, deepening understanding despite limited orderliness discernment. These findings not only enhance our understanding of metallic glasses or amorphous alloys but also offer opportunities for tailored design and improved applications across various technological domains.

Recent progress about transmission electron microscopy characterizations on lithium-ion batteries

With the rapid development of portable electronics, new energy vehicles, and smart grids, ion batteries are becoming one of the most widely used energy storage devices, while the safety concern of ion batteries has always been an urgent problem to be solved. To develop a safety-guaranteed battery, the characterization of the internal structure is indispensable, where electron microscopy plays a crucial role. Based on this, this paper summarizes the application of transmission electron microscopy (TEM) in battery safety, further concludes and analyzes the aspects of dendrite growth and solid electrolyte interface (SEI) formation that affect the safety of ion batteries, and emphasizes the importance of electron microscopy in battery safety research and the potential of these techniques to promote the future development of this field. These advanced electron microscopy techniques and their prospects are also discussed.

Laser powder bed fusion of pure copper electrodes

This study explores the fabrication and characterization of a pure copper electrode for an EDM equipment using laser powder bed fusion (LPBF) and comparing its performance with an original cast sample. The microstructural, mechanical, electrical, thermal, and corrosion characteristics of the samples were analyzed. The microstructure of the additively manufactured (AM) sample exhibited superior mechanical properties, with an 18 % increase in ultimate tensile strength and more than two times greater elongation in comparison with those of the cast sample. Moreover, the electrical and thermal conductivity coefficients of the AM sample were found to be consistent with industry standards as 5.52 × 107 S/m and 361 W/mK, respectively. Additionally, the potentiodynamic polarization corrosion test results of the AM sample further exhibited superior corrosion resistance in terms of the corrosion potential particularly in a 3.5 % NaCl environment. Advanced electron microscopy techniques were used to investigate the differences in the properties of the AM and cast samples and further shed light on the superior properties of the LPBF counterpart. Despite challenges in manufacturing pure copper components through LPBF, this study demonstrates the feasibility of producing a functional part that competes effectively with cast counterparts and excels in certain aspects.

Deep convolutional neural networks to restore single-shot electron microscopy images

Advanced electron microscopy techniques, including scanning electron microscopes (SEM), scanning transmission electron microscopes (STEM), and transmission electron microscopes (TEM), have revolutionized imaging capabilities. However, achieving high-quality experimental images remains a challenge due to various distortions stemming from the instrumentation and external factors. These distortions, introduced at different stages of imaging, hinder the extraction of reliable quantitative insights. In this paper, we will discuss the main sources of distortion in TEM and S(T)EM images, develop models to describe them, and propose a method to correct these distortions using a convolutional neural network. We validate the effectiveness of our method on a range of simulated and experimental images, demonstrating its ability to significantly enhance the signal-to-noise ratio. This improvement leads to a more reliable extraction of quantitative structural information from the images. In summary, our findings offer a robust framework to enhance the quality of electron microscopy images, which in turn supports progress in structural analysis and quantification in materials science and biology.

Innovative Microfluidic chip for Raman spectroscopy and advanced electron microscopy techniques

Innovative Microfluidic chip for Raman spectroscopy and advanced electron microscopy techniques

Influence of drop on the ultrastructure lipid composition of liver hepatocytes of pregnant rats

The influence of a toxic agent on the structure of the liver is inevitable. Of interest are the effects of pesticides on intrauterine formation and their teratogenic and embryotoxic properties. The influence of teratogens may manifest itself at different levels of organization of a living organism, and some aspects of cell metabolism change. Using advanced electron microscopy techniques combined with modern knowledge of membranology and toxicology, we conducted a detailed study of morphological changes in the subcellular architecture of the liver after repeated dropplet exposure. Ultrastructural studies were carried out on pregnant rats and their embryos on the 3rd, 13th, 19th days of pregnancy and embryonic development. Poisoning of animals with the pesticide dropp causes clear degenerative processes in the cellular and subcellular structures of the liver.

Advanced Pore Structure Analysis of Silver Nanoparticles via Electron Microscopy: Implications for Functional Optimization

In this paper, quantitative analysis of the pore structure of AgNPs is presented by combined analysis of advanced electron microscopy techniques. The synchrotron-based analysis of silver nanoparticles with 18-30 nm in size confirmed detailed information about the internal structure of their porous nature of the nanoparticles and their surface characteristics. Although the pore volume of AgNPs changed from 28 nm³ to 40 nm³, pore size ranged between 3 nm to 10 nm. Specific pore volume values referring to AgNP mass were within 10–26 nm 2 /g depending on nanoparticle size. Furthermore, the surface area values varied between 25 m²/g and 50 m²/g evidencing the influence of nanoparticle size on internal as well as exterior surface area. Taken together, the findings suggest a direct dependency of size dependent nanoparticle on the pore structure and surface area of the support material: Diameter of AgNP has direct impact on porosity of the samples. These findings are useful for optimizing internal porosity and surface properties of AgNPs for particular uses such as catalysis, drug delivery, and sensing. This vast study provides a framework for synthesising AgNPs with any types of pore structures to improve nanotechnology applications through careful tailoring of materials.

Probing Oxidation-Driven Amorphized Surfaces in a Ta(110) Film for Superconducting Qubit.

Recent advances in superconducting qubit technology have led to significant progress in quantum computing, but the challenge of achieving a long coherence time remains. Despite the excellent lifetime performance that tantalum (Ta) based qubits have demonstrated to date, the majority of superconducting qubit systems, including Ta-based qubits, are generally believed to have uncontrolled surface oxidation as the primary source of the two-level system loss in two-dimensional transmon qubits. Therefore, atomic-scale insight into the surface oxidation process is needed to make progress toward a practical quantum processor. In this study, the surface oxidation mechanism of native Ta films and its potential impact on the lifetime of superconducting qubits were investigated using advanced scanning transmission electron microscopy (STEM) techniques combined with density functional theory calculations. The results suggest an atomistic model of the oxidized Ta(110) surface, showing that oxygen atoms tend to penetrate the Ta surface and accumulate between the two outermost Ta atomic planes; oxygen accumulation at the level exceeding a 1:1 O/Ta ratio drives disordering and, eventually, the formation of an amorphous Ta2O5 phase. In addition, we discuss how the formation of a noninsulating ordered TaO1-δ (δ < 0.1) suboxide layer could further contribute to the losses of superconducting qubits. Subsurface oxidation leads to charge redistribution and electric polarization, potentially causing quasiparticle loss and decreased current-carrying capacity, thus affecting superconducting qubit coherence. The findings enhance the comprehension of the realistic factors that might influence the performance of superconducting qubits, thus providing valuable guidance for the development of future quantum computing hardware.

Unlocking the key role of bentonite fungal isolates in tellurium and selenium bioremediation and biorecovery: Implications in the safety of radioactive waste disposal

Research on eco-friendly bioremediation strategies for mitigating the environmental impact of toxic metals has gained attention in the last years. Among all promising solutions, bentonite clays, to be used as artificial barriers to isolate radioactive wastes within the deep geological repository (DGR) concept, have emerged as effective reservoir of microorganisms with remarkable bioremediation potential. The present study aims to investigate the impact of bentonite fungi in the speciation and mobility of selenium (Se) and tellurium (Te), as natural analogues 79Se and 132Te present in radioactive waste, to screen for those strains with bioremediation potential within the context of DGR. For this purpose, a multidisciplinary approach combining microbiology, biochemistry, and microscopy was performed. Notably, Aspergillus sp. 3A demonstrated a high tolerance to Te(IV) and Se(IV), as evidenced by minimal inhibitory concentrations of >16 and >32 mM, respectively, along with high tolerance indexes. The high metalloid tolerance of Aspergillus sp. 3A is mediated by its capability to reduce these mobile and toxic elements to their elemental less soluble forms [Te(0) and Se(0)], forming nanostructures of various morphologies. Advanced electron microscopy techniques revealed intracellular Te(0) manifesting as amorphous needle-like nanoparticles and extracellular Te(0) forming substantial microspheres and irregular accumulations, characterized by a trigonal crystalline phase. Similarly, Se(0) exhibited a diverse array of morphologies, including hexagonal, irregular, and needle-shaped structures, accompanied by a monoclinic crystalline phase. The formation of less mobile Te(0) and Se(0) nanostructures through novel and environmentally friendly processes by Aspergillus sp. 3A suggests it would be an excellent candidate for bioremediation in contaminated environments, such as the vicinity of deep geological repositories. It moreover holds immense potential for the recovery and synthesis of Te and Se nanostructures for use in numerous biotechnological and biomedical applications.

Resolving exit strategies of mycobacteria in Dictyostelium discoideum by combining high-pressure freezing with 3D-correlative light and electron microscopy.

The infection course of Mycobacterium tuberculosis is highly dynamic and comprises sequential stages that require damaging and crossing of several membranes to enable the translocation of the bacteria into the cytosol or their escape from the host. Many important breakthroughs such as the restriction of mycobacteria by the autophagy pathway and the recruitment of sophisticated host repair machineries to the Mycobacterium-containing vacuole have been gained in the Dictyostelium discoideum/M. marinum system. Despite the availability of well-established light and advanced electron microscopy techniques in this system, a correlative approach integrating both methods with near-native ultrastructural preservation is currently lacking. This is most likely due to the low ability of D. discoideum to adhere to surfaces, which results in cell loss even after fixation. To address this problem, we improved the adhesion of cells and developed a straightforward and convenient workflow for 3D-correlative light and electron microscopy. This approach includes high-pressure freezing, which is an excellent technique for preserving membranes. Thus, our method allows to monitor the ultrastructural aspects of vacuole escape which is of central importance for the survival and dissemination of bacterial pathogens.