• Applied Microscopy
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• v.51
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• pp.19.1-19.7
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• 2021

The main purpose of this paper is the preparation of transmission electron microscopy (TEM) samples from the microsized powders of lithium-ion secondary batteries. To avoid artefacts during TEM sample preparation, the use of ion slicer milling for thinning and maintaining the intrinsic structure is described. Argon-ion milling techniques have been widely examined to make optimal specimens, thereby making TEM analysis more reliable. In the past few years, the correction of spherical aberration (Cs) in scanning transmission electron microscopy (STEM) has been developing rapidly, which results in direct observation at an atomic level resolution not only at a high acceleration voltage but also at a deaccelerated voltage. In particular, low-kV application has markedly increased, which requires a sufficiently transparent specimen without structural distortion during the sample preparation process. In this study, sample preparation for high-resolution STEM observation is accomplished, and investigations on the crystal integrity are carried out by Cs-corrected STEM.

• Journal of the Korean Ceramic Society
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• v.31 no.12
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• pp.1501-1506
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• 1994

The precipitate of FeCl2.4H2O and NaOH, Fe(OH)2 was rapidly made to oxidize by H2O2 to prepare $\delta$-FeOOH. The particle size, surface and morphology of $\delta$-FeOOH, and the shape and structure of thermally decomposed $\delta$-FeOOH were investigated by the use of high resolution STEM. $\delta$-FeOOH prepared under the condition of reaction temperature of Fe(OH)2 at 4$0^{\circ}C$, [OH-][Fe2+]=5 and aging time of 2 hr Fe(OH)2, had 630$\AA$ mean particle size, 4~5 aspect ratio, 20.8 emu/g saturation magnetization and 210 Oe coercivity. The edges of $\delta$-FeOOH were inclined to (001) about 41$^{\circ}$, 60$^{\circ}$ and coincident with (102), (101) respectively. When $\delta$-FeOOH was thermally decomposed at 25$0^{\circ}C$ for 2 hr in vacuo, which had micropores of 0.9 nm thickness and crystallites of 2.4 nm thickness. (001)hex, [10]hex. of $\delta$-FeOOH parallel with (001)hex, [100]hex. of $\alpha$-Fe2O3 respectively. This showed three dimensional topotaxial structure transition, which was investigated by SADP (Selected Area Diffraction Pattern) of STEM.

• Korean Journal of Materials Research
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• v.28 no.10
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• pp.595-600
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• 2018

This study investigates the microstructural properties of CoCrFeMnNi high entropy alloy (HEA) oxynitride thin film. The HEA oxynitride thin film is grown by the magnetron sputtering method using nitrogen and oxygen gases. The grown CoCrFeMnNi HEA film shows a microstructure with nanocrystalline regions of 5~20 nm in the amorphous region, which is confirmed by high-resolution transmission electron microscopy (HR-TEM). From the TEM electron diffraction pattern analysis crystal structure is determined to be a face centered cubic (FCC) structure with a lattice constant of 0.491 nm, which is larger than that of CoCrFeMnNi HEA. The HEA oxynitride film shows a single phase in which constituting elements are distributed homogeneously as confirmed by element mapping using a Cs-corrected scanning TEM (STEM). Mechanical properties of the CoCrFeMnNi HEA oxynitride thin film are addressed by a nano indentation method, and a hardness of 8.13 GPa and a Young's modulus of 157.3 GPa are obtained. The observed high hardness value is thought to be the result of hardening due to the nanocrystalline microstructure.