The γ″ phase (hexagonal structure with space group ${ P\bar{6}}2{ m}$) plays an important role in the strengthening of Mg–Gd–Y–Ag–Zr alloy. In this study, Cs-corrected high-angle annular dark-field scanning transmission electron microscopy was applied to characterize the Mg–Gd–Y–Ag–Zr alloy in different conditions (as-cast, solution-treated, and isothermally aged at 200 °C). The nucleation, growing process, and transformation behavior of the plate-shaped γ″ phase were systematically investigated on the atomic scale. We found that the nucleation sites of the γ″ phase were separated by close-packed planes of the Mg matrix and the γ″ phase developed in two perpendicular directions of $\langle 10\bar{1}0 \rangle$ and ⟨0001⟩. The growing process of the γ″ phase on the atomic scale was captured. The γ″ phase was thermodynamically stable at room temperature, and no transformation behavior of the γ″ phase was observed up to 200 h during isothermal aging at 200 °C.

It is pertinent to the safety case for geological disposal in the UK that the behaviour of vitrified wastes in proximity to cementitious materials is understood. In this study, vitrified simulant intermediate level nuclear waste (ILW) was subject to dissolution in a synthetic cement water solution to simulate disposal conditions. Results show that the presence of alkali / alkaline earth elements in the cementitious solution can be favourable, at least in the short-term, leading to lower dissolution rates associated with incorporation of these elements into the altered layer of the glass.

Atomically resolved imaging of materials enabled by the advent of aberration-corrected scanning transmission electron microscopy (STEM) has become a mainstay of modern materials science. However, much of the wealth of quantitative information contained in the fine details of atomic structure or spectra remains largely unexplored. In this article, we discuss new opportunities enabled by physics-informed big data and machine learning technologies to extract physical information from static and dynamic STEM images, ranging from statistical thermodynamics of alloys to kinetics of solid-state reactions at a single defect level. The synergy of deep-learning image analytics and real-time feedback further allows harnessing beam-induced atomic and bond dynamics to enable direct atom-by-atom fabrication. Examples of direct atomic motion over mesoscopic distances, engineered doping at selected lattice sites, and assembly of multiatomic structures are reviewed. These advances position the scanning transmission electron microscope to transition from a mere imaging tool toward a complete nanoscale laboratory for exploring electronic, phonon, and quantum phenomena in atomically engineered structures.

Defects in crystalline solids control the properties of engineered and natural materials, and their characterization focuses our strategies to optimize performance. Electron microscopy has served as the backbone of our understanding of defect structure and their interactions, owing to beneficial spatial resolution and contrast mechanisms that enable direct imaging of defects. These defects reside in complex microstructures and chemical environments, demanding a combination of experimental approaches for full defect characterization. In this article, we describe recent progress and trends in methods for examining defects using scanning electron microscopy platforms. Several emerging approaches offer attractive benefits, for instance, in correlative microscopy across length scales and in in situ studies of defect dynamics.

In situ nanomechanical testing in (scanning) transmission electron microscopy provides unique opportunities for studying fundamental deformation processes in materials. New insights have been gained by combining advanced imaging techniques with novel preparation methods and controlled loading scenarios. For instance, by applying in situ high-resolution imaging during tensile deformation of metallic nanostructures, the interplay of dislocation slip and surface diffusion has been identified as the key enabler of superplasticity. Evidence for dislocation pinning by hydrogen defect complexes has been provided by in situ imaging under cyclic pillar compression in a tunable gas environment. And, for the very first time, individual dislocations have been moved around in situ in two-dimensional materials by combining micromanipulation and imaging in a scanning electron microscope.

Nano-porous palladium (Pd) thin films could potentially be applied to hydrogen gas sensing materials with high sensitivity and selectivity. In our previous study, a nano-porous Pd film was fabricated with a three-dimensional network structure from an AlPd mother alloy film by a dealloying method using the chelating ability of an organic acid. This process was simple and environmentally friendly because it only required organic acid in a ppm concentration, and did not exhaust a strong acid waste solution, including heavy metal ions. This method was modified to improve the Pd purity of the dealloyed specimen, reaction rate, and morphology control. In this study, the existence of a composition undulation pattern was shown in the AlPd mother alloy film, and its effects on the morphology of the dealloyed specimen were evaluated. Furthermore, this pattern could be controlled by N2 gas addition to the Ar sputtering gas during the preparation of the AlPd mother alloy film.

The microstructure of In(As,Bi)/GaAs heterostructures grown by low-temperature molecular beam epitaxy with special attention to the interfaces was studied by scanning/transmission electron microscopy, energy dispersive X-ray microanalysis, and X-ray diffraction and reflectivity. Two samples grown at similar conditions with and without the presence of the Bi-contained layer, formed at 350 °C, are considered. These samples were jointly analyzed to clarify Bi influence on the crystal structure. Two types of QD-like clusters at the GaAs/In(As,Bi) interface were found. The first type exhibited a zinc blend crystal structure, which is typical for A3B5 semiconductors. The second type adopted a tetragonal PbO crystal structure and was found in different orientations. The joint analysis by electron microscopy and X-ray methods demonstrated that the incorporation of Bi atoms into the InAs layer leads to the strain relaxation at the interface in the growth direction. According to electron microscopy data, this strain release is more pronounced around the clusters of the second type.

In this paper, corrosion behavior of 2198 Al–Cu–Li alloy in different aging stages is investigated using immersion and electrochemical measurements in 3.5 wt% NaCl aqueous solution. The corrosion resistance is found to decrease from the solution-anneal to the peak-aged condition but increase after the peak-aged, which is due to microstructure evolution of three main kinds of precipitating phases with the aging process: T1 (Al2CuLi), θ′ (Al2Cu), and a few δ′ (Al3Li) phases. The anode T1 phase grows and increases with the aging treatment and becomes nearly unchanged after the peak-aged. Moreover, the cathode θ′ phase slightly decreases in the over-aged. The potentiodynamic polarization curves also indicate the most positive corrosion potential and the lowest corrosion current density in the peak-aged. The results of electrochemical impedance spectroscopy are in agreement with the corrosion morphologies. Furthermore, the related equivalent circuit is established to investigate the corrosion mechanism of this alloy.

Due to its excellent optical properties, gold nanomaterials with anisotropic morphology are playing an important role in biomedical applications, specifically in the use of Surface Enhanced Raman Spectroscopy (SERS) technique for biological assays. In this work, we verified the behavior of the star shape nanoparticle peaks obtained by chemical synthesis (precursor reactant: HAuCl4, cationic surfactant: CTAB) and whose peaks were formed from the different concentrations of gold seeds (55, 65, 75 and 85 ul) which were added to the total solution (5.275 ml). The shape and size of the nanoparticles was verified with a Hitachi S-5500 microscope with a BF & DF SEM / STEM detector, and for the diameter distribution (hydrodynamic) was carried out by the dynamic light distribution technique with a Malvern DLS system Zetasizer Nano ZS. Particle sizes (peak-to-peak considering) were obtained with variations from 107 to 166 nm. The results suggest adding 75 ul of gold seeds to obtain uniform nanostars with well defined peaks. These gold nano-stars could be applied for identification of specific membrane markers for the study of different types of cancer by the SERS technique.

Chlorophenols are among the priority listed water contaminants due to their estrogenic, mutagenic or carcinogenic health effects. The Ag/ZnO nanocomposites (NCs) were synthesized, characterized and tested for photacatalytic degradation of chlorophenols in water. The synthesis was done using zinc nitrate hexahydrate (ZnNO3. 6H2O) precursor and sodium hydroxide (NaOH). Silver nitrate (AgNO3) was added to ZnO and reduced with sodium brohydride to produce the silver nanoparticles (NPs) within the ZnO structure. The silver content was varied from 1, 3 and 5wt% for optimisation. The nanocomposites were characterised using ultraviolet - visible spectroscopy (UV-Vis), photolumniscence (PL), x-ray diffraction (XRD), and scanning transmission electron microscopy (STEM). The nanocomposites were tested for their photocatalytic properties on 2- chlorophenol (CP), 2- chlorophenol (CP) and 2,4- dichlorophenol (DCP) in water. The UV-Vis results showed that, as the amount of silver was increased a gradual slight red shift was observed. The XRD patterns for Ag/ZnO exhibited peaks that were characteristic of the hexagonal wurzite structure and peaks characteristic for Ag appeared at 38.24o, 44.37o, 64.67o and 77.58o corresponding to (111), (200), (220) and (311) reflection planes. STEM results showed the presence of Ag in ZnO with ZnO appearing as rods shapes. The EDX elemental analysis confirmed the presence of Ag in the Ag/ZnO nanocomposites with no contaminants peaks. On testing the nanocomposites for phohotocatalytic degradation of chlorophenols, addition of Ag to ZnO improved degradation of the chlorophenols compared to the pristine ZnO.

High-power single-mode (SM) and multi-mode (MM) InGaAs-AlGaAs strained quantum well (QW) lasers with emission wavelengths of 910 − 980 nm are extensively used in various fiber lasers and amplifiers for both telecom and defense applications. In particular, underseas and satellite communication systems require stringent reliability from these lasers. Since these lasers predominantly fail by catastrophic and sudden degradation due to COD, it is crucial especially for space satellite applications to investigate reliability, failure modes, and degradation mechanisms of these lasers. Catastrophic optical mirror damage (COMD) was known to be the only failure mode until our group reported a new failure mode in MM and SM InGaAs-AlGaAs strained QW lasers in 2009 and 2016, respectively. Our group reported that bulk failure due to catastrophic optical bulk damage (COBD) has become the dominant failure mode of both SM and MM lasers. Since there have been limited reports on COBD compared to COMD, the intent of this paper is to introduce our studies on COBD that have spanned the last decade. We investigated reliability, failure modes, and degradation processes in SM and MM InGaAs-AlGaAs strained QW lasers by performing short-term step-stress tests and long-term accelerated life-tests as well as failure mode analyses using various nondestructive and destructive micro-analytical techniques including electron beam induced current (EBIC), time-resolved electroluminescence (EL), deep level transient spectroscopy (DLTS), focused ion beam (FIB), and high-resolution TEM. EBIC and EL techniques were employed to study dark line defects generated in degraded lasers stressed under different test conditions. Time-resolved EL techniques were employed to study initiation and progressions of dark spots and dark lines in real time as lasers were aged. DLTS techniques were employed to study electron traps in both pristine and degraded lasers. Lastly, FIB and high-resolution TEM were employed to prepare cross sectional and plan view TEM specimens to study DLD areas in post-aged lasers. We also report our current understanding on degradation mechanisms responsible for COBD in both SM and MM lasers.

The origin of the extraordinary strengthening of the highly alloyed austenitic stainless steel Sanicro 25 during cyclic loading at 700 °C was investigated by the use of advanced scanning transmission electron microscopy (STEM). Along with substantial change of the dislocation structure, nucleation of two distinct populations of nanoparticles was revealed. Fully coherent Cu-rich nanoparticles were observed to be homogeneously dispersed with high number density along with nanometer-sized incoherent NbC carbides precipitating on dislocations during cyclic loading. Probe-corrected high-angle annular dark-field STEM imaging was used to characterize the atomic structure of nanoparticles. Compositional analysis was conducted using both electron energy loss spectroscopy and high spatial resolution energy dispersive X-ray spectroscopy. High-temperature exposure-induced precipitation of spatially dense coherent Cu-rich nanoparticles and strain-induced nucleation of incoherent NbC nanoparticles leads to retardation of dislocation movement. The pinning effects and associated obstacles to the dislocation motion prevent recovery and formation of the localized low-energy cellular structures. As a consequence, the alloy exhibits remarkable cyclic hardening at elevated temperatures.

Phase separation of InxGa1−xN into Ga-rich and In-rich regions has been studied by electron energy-loss spectroscopy (EELS) in a monochromated, aberration corrected scanning transmission electron microscope (STEM). We analyze the full spectral information contained in EELS of InGaN, combining for the first time studies of high-energy and low-energy ionization edges, plasmon, and valence losses. Elemental maps of the N K, In M4,5 and Ga L2,3 edges recorded by spectrum imaging at 100 kV reveal sub-nm fluctuations of the local indium content. The low energetic edges of Ga M4,5 and In N4,5 partially overlap with the plasmon peaks. Both have been fitted iteratively to a linear superimposition of reference spectra for GaN, InN, and InGaN, providing a direct measurement of phase separation at the nm-scale. Bandgap measurements are limited in real space by scattering delocalization rather than the electron beam size to ∼10 nm for small bandgaps, and their energetic accuracy by the method of fitting the onset of the joint density of states rather than energy resolution. For an In0.62Ga0.38N thin film we show that phase separation occurs on several length scales.

Transmission electron microscopy is a powerful technique for the analysis of solid samples, but it can also be used to image in liquid environments, gaining a unique view of processes and structures in liquids. Here, we describe recent developments in electron microscopy of liquids and discuss applications in several areas. We first describe closed-liquid-cell microscopy with its opportunities for visualizing electrochemical processes. We then discuss imaging of low-vapor-pressure liquids relevant to the operation of rechargeable batteries. Finally, we describe imaging of thick biological materials to obtain information on membrane proteins in intact mammalian cells that cannot be observed classically under dry or frozen conditions. Electron microscopy in liquid environments is developing rapidly and has the potential to solve key problems in materials science, physics, chemistry, and biology.

Although the strong coupling of polarization to spontaneous strain in ferroelectrics would impart a flux-closure with severe disclination strains, recent studies have successfully stabilized such a domain via a nano-scaled multi-layer growth. Nonetheless, the detailed distributions of polarizations in three-dimensions (3D) and how the strains inside a flux closure affect the structures of domain walls are still less understood. Here we report a 3D polarization texture of a 4-fold flux closure domain identified in tensile strained ferroelectric PbTiO3/SrTiO3 multilayer films. Ferroelectric displacement analysis based on aberration-corrected scanning transmission electron microscopic imaging reveals highly inhomogeneous strains with strain gradient above 107/m. These giant disclination strains significantly broaden the 90° domain walls, while the flexoelectric coupling at 180° domain wall is less affected. The present observations are helpful for understanding the basics of topological dipole textures and indicate novel applications of ferroelectrics through engineering strains.

Three-dimensional (3D) tomography using electrons and x-rays has pushed and expanded our understanding of the micro- and nanoscale spatial organization of inorganic, organic, and biological materials. While a significant impact on the field of materials science has already been realized from tomography applications, new advanced methods are quickly expanding the versatility of this approach to better link structure, composition, and function of complex 3D assemblies across multiple scales. In this article, we highlight several frontiers where new developments in tomography are empowering new science across biology, chemistry, and physics. The five articles that appear in this issue of MRS Bulletin describe some of these latest developments in detail, including analytical electron tomography, atomic resolution electron tomography, advanced recording schemes in scanning transmission electron microscopy (STEM) tomography, cryo-STEM tomography of whole cells, and multiscale correlative tomography.

Three-dimensional (3D) scanning transmission electron microscopy (STEM) has become one of the primary tools for analytical characterization in materials science and also finds increasing use in the life sciences. A number of different recording schemes exist for the acquisition of 3D data using STEM, each capturing different spatial frequencies and, thus, different information about the shape of a specimen. In this article, we present and compare different sampling approaches based on images with both large and small depth of field. We highlight the latest contribution to 3D data acquisition, the combined tilt, and focal series. This recording scheme combines the advantages of tilt series-based tomography with 3D data acquisition using a focal series and is particularly beneficial for imaging specimens with a thickness of 1 µm or greater.

This article highlights recent advances in analytical electron tomography (AET), the three-dimensional (3D) extension of conventional nanoanalytical techniques, in which electron energy loss, x-ray spectroscopy, and electron diffraction are combined with tomographic acquisition and reconstruction. Examples from the literature illustrate how new 3D information, gleaned from AET, provides insights into not just morphology and composition, but also the electronic, chemical, and optical properties of materials at the nanoscale. We describe how the “multidimensional” nature of AET leads to “big data” sets, how these can be analyzed optimally, and how AET may develop further.

The electron microscope has made paramount contributions to understanding the structure of biological molecules, cells, and tissues. In general, the most faithful preservation of biological specimens and other soft-organic materials is achieved through cryogenic fixation. The embedding medium is the native aqueous environment itself, immobilized in vitrified form by rapid or pressurized cooling. Until recently, imaging of such vitrified thin specimens by electron cryo-microscopy has been nearly synonymous with wide-field transmission electron microscopy (TEM). Several new approaches have entered the cryo-microscopy field, including soft x-ray imaging, serial surface imaging using focused ion beam scanning electron microscopy, phase plates, and scanning TEM (STEM). In this article, we focus on the STEM method and its adaptation to biological cryo-microscopy. Cryogenic imaging of unstained specimens by STEM introduces specific challenges. Difficulties were long considered insurmountable, and the potential advantages were underappreciated. Future developments in experimental setup and detector technologies will allow for extension of the method to thicker specimens with improved resolution and analytic capabilities.

The effects of pre-treatments on the precipitate microstructures of an Al–Zn–Mg–Cu alloy are investigated. Meanwhile, the creep-rupture behavior of the under-aged and peak-aged alloys are comparatively analyzed. Additionally, the effects of pre-treatment on the fracture mechanisms are discussed. It is found that the precipitate microstructures are sensitive to pre-treatments. The intragranular precipitates of the peak-aged alloy are larger than those of the under-aged. The precipitate free zone of the peak-aged alloy is wider than that of the under-aged. Some large intergranular precipitates appear on the grain boundaries of the under-aged alloy, and induce the nucleation of microvoids. Eventually, the creep fracture of the under-aged alloy is accelerated. Therefore, the differences in microstructures lead to the shorter creep-rupture life of the under-aged alloy, compared to the peak-aged alloy.