Visualization of lithium ions by annular bright field imaging.

The detection of lithium ions is required for characterization of lithium ion batteries, since the movement of lithium ions in the battery is one of the key ways to improve the performance. Annular bright field (ABF) imaging enables us to visualize individual lithium atomic columns simultaneously with heavy elements. Furthermore, it has been found that the number of lithium ions at the column is countable when the specimen is thin.

Phase transitions in a LiMn2O4 nanowire battery observed by operando electron microscopy.

Fast charge-discharge process has been reported to give a high capacity loss. A nanobattery consisting of a single LiMn2O4 nanowire cathode, ionic liquid electrolyte and lithium titanium oxide anode was developed for in situ transmission electron microscopy. When it was fully charged or discharged within a range of 4 V in less than half an hour (corresponding average C rate: 2.

Development of an electrochemical cell for in situ transmission electron microscopy observation.

A new type of electrochemical cell was developed for in situ transmission electron microscopy observation that enables the electrode materials to be conveniently changed. The electrochemical cell was used to observe the electrochemical growth or dissolution of copper islands on a gold film with simultaneous cyclic voltammetry measurements. The copper islands could be explained by three-dimensional growing model.

Determination of aberration center of Ronchigram for automated aberration correctors in scanning transmission electron microscopy.

A generic method to determine the aberration center is established, which can be utilized for aberration calculation and axis alignment for aberration corrected electron microscopes. In this method, decentering induced secondary aberrations from inherent primary aberrations are minimized to find the appropriate axis center. The fitness function to find the optimal decentering vector for the axis was defined as a sum of decentering induced secondary aberrations with properly distributed weight values according to the aberration order.

Reversible contrast in focus series of annular bright field images of a crystalline LiMn₂O₄ nanowire.

A through-focus series of annular bright field (ABF) images were observed simultaneously with high-angle annular dark field (HAADF) images of very thin lithium manganese oxide (LiMn₂O₄), a typical cathode material used in lithium ion batteries, using a spherical aberration corrected electron microscope with a 50 pm resolution (R005). The ABF images showed dark dips at the positions of Li and Mn--O atomic columns, which reversed to bright peaks when the defocus sign was changed, as commonly observed in phase contrast images. The optimal defocus for the ABF images was about 2 nm of over-focus, while that for the HAADF images was 2 nm of under-focus for an incident probe with a convergent semi-angle of 30 mrad.

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.

Study on probe current dependence of the intensity distribution in annular dark field images.

The intensity profile of atomic columns in annular dark field (ADF) images was quantitatively investigated for a silicon (001) crystal using a cold field emission source in an aberration corrected scanning transmission electron microscope. The intensity distribution at the atomic column in the annular dark field image was blurred by increasing the probe current from 10 to 40 pA, which was quantitatively well fit by a simulated distribution convolved by Gaussian envelopes with area proportional to the probe current. The blur of the ADF images was primarily determined by the size of the cold field emission source.

Exceeding conventional resolution limits in high-resolution transmission electron microscopy using tilted illumination and exit-wave restoration.

Tilted illumination exit-wave restoration is compared for two aberration-corrected instruments at different accelerating voltages. The experimental progress of this technique is also reviewed and the significance of off-axial aberrations examined. Finally, the importance of higher order aberration compensation combined with careful correction of the lower order aberrations is highlighted.

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.

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.

Helical gold nanotube synthesized at 150 K.

Gold nanowires were synthesized at 150 K by electron beam thinning of a gold thin foil in an UHV electron microscope. The gold nanowires were found to have a helical multishell structure (HMS). One particular nanowire, which was thinner than the 7-1 HMS nanowire, was found to have a tubular structure.

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.