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4D scanning transmission electron microscope (STEM) techniques have been increasingly featured among the electron microscopy characterization approaches, as they provide a perspective of improved information retrieval from samples overall. To make 4D STEM experiments as viable as conventional STEM image acquisition, the recording of diffraction patterns with a pixelated detector at fast frame rates, sufficient sensitivity to capture single electron hits, and high dynamic range is necessary. This paper addresses the recent development in hybrid-pixel detector technology that now allows 4D STEM experiments with a similar setup to conventional STEM imaging with pixel collection time under 10 µs. Application examples on virtual STEM detectors and crystal phase-orientation mapping are presented. [ABSTRACT FROM AUTHOR]

Over the last decade, scanning transmission electron microscopy has become one of the most powerful tools to characterise nanomaterials at the atomic scale. Often, the ultimate goal is to retrieve the three-dimensional structure, which is very challenging since small species are typically sensitive to electron irradiation. Nevertheless, measuring individual atomic positions is crucial to understand the relation between the structure and physicochemical properties of these (nano)materials. In this review, we highlight the latest approaches that are available to reveal the 3D atomic structure of small species. Finally, we will provide an outlook and will describe future challenges where the limits of electron microscopy will be pushed even further.

In this report, we applied annular bright-field and annular dark-field low-energy (30 keV) scanning transmission electron microscopy imaging to a vitreous ice-embedded biological macromolecule, T4 phage, to investigate the applicability of these methods for morphological investigation and sample screening. Multiple camera lengths were examined to find the optimal acceptance angle for both modes. Image clarity differed substantially between the modes, with the presence of ice also strongly influencing the quality of acquired micrographs. In annular dark-field mode, the proper discrimination of electrons scattered by the specimen from those scattered by the background ice was found to be difficult due to the severe overlap of the scattered electrons. The resulting micrographs lacked clarity, and the ice-embedded phage particles could only be discerned after post-processing image adjustment. However, in annular bright-field mode, despite similar overlapping of the scattered electrons, it was possible to assess the morphology and intactness of the specimen in the embedding ice, suggesting that this mode may find utility in low-energy cryo-scanning transmission electron microscopy imaging methods., (© The Author(s) 2022. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.)

We present a new method of multiple immunolabeling that is suitable for a broad spectrum of biomedical applications. The general concept is to label both sides of the ultrathin section with the thickness of 70-80 nm with different antibodies conjugated to gold nanoparticles and to distinguish the labeled side by advanced imaging methods with high resolution scanning electron microscopy, such as by correlating images acquired at different energies of primary electrons using different signals. From the Clinical Editor The use of transmission electron microscopy has become an indispensible tool in the detection of cellular proteins. In this short but interesting article, the authors described their new method of labeling and the identification of four different proteins simultaneously, which represents another advance in imaging technique. [ABSTRACT FROM AUTHOR]

A Mo-V-Nb-Te-O oxidation catalyst has been imaged using scanning transmission electron microscopy at 780 K, which is slightly above its operating temperature. We observe a sublattice disordering of the corner-sharing octahedra forming the catalytic sites containing V while the edge-sharing pentagonal bipyramidal {Nb(Mo)} sublattice remains structurally more rigid and thereby maintains the overall structural integrity of the catalyst. Imaging the termination of the edges of the [001] basal zones at room temperature reveal a preference for presence of a closed network of secondary structural {Nb(Mo)} units providing further evidence of the stability of this sublattice structure. We propose that sublattice disordering of catalytic sites enables structural flexibility to accommodate different oxidation states during multistep chemical reactions within a more rigid superstructure and presents a new paradigm for compositionally and structurally complex catalysts. [ABSTRACT FROM AUTHOR]

The lithium-rich layered oxides are one of the most attractive cathode materials for lithium-ion batteries. Here, two types of Li 1.20 Ni 0.32 Co 0.004 Mn 0.476 O 2 were synthesized using Li 2 CO 3 and LiOH as lithium sources. An electrochemical activation process occurs in Li 1.2 Ni 0.32 Co 0.004 Mn 0.476 O 2 prepared from Li 2 CO 3 (LLO-1), while no obvious activation in Li 1.2 Ni 0.32 Co 0.004 Mn 0.476 O 2 prepared from LiOH (LLO-2) is observed. Via advanced scanning transmission electron microscopy (STEM), we found that Li 2 MnO 3 -like structure is rich in the surface region of LLO-2. The study provides a direct explanation for the electrochemical activation of lithium-rich materials. The sample with more LiMO 2 -like phase at the surface region shows a better cycling performance. It is likely that more LiMO 2 -like phase at the surface region could stabilize the interface and improve the cycling performance of the Li-rich cathode materials. [ABSTRACT FROM AUTHOR]

Graphene is an ultrathin, impervious membrane. The controlled introduction of nanoscale pores in graphene would lead to applications that involve water purification, chemical separation, and DNA sequencing. However, graphene nanopores are unstable against filling by carbon adatoms. Here, using aberration-corrected scanning transmission electron microscopy and density-functional calculations, we report that Si atoms stabilize graphene nanopores by bridging the dangling bonds around the perimeter of the hole. Si-passivated pores remain intact even under intense electron beam irradiation, and they were observed several months after the sample fabrication, demonstrating that these structures are intrinsically robust and stable against carbon filling. Theoretical calculations reveal the underlying mechanism for this stabilization effect: Si atoms bond strongly to the graphene edge, and their preference for tetrahedral coordination forces C adatoms to form dendrites sticking out of the graphene plane, instead of filling the nanopore. Our results provide a novel way to develop stable nanopores, which is a major step toward reliable graphene-based molecular translocation devices. [ABSTRACT FROM AUTHOR]

Abstract: Quantitative analysis of lattice resolved images generated by scanning transmission electron microscopy (STEM) requires specification of probe characteristics, such as defocus, aberration and source distribution. In this paper we show that knowledge of such characteristics is unnecessary for quantitative interpretation, if the signal is integrated over a unit cell. Such a condition, whether the result of experimental setup or post-processing of lattice resolved images, reduces the intensity distribution to that of channelling contrast, where the signal for plane wave incidence is averaged over the angular range of the probe, and the result is independent of the probe characteristics. We use a Bloch wave model to show analytically how this applies to all forms of STEM imaging, such as that formed by annular dark field or backscatter detection, as well as characteristic X-ray fluorescence or electron energy loss. As a specific example, we consider how the signal from an annular dark field detector can be used to determine specimen thickness via a transfer curve for the zone axis and scattering geometries employed. This method has advantages over matching lattice images with calculations since these are sensitive to probe coherence and aberration, and saturation of the on-column intensity is approached more rapidly. [Copyright &y& Elsevier]

Incorporating magnetism into two-dimensional (2D) van der Waals (vdW) heterostructures is crucial for the development of functional electronic and magnetic devices. Here, we show that Nb 3 X 8 (X = Cl, Br) is a family of 2D layered trimerized kagomé magnets that are paramagnetic at high temperatures and undergo a first-order phase transition on cooling to a singlet magnetic state. X-ray diffraction shows that a rearrangement of the vdW stacking accompanies the magnetic transition, with high- and low-temperature phases consistent with scanning transmission electron microscopy images of the end members α-Nb 3 Cl 8 and β-Nb 3 Br 8 . The temperature of this transition is systematically varied across the solid solution Nb 3 Cl 8- x Br x ( x = 0-8), with x = 6 having transitions near room temperature. The solid solution also varies the optical properties, which are further modulated by the phase transition. As such, they provide a platform on which to understand and exploit the interplay between dimensionality, magnetism, and optoelectronic behavior in vdW materials.

Organic surfactant controls the synthesis of nanocrystals (NCs) with uniform size and morphology by attaching on the surface of NCs and further facilitates their assembly into ordered superstructure, which produces versatile functional nanomaterials for practical applications. It is essential to directly resolve the surfactant molecules on the surface of NCs to improve the understanding of surface chemistry of NCs. However, the imaging resolution and contrast are insufficient for a single molecule of organic surfactant on NCs. In this work, direct characterization of organic surfactant on CeO 2 NCs is conducted by using the state-of-the-art aberration corrected scanning transmission electron microscopy (STEM) imaging and electron energy loss spectra (EELS) techniques. The explicit evidence for the existence and distribution of organic surfactant on CeO 2 NCs are obtained on the atomic scale by EELS elemental mapping. Besides, STEM imaging parameters are systematically adjusted and optimized for the direct imaging of a single molecular chain of organic surfactant on CeO 2 NCs. Such direct visualization of organic surfactant molecule on the surface of NCs can be a significant step forward in the fields of nanomaterials surface chemistry and materials characterization., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

We present a new method of multiple immunolabeling that is suitable for a broad spectrum of biomedical applications. The general concept is to label both sides of the ultrathin section with the thickness of 70-80 nm with different antibodies conjugated to gold nanoparticles and to distinguish the labeled side by advanced imaging methods with high resolution scanning electron microscopy, such as by correlating images acquired at different energies of primary electrons using different signals. From the Clinical Editor: The use of transmission electron microscopy has become an indispensible tool in the detection of cellular proteins. In this short but interesting article, the authors described their new method of labeling and the identification of four different proteins simultaneously, which represents another advance in imaging technique., (Copyright © 2015 Elsevier Inc. All rights reserved.)

Graphene is an ultrathin, impervious membrane. The controlled introduction of nanoscale pores in graphene would lead to applications that involve water purification, chemical separation, and DNA sequencing. However, graphene nanopores are unstable against filling by carbon adatoms. Here, using aberration-corrected scanning transmission electron microscopy and density-functional calculations, we report that Si atoms stabilize graphene nanopores by bridging the dangling bonds around the perimeter of the hole. Si-passivated pores remain intact even under intense electron beam irradiation, and they were observed several months after the sample fabrication, demonstrating that these structures are intrinsically robust and stable against carbon filling. Theoretical calculations reveal the underlying mechanism for this stabilization effect: Si atoms bond strongly to the graphene edge, and their preference for tetrahedral coordination forces C adatoms to form dendrites sticking out of the graphene plane, instead of filling the nanopore. Our results provide a novel way to develop stable nanopores, which is a major step toward reliable graphene-based molecular translocation devices.