2.5-dimensional covalent organic frameworks.

Covalently bonded crystalline substances with micropores have broad applications. Covalent organic frameworks (COFs) are representative of such substances. They have so far been classified into two-dimensional (2D) and three-dimensional (3D) COFs.

Development of a secondary electron energy analyzer for a transmission electron microscope.

A secondary electron (SE) energy analyzer was developed for a transmission electron microscope. The analyzer comprises a microchannel plate (MCP) for detecting electrons, a coil for collecting SEs emitted from the specimen, a tube for reducing the number of backscattered electrons incident on the MCP, and a retarding mesh for selecting the energy of SEs incident on the MCP. The detection of the SEs associated with charging phenomena around a charged specimen was attempted by performing electron holography and SE spectroscopy using the energy analyzer.

Electron ptychographic phase imaging of light elements in crystalline materials using Wigner distribution deconvolution.

Recent development in fast pixelated detector technology has allowed a two dimensional diffraction pattern to be recorded at every probe position of a two dimensional raster scan in a scanning transmission electron microscope (STEM), forming an information-rich four dimensional (4D) dataset. Electron ptychography has been shown to enable efficient coherent phase imaging of weakly scattering objects from a 4D dataset recorded using a focused electron probe, which is optimised for simultaneous incoherent Z-contrast imaging and spectroscopy in STEM. Therefore coherent phase contrast and incoherent Z-contrast imaging modes can be efficiently combined to provide a good sensitivity of both light and heavy elements at atomic resolution.

Phase-contrast scanning transmission electron microscopy.

This report introduces the first results obtained using phase-contrast scanning transmission electron microscopy (P-STEM). A carbon-film phase plate (PP) with a small center hole is placed in the condenser aperture plane so that a phase shift is introduced in the incident electron waves except those passing through the center hole. A cosine-type phase-contrast transfer function emerges when the phase-shifted scattered waves interfere with the non-phase-shifted unscattered waves, which passed through the center hole before incidence onto the specimen.

Magnified pseudo-elemental map of atomic column obtained by Moiré method in scanning transmission electron microscopy.

Moiré method in scanning transmission electron microscopy allows observing a magnified two-dimensional atomic column elemental map of a higher pixel resolution with a lower electron dose unlike conventional atomic column mapping. The magnification of the map is determined by the ratio between the pixel size and the lattice spacing. With proper ratios for the x and y directions, we could observe magnified elemental maps, homothetic to the atomic arrangement in the sample of SrTiO3 [0 0 1].

Development of Cs and Cc correctors for transmission electron microscopy.

Novel spherical aberration (Cs) and chromatic aberration (Cc) correctors, which correct aberrations using a new principle, were developed. The asymmetric Cs correctors were designed for use in the probe- and image-forming systems at 300 kV to diminish undesired parasitic aberrations. The correctors composed of non-equivalent multipoles connecting with a demagnifying transfer doublet in the system.

Element discrimination in a hexagonal boron nitride nanosheet by aberration corrected transmission electron microscopy.

Boron nitride nanosheets prepared by an exfoliation technique were observed by aberration corrected transmission electron microscopy at 300 kV acceleration voltage. Single boron and nitrogen atoms in a monolayer region were imaged with different image contrast; a boron atom gave 16% less intensity reduction than a nitrogen atom. The number of atoms at each hexagonal ring site was determined by the image intensity that changed discretely with a 0.

Annular electron energy-loss spectroscopy in the scanning transmission electron microscope.

We study atomic-resolution annular electron energy-loss spectroscopy (AEELS) in scanning transmission electron microscopy (STEM) imaging with experiments and numerical simulations. In this technique the central part of the bright field disk is blocked by a beam stop, forming an annular entry aperture to the spectrometer. The EELS signal thus arises only from electrons scattered inelastically to angles defined by the aperture.

Direct imaging of hydrogen-atom columns in a crystal by annular bright-field electron microscopy.

Enhancing the imaging power of microscopy to identify all chemical types of atom, from low- to high-atomic-number elements,would significantly contribute for a direct determination of material structures. Electron microscopes have successfully provided images of heavy-atom positions, particularly by the annular dark-field method, but detection of light atoms was difficult owing to their weak scattering power. Recent developments of aberration-correction electron optics have significantly advanced the microscope performance, enabling identification of individual light atoms such as oxygen, nitrogen, carbon, boron and lithium.

Quantitative annular dark-field STEM images of a silicon crystal using a large-angle convergent electron probe with a 300-kV cold field-emission gun.

Annular dark-field scanning transmission electron microscope (ADF-STEM) images of an Si (001) crystal were obtained by using an aberration-corrected electron microscope, at 30-mrad convergent probe and cold field-emission gun at 300 kV. The intensity of ADF-STEM images, that is, the number of scattered electrons relative to the incident electrons, obtained for specimen thickness from 10 to 50 nm was compared quantitatively with  absorptive multi-slice simulation. The column and background intensities were analyzed by column-by-column two-dimensional Gaussian fitting.

Dependence of beam broadening on detection angle in scanning transmission electron microtomography.

It has been shown that scanning transmission electron microtomography (STEMT) is quite effective for observing specimens with thicknesses on the order of micrometers in three dimensions (3D). In STEMT, the specimen is scanned using a focused electron beam, and the electrons from the convergence point are detected at the detector placed at a certain detection angle. Until recently, a wide detection angle corresponding to the mode often called the dark-field (DF) mode was mainly used.

Performance of low-voltage STEM/TEM with delta corrector and cold field emission gun.

To reduce radiation damage caused by the electron beam and to obtain high-contrast images of specimens, we have developed a highly stabilized transmission electron microscope equipped with a cold field emission gun and spherical aberration correctors for image- and probe-forming systems, which operates at lower acceleration voltages than conventional transmission electron microscopes. A delta-type aberration corrector is designed to simultaneously compensate for third-order spherical aberration and fifth-order 6-fold astigmatism. Both were successfully compensated in both scanning transmission electron microscopy (STEM) and transmission electron microscopy (TEM) modes in the range 30-60 kV.

New area detector for atomic-resolution scanning transmission electron microscopy.

A new area detector for atomic-resolution scanning transmission electron microscopy (STEM) is developed and tested. The circular detector is divided into 16 segments which are individually optically coupled with photomultiplier tubes. Thus, 16 atomic-resolution STEM images which are sensitive to the spatial distribution of scattered electrons on the detector plane can be simultaneously obtained.

Direct imaging of lithium atoms in LiV₂O₄ by spherical aberration-corrected electron microscopy.

We visualized lithium atom columns in LiV₂O₄ crystals by combining scanning transmission electron microscopy with annular bright field (ABF) imaging using a spherical aberration-corrected electron microscope (R005) viewed from the [110] direction. The incident electron beam was coherent with a convergent angle of 30 mrad (semi-angle), and the detector collected scattered electrons over 20-30 mrad (semi-angle). The ABF image showed dark dots corresponding to lithium, vanadium and oxygen columns.

Visualizing and identifying single atoms using electron energy-loss spectroscopy with low accelerating voltage.

Visualizing atoms and discriminating between those of different elements is a goal in many analytical techniques. The use of electron energy-loss spectroscopy (EELS) in such single-atom analyses is hampered by an inherent difficulty related to the damage caused to specimens by incident electrons. Here, we demonstrate the successful EELS single-atom spectroscopy of various metallofullerene-doped single-wall nanotubes (known as peapods) without massive structural destruction.

STEM imaging of 47-pm-separated atomic columns by a spherical aberration-corrected electron microscope with a 300-kV cold field emission gun.

A spherical aberration-corrected electron microscope has been developed recently, which is equipped with a 300-kV cold field emission gun and an objective lens of a small chromatic aberration coefficient. A dumbbell image of 47 pm spacing, corresponding to a pair of atomic columns of germanium aligned along the [114] direction, is resolved in high-angle annular dark field (HAADF) scanning transmission electron microscopy (STEM) with a 0.4-eV energy spread of the electron beam.

Development of a multifunctional TEM specimen holder equipped with a piezodriving probe and a laser irradiation port.

The double-probe piezodriving specimen holder that was recently developed by some of the present authors is modified to introduce a laser irradiation port in one of its two arms. As a result, the new specimen holder consists of a piezodriving probe and a laser irradiation port, both of which can be three-dimensionally controlled by using piezoelectric elements and micrometers. While the piezodriving probe interacts with the specimen set in the holder in several ways, the laser beam causes photo-induced phenomena to occur.

Ultrahigh-vacuum third-order spherical aberration (Cs) corrector for a scanning transmission electron microscope.

Initial results from an ultrahigh-vacuum (UHV) third-order spherical aberration (Cs) corrector for a dedicated scanning transmission electron microscopy, installed at the National Institute for Materials Science, Tsukuba, Japan, are presented here. The Cs corrector is of the dual hexapole type. It is UHV compatible and was installed on a UHV column.

High-resolution ultrahigh-vacuum electron microscopy of helical gold nanowires: junction and thinning process.

Helical multishell (HMS) gold nanowires were observed in situ by ultra-high-vacuum electron microscopy. During thinning of the helical nanowire, a junction was formed between two nanowires of different diameter. The structure of the gold junction is proposed in comparison with the multiwall carbon nanotube.