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result(s) for
"Scanning transmission electron microscopy"
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Four-Dimensional Scanning Transmission Electron Microscopy (4D-STEM): From Scanning Nanodiffraction to Ptychography and Beyond
2019
Scanning transmission electron microscopy (STEM) is widely used for imaging, diffraction, and spectroscopy of materials down to atomic resolution. Recent advances in detector technology and computational methods have enabled many experiments that record a full image of the STEM probe for many probe positions, either in diffraction space or real space. In this paper, we review the use of these four-dimensional STEM experiments for virtual diffraction imaging, phase, orientation and strain mapping, measurements of medium-range order, thickness and tilt of samples, and phase contrast imaging methods, including differential phase contrast, ptychography, and others.
Journal Article
Ultraviolet Light-Induced Surface Changes of Tungsten Oxide in Air: Combined Scanning Transmission Electron Microscopy and X-ray Photoelectron Spectroscopy Analysis
by
Shibayama, Tamaki
,
Shiratsuchi, Yasuhiro
,
Nakagawa, Yuki
in
Catalysis
,
Contact angle
,
Dielectric films
2024
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.
Journal Article
Sporosarcina pasteurii can form nanoscale calcium carbonate crystals on cell surface
by
Montemagno, Carlo
,
Kumar, Aloke
,
Bhaduri, Swayamdipta
in
Bacteria
,
Biofilms
,
Biology and Life Sciences
2019
The bacterium Sporosarcina pasteurii (SP) is known for its ability to cause the phenomenon of microbially induced calcium carbonate precipitation (MICP). We explored bacterial participation in the initial stages of the MICP process at the cellular length scale under two different growth environments (a) liquid culture (b) MICP in a soft agar (0.5%) column. In the liquid culture, ex-situ imaging of the cellular environment indicated that S. pasteurii was facilitating nucleation of nanoscale crystals of calcium carbonate on bacterial cell surface and its growth via ureolysis. During the same period, the meso-scale environment (bulk medium) was found to have overgrown calcium carbonate crystals. The effect of media components (urea, CaCl2), presence of live and dead in the growth medium were explored. The agar column method allows for in-situ visualization of the phenomena, and using this platform, we found conclusive evidence of the bacterial cell surface facilitating formation of nanoscale crystals in the microenvironment. Here also the bulk environment or the meso-scale environment was found to possess overgrown calcium carbonate crystals. Extensive elemental analysis using Energy dispersive X-ray spectroscopy (EDS) and X-ray powder diffraction (XRD), confirmed that the crystals to be calcium carbonate, and two different polymorphs (calcite and vaterite) were identified. Active participation of S. pasteurii cell surface as the site of calcium carbonate precipitation has been shown using EDS elemental mapping with Scanning transmission electron microscopy (STEM) and scanning electron microscopy (SEM).
Journal Article
Single-particle cryo-EM structures from iDPC–STEM at near-atomic resolution
by
Müller-Caspary, Knut
,
Lazić, Ivan
,
Bosch, Eric G. T.
in
631/1647/2258/1258/1259
,
631/1647/2258/1258/1260
,
Bioinformatics
2022
In electron cryomicroscopy (cryo-EM), molecular images of vitrified biological samples are obtained by conventional transmission microscopy (CTEM) using large underfocuses and subsequently computationally combined into a high-resolution three-dimensional structure. Here, we apply scanning transmission electron microscopy (STEM) using the integrated differential phase contrast mode also known as iDPC–STEM to two cryo-EM test specimens, keyhole limpet hemocyanin (KLH) and tobacco mosaic virus (TMV). The micrographs show complete contrast transfer to high resolution and enable the cryo-EM structure determination for KLH at 6.5 Å resolution, as well as for TMV at 3.5 Å resolution using single-particle reconstruction methods, which share identical features with maps obtained by CTEM of a previously acquired same-sized TMV data set. These data show that STEM imaging in general, and in particular the iDPC–STEM approach, can be applied to vitrified single-particle specimens to determine near-atomic resolution cryo-EM structures of biological macromolecules.
This paper explores the use of scanning transmission electron microscopy (STEM) to vitrified biological samples for biomolecular structure elucidation. Integrated differential phase contrast (iDPC)–STEM imaging of keyhole limpet hemocyanin and tobacco mosaic virus enabled cryo-EM structure determination at 6.5 and 3.5 Å resolution, respectively.
Journal Article
Atomically unveiling the structure-activity relationship of biomacromolecule-metal-organic frameworks symbiotic crystal
2022
Crystallization of biomacromolecules-metal-organic frameworks (BMOFs) allows for orderly assemble of symbiotic hybrids with desirable biological and chemical functions in one voxel. The structure-activity relationship of this symbiotic crystal, however, is still blurred. Here, we directly identify the atomic-level structure of BMOFs, using the integrated differential phase contrast-scanning transmission electron microscopy, cryo-electron microscopy and x-ray absorption fine structure techniques. We discover an obvious difference in the nanoarchitecture of BMOFs under different crystallization pathways that was previously not seen. In addition, we find the nanoarchitecture significantly affects the bioactivity of the BMOFs. This work gives an important insight into the structure-activity relationship of BMOFs synthesized in different scenarios, and may act as a guide to engineer next-generation materials with excellent biological and chemical functions.
Biomolecule-metal-organic-frameworks allow for the creation of hybrid materials with desired biological and chemical function. Here, the authors refine the structure-function relationship by identifying the atomic-layer structure of the hybrids and show differences in structure upon different crystallisation pathways.
Journal Article
High Dynamic Range Pixel Array Detector for Scanning Transmission Electron Microscopy
by
Ralph, Daniel C.
,
Nguyen, Kayla X.
,
Philipp, Hugh T.
in
Data acquisition
,
Data collection
,
Design
2016
We describe a hybrid pixel array detector (electron microscope pixel array detector, or EMPAD) adapted for use in electron microscope applications, especially as a universal detector for scanning transmission electron microscopy. The 128×128 pixel detector consists of a 500 µm thick silicon diode array bump-bonded pixel-by-pixel to an application-specific integrated circuit. The in-pixel circuitry provides a 1,000,000:1 dynamic range within a single frame, allowing the direct electron beam to be imaged while still maintaining single electron sensitivity. A 1.1 kHz framing rate enables rapid data collection and minimizes sample drift distortions while scanning. By capturing the entire unsaturated diffraction pattern in scanning mode, one can simultaneously capture bright field, dark field, and phase contrast information, as well as being able to analyze the full scattering distribution, allowing true center of mass imaging. The scattering is recorded on an absolute scale, so that information such as local sample thickness can be directly determined. This paper describes the detector architecture, data acquisition system, and preliminary results from experiments with 80–200 keV electron beams.
Journal Article
Z Dependence of Electron Scattering by Single Atoms into Annular Dark-Field Detectors
2011
A simple parameterization is presented for the elastic electron scattering cross sections from single atoms into the annular dark-field (ADF) detector of a scanning transmission electron microscope (STEM). The dependence on atomic number, Z, and inner reciprocal radius of the annular detector, q0, of the cross section σ(Z,q0) is expressed by the empirical relation
\\[
\\sigma(Z,q_{0}) = A(q_{0})\\,Z^{n(Z,q_{0})}.
\\]
where A(q0) is the cross section for hydrogen (Z = 1), and the detector is assumed to have a large outer reciprocal radius. Using electron elastic scattering factors determined from relativistic Hartree-Fock simulations of the atomic electron charge density, values of the exponent n(Z,q0) are tabulated as a function of Z and q0, for STEM probe sizes of 1.0 and 2.0 Å. Comparison with recently published experimental data for single-atom scattering [Krivanek et al. (2010). Nature464, 571–574] suggests that experimentally measured exponent values are systematically lower than the values predicted for elastic scattering from low-Z atoms. It is proposed that this discrepancy arises from the inelastic scattering contribution to the ADF signal. A simple expression is proposed that corrects the exponent n(Z,q0) for inelastic scattering into the annular detector.
Journal Article
Physics Discovery in Nanoplasmonic Systems via Autonomous Experiments in Scanning Transmission Electron Microscopy
by
Ziatdinov, Maxim
,
Roccapriore, Kevin M.
,
Kalinin, Sergei V.
in
Active learning
,
automated experiment
,
Automation
2022
Physics‐driven discovery in an autonomous experiment has emerged as a dream application of machine learning in physical sciences. Here, this work develops and experimentally implements a deep kernel learning (DKL) workflow combining the correlative prediction of the target functional response and its uncertainty from the structure, and physics‐based selection of acquisition function, which autonomously guides the navigation of the image space. Compared to classical Bayesian optimization (BO) methods, this approach allows to capture the complex spatial features present in the images of realistic materials, and dynamically learn structure–property relationships. In combination with the flexible scalarizer function that allows to ascribe the degree of physical interest to predicted spectra, this enables physical discovery in automated experiment. Here, this approach is illustrated for nanoplasmonic studies of nanoparticles and experimentally implemented in a truly autonomous fashion for bulk‐ and edge plasmon discovery in MnPS3, a lesser‐known beam‐sensitive layered 2D material. This approach is universal, can be directly used as‐is with any specimen, and is expected to be applicable to any probe‐based microscopic techniques including other STEM modalities, scanning probe microscopies, chemical, and optical imaging. The scanning transmission electron microscope is autonomously operated using the live electron energy loss spectroscopy data stream. During operation and without any pretraining, deep kernel learning (DKL) is used to build structure–property relationships between annular dark field image patches and their corresponding spectral signatures. The knowledge gained on‐the‐fly guides each future measurement throughout the experiment, here leading to physical discovery.
Journal Article
In situ trapped high-density single metal atoms within graphene: Iron-containing hybrids as representatives for efficient oxygen reduction
by
Liu, Qin
,
Chen, Shuangming
,
Wang, Yu
in
Anchoring
,
Atomic structure
,
Atomic/Molecular Structure and Spectra
2018
Atomically dispersed catalysts have attracted attention in energy conversion applications because their efficiency and chemoselectivity for special catalysis are superior to those of traditional catalysts. However, they have limitations owing to the extremely low metal-loading content on supports, difficulty in the precise control of the metal location and amount as well as low stability at high temperatures. We prepared a highly doped single metal atom hybrid via a single-step thermal pyrolysis of glucose, dicyandiamide, and inorganic metal salts. High-angle annular dark field-scanning transmission electron microscopy (HAADF-STEM) and X-ray absorption fine structure spectroscopy (XAFS) revealed that nitrogen atoms doped into the graphene matrix were pivotal for metal atom stabilization by generating a metal-Nx coordination structure. Due to the strong anchoring effect of the graphene matrix, the metal loading content was over 4 wt.% in the isolated atomic hybrid (the Pt content was as high as 9.26 wt.% in the Pt-doped hybrid). Furthermore, the single iron-doped hybrid (Fe@N-doped graphene) showed a remarkable electrocatalytic performance for the oxygen reduction reaction. The peak power density was ∼199 mW·cm
−2
at a current density of 310 mA·cm
−2
and superior to that of a commercial Pt/C catalyst when it was used as a cathode catalyst in assembled zinc-air batteries. This work offered a feasible approach to design and fabricate highly doped single metal atoms (SMAs) catalysts for potential energy applications.
Journal Article