STEM Detector Research Articles

Characterization of extended defects in 2D materials using aperture-based dark-field STEM in SEM

Quantitative diffraction contrast analysis with defined diffraction vectors is a well-established method in TEM for studying defects in crystalline materials. A comparable transmission technique is however not available in the more widely used SEM platforms. In this work, we transfer the aperture-based dark-field imaging method from the TEM to the SEM, thus enabling quantitative diffraction contrast studies at lower voltages in SEM. This is achieved in STEM mode by inserting a custom-made aperture between the sample and the STEM detector and centering the hole on a desired reflection. To select individual reflections for dark-field imaging, we use our Low Energy Nanodiffraction (LEND) setup [Schweizer et al., Ultramicroscopy 213, 112956 (2020)], which captures transmission diffraction patterns from a fluorescent screen positioned below the sample. The aperture-based dark-field STEM method is particularly useful for studying extended defects in 2D materials, where (i) stronger diffraction at the lower voltages used in SEM is advantageous, but (ii) two-beam conditions cannot be established, making quantitative diffraction contrast analysis with standard bright-field and annular dark-field detectors impossible. We demonstrate the method by studying basal plane dislocations in bilayer graphene, which have attracted considerable research interest due to their exceptional structural and electronic properties. Direct comparison of results obtained on identical dislocations by the established TEM method and by the new aperture-based dark-field STEM method in SEM shows that a reliable Burgers vector analysis is possible by applying the well-known g·b=0 invisibility criterion. We further use the LEND setup to acquire 4D-STEM data and show that the virtual dark-field images match well with those in aperture-based dark-field STEM images for reliable Burgers vector analysis.

A New Fully Integrated Retractable 4D STEM Detector for Scanning Electron Microscopes Using Timepix3 Based Pixelated Detector

A New Fully Integrated Retractable 4D STEM Detector for Scanning Electron Microscopes Using Timepix3 Based Pixelated Detector

Simultaneous Acquisition of 4D and EELS Data by Newly Developed Pixelated STEM Detector

Simultaneous Acquisition of 4D and EELS Data by Newly Developed Pixelated STEM Detector

Towards Quantitative Imaging of Atomic Vibrations with Multi-dimensional STEM Detectors

Towards Quantitative Imaging of Atomic Vibrations with Multi-dimensional STEM Detectors

GaN atomic electric fields from a segmented STEM detector: Experiment and simulation.

Atomic electric fields in a thin GaN sample are measured with the centre-of-mass approach in 4D-scanning transmission electron microscopy (4D-STEM) using a 12-segmented STEM detector in a Spectra 300 microscope. The electric fields, charge density and potential are compared to simulations and an experimental measurement using a pixelated 4D-STEM detector. The segmented detector benefits from a high recording speed, which enables measurements at low radiation doses. However, there is measurement uncertainty due to the limited number of segments analysed in thisstudy.

Quarantotto: A 48-segment STEM detector for enhanced STEM performance and new applications

Quarantotto: A 48-segment STEM detector for enhanced STEM performance and new applications

Simultaneous Acquisition of 4D and EELS Data by Newly Developed Pixelated STEM Detector

Simultaneous Acquisition of 4D and EELS Data by Newly Developed Pixelated STEM Detector

Atomic-scale imaging of polyvinyl alcohol crystallinity using electron ptychography

Polyvinyl alcohol (PVA) is considered to have great potential in medical, pharmaceutical, and packaging applications because of its outstanding biocompatibility, water solubility, low density and relatively low cost. PVA crystallinity, central to the materials properties, has been studied by X-ray diffraction, but two possible crystal structures are mooted. Electron microscopic techniques can potentially image PVA at high resolution. Still, it is challenging for conventional electron microscopies because of the relatively low crystallinity of PVA, its severe beam sensitivity, and the poor contrast of light elements. Electron ptychography makes use of a 4D STEM dataset comprising the intensity in the STEM detector plane recorded as a function of each probe position and has lower sample damage and better phase-contrast compared to traditional techniques. Here, we use electron ptychography to image PVA crystallinity. The reconstructed images, which show good agreement in the unit cell dimension with X-ray diffraction data, can show how the atoms order in the materials, however, deviations from previous models derived from X-ray diffraction are observed. To interpret the data, we propose a series of changes based on previous models to formulate a description of PVA crystal structure. Simulated results from this new model accord well with the experimental images. This study manages to image both carbon and oxygen atoms in PVA, which has not previously been achieved by any conventional method. The results are expected to bring a new and deeper understanding of PVA crystal structure, and illustrate the opportunity presented by this approach for directly imaging molecular order in polymer crystals.

Defect Contrast with 4D-STEM: Understanding Crystalline Order with Virtual Detectors and Beam Modification.

Material properties strongly depend on the nature and concentration of defects. Characterizing these features may require nano- to atomic-scale resolution to establish structure-property relationships. 4D-STEM, a technique where diffraction patterns are acquired at a grid of points on the sample, provides a versatile method for highlighting defects. Computational analysis of the diffraction patterns with virtual detectors produces images that can map material properties. Here, using multislice simulations, we explore different virtual detectors that can be applied to the diffraction patterns that go beyond the binary response functions that are possible using ordinary STEM detectors. Using graphene and lead titanate as model systems, we investigate the application of virtual detectors to study local order and in particular defects. We find that using a small convergence angle with a rotationally varying detector most efficiently highlights defect signals. With experimental graphene data, we demonstrate the effectiveness of these detectors in characterizing atomic features, including vacancies, as suggested in simulations. Phase and amplitude modification of the electron beam provides another process handle to change image contrast in a 4D-STEM experiment. We demonstrate how tailored electron beams can enhance signals from short-range order and how a vortex beam can be used to characterize local symmetry.

Electron Ptychographic Phase Imaging of Beam-sensitive All-inorganic Halide Perovskites Using Four-dimensional Scanning Transmission Electron Microscopy.

Halide perovskites (HPs) are promising candidates for optoelectronic devices, such as solar cells or light-emitting diodes. Despite recent progress in performance optimization and low-cost manufacturing, their commercialization remains hindered due to structural instabilities. While essential to the development of the technology, the relation between the microscopic properties of HPs and the relevant degradation mechanisms is still not well understood. The sensitivity of HPs toward electron-beam irradiation poses significant challenges for transmission electron microscopy (TEM) investigations of structure and degradation mechanisms at the atomic scale. However, technological advances and the development of direct electron cameras (DECs) have opened up a completely new field of electron microscopy: four-dimensional scanning TEM (4D-STEM). From a 4D-STEM dataset, it is possible to extract not only the intensity signal for any STEM detector geometry but also the phase information of the specimen. This work aims to show the potential of 4D-STEM, in particular, electron exit-wave phase reconstructions via focused probe ptychography as a low-dose and dose-efficient technique to image the atomic structure of beam-sensitive HPs. The damage mechanism under conventional irradiation is described and atomically resolved almost aberration-free phase images of three all-inorganic HPs, CsPbBr3, CsPbIBr2, and CsPbI3, are presented with a resolution down to the aperture-constrained diffraction limit.

Precise measurement of the electron beam current in a TEM

Modern quantitative TEM methods such as the ζ-factor technique require precise knowledge of the electron beam current. To this end, a macroscopic Faraday cup was designed and constructed. It can replace the viewing screen in the projection chamber of a TEM and guarantees highly accurate measurement of the electron beam with precision only limited by the used amperemeter. The easy to install, affordable device is shown to be highly apt for precision measurement of currents >5pA. The Faraday cup results are used for an assessment and a comparison of various other beam current measurement methods. It is found that the built-in screen amperemeter of the used TEM is quite inaccurate and that measurements using the screen in general tend to underestimate the current. If present, the drift tube of a spectrometer can also be used as a Faraday cup, but certain described peculiarities have to be taken into account. Direct ultrafast electron detection cameras allow precise measurement at very small currents. For the electron counting technique, which exploits single electron detection capabilities of STEM detectors, a systematic current underestimation was observed and investigated. This results in a reformulated routine for the method and with these improvements it is demonstrated to be capable of accurate high-precision measurements for currents <5pA.

Introduction to Electron Ptychography by Pixelated STEM Detector

Introduction to Electron Ptychography by Pixelated STEM Detector

Application of Modern Scanning/Transmission Electron Microscope with Pixelated STEM Detector for Radiation Damage Study

Application of Modern Scanning/Transmission Electron Microscope with Pixelated STEM Detector for Radiation Damage Study

Visualization of unstained homo/heterogeneous DNA nanostructures by low-voltage scanning transmission electron microscopy

Three-dimensional (3D) homo/heterogeneous DNA nanostructures were studied with low-voltage scanning transmission electron microscopy (LV-STEM). Four types of 3D DNA nanostructures were designed and fabricated by the origami method including newly proposed protocols. The low-energy electron probe and optimized dark-field STEM detector enabled individual unstained DNA nanostructures to be clearly imaged by the single acquisition without the averaging process. For the vertically stacked double structures, assembled through modified single-stranded domains, and the structures containing a square opening (i.e., a hole) in the center, the LV-STEM successfully reveals the vertical information of these 3D structures as the contrast differences compared to the reference. For the heterogeneous structures, the LV-STEM visualized both regions of the functionalized gold nanoparticles and the DNA base structure with distinct contrasts. This study introduces a straightforward method to fabricate stackable DNA nanostructures or nanoparticles by replacing a relatively small number of incumbent DNA strands, which could realize the simple and sophisticated fabrication of higher-order 3D DNA homo/hetero nanostructures. Together with these design techniques of DNA nanostructures, this study has demonstrated that the LV-STEM is the swift and simple method for visualizing the 3D DNA nanostructures and certifying the fabricated products as the specified design, which is applicable to various research fields on soft materials including DNA nanotechnology.

Local Structural Study of Ferroelectric Domain Boundaries Using STEM-CBED with a Fast Pixelated STEM Detector

Local Structural Study of Ferroelectric Domain Boundaries Using STEM-CBED with a Fast Pixelated STEM Detector

Investigation of Image Contrast in Biological Samples by Pixelated STEM Detector

Investigation of Image Contrast in Biological Samples by Pixelated STEM Detector

Synthesis of gold and silver nanoparticles using flavonoid quercetin and their effects on lipopolysaccharide induced inflammatory response in microglial cells.

Quercetin is a plant origin phytochemical with several pharmaceutical activities such as antioxidant, immunomodulatory, and anti-inflammatory effects. However, consumption of quercetin is limited due to its low aqueous solubility and poor bioavailability. The aim of the present study was to synthesize silver and gold nanoparticles of quercetin with a view to improve its aqueous phase solubility and investigate the effects on LPS-induced neuroinflammation in BV-2 microglial cells. The average size of silver and gold-quercetin nanoparticles was 53 and 27nm, respectively. Absorption peaks in the UV-Vis spectra were observed at 555 and 405nm for gold and silver-quercetin nanoparticles, respectively. The particle size and mapping of silver and gold-quercetin nanoparticles were also determined using a STEM detector. The inflammatory stimulation of the BV-2 cells with LPS caused an elevated release of proinflammatory prostaglandin, E2, nitric oxide (NO), upregulated cyclooxygenase-2, inducible NO synthase mRNA, and protein levels, which were markedly inhibited by the pretreatment with gold-quercetin nanoparticles (highly soluble in water) without causing any cytotoxic effects. The findings of the present study suggest that the potential of gold-quercetin nanoparticles are much better than quercetin and that gold-quercetin nanoparticles might provide protection against inflammatory neurodegenerative disease via suppression of acute microglial activation.

Quantitative STEM imaging of electron beam induced mass loss of epoxy resin sections

In sample preparation of biological samples for electron microscopy, many types of embedding media are widely used. Unfortunately, none of them is perfectly resistant to beam induced damage. The article is focused on mass loss measuring of pure epoxy resin EMbed 812 that replaced Epon – the most widely used embedding resin for biological electron microscopy, in a form of ultrathin sections with thicknesses ranging from 30 to 100 nm. The STEM imaging was performed in a quantitative way which allowed us to estimate the mass loss directly up to the total dose of 3000 e−/nm2. For data acquisition we used SEM equipped with a commercial STEM detector working at a relatively low acceleration voltage of 30 kV. In this study we estimated the influence of various factors which can affect the endurance of the epoxy resin EMbed 812 ultrathin sections under an electron beam, such as the sample aging, differences between storing the samples in forms of ultrathin sections and whole blocks, ultrathin sections thicknesses, temperature of the sample, probe current, and one or two-sided carbon coating of ultrathin sections. The aim of this work is to investigate beam induced mass loss at electron energies of SEM and find out how to reduce the mass loss.

Atmospheric scanning electron microscopy and its applications for biological specimens.

Scanning electron microscopy in ambient conditions (Air-SEM) was developed recently and has been used mainly for industrial applications. We assessed the potential application of Air-SEM for the analysis of biological tissues by using rat brain, kidney, human tooth, and bone. Hard tissues prepared by grinding and frozen sections were observed. Basic cytoarchitecture of bone and tooth was identified in the without heavy metal staining. Kidney tissue prepared using routine SEM methodology yielded images comparable to those of field emission (FE)-SEM. Sharpness was lower than that of FE-SEM, but foot process of podocytes was observed at high magnification. Air-SEM observation of semithin sections of kidney samples revealed glomerular basement membrane and podocyte processes, as seen using conventional SEM. Neuronal structures of soma, dendrites, axons, and synapses were clearly observed by Air-SEM with STEM detector and were comparable to conventional transmission electron microscopy images. Correlative light and electron microscopy observation of zebrafish embryos based on fluorescence microscopy and Air-SEM indicated the potential for a correlative approach. However, the image quality should be improved before becoming routine use in biomedical research.

Low Dose Imaging by STEM Ptychography Using Pixelated STEM Detector

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