Bright-field Scanning Transmission Electron Microscopy Research Articles

A P2/P3 Biphasic Layered Oxide Composite as a High-Energy and Long-Cycle-Life Cathode for Potassium-Ion Batteries.

Layered transition metal oxides are extensively considered as appealing cathode candidates for potassium-ion batteries (PIBs) due to their abundant raw materials and low cost, but their further implementations are limited by slow dynamics and impoverished structural stability. Herein, a layered composite having a P2 and P3 symbiotic structure is designed and synthesized to realize PIBs with large energy density and long-term cycling stability. The unique intergrowth of P2 and P3 phases in the obtained layered oxide is plainly characterized by X-ray diffraction refinement, high-angle annular dark field and annular bright field-scanning transmission electron microscopy at atomic resolution, and Fourier transformation images. The synergistic effect of the two phases of this layered P2/P3 composite is well demonstrated in K+ intercalation/extraction process. The as-prepared layered composite can present a large discharge capacity with the remarkable energy density of 321 Wh kg-1 and also manifest excellent capacity preservation after 600 cycles of K+ uptake/removal.

Experimental determination of critical thickness limitations of (010) β -(AlxGa1−x)2O3 heteroepitaxial films

The effect of heteroepitaxial β-(AlxGa1−x)2O3 film thickness and Al content on surface morphology was characterized to experimentally determine the critical thickness limitations of the (010) β-(AlxGa1−x)2O3/Ga2O3 heterostructure. High-resolution x-ray diffraction was used to assess the strain state of the films; reciprocal space mapping (RSM) revealed that even cracked films were still fully strained. In cracked films, diffuse scattering was observed in RSMs, indicating lattice tilting. Cracking of the films was investigated using atomic force microscopy (AFM), x-ray topography (XRT), bright-field scanning transmission electron microscopy (BF-STEM), and high-resolution transmission electron microscopy. Using both AFM and XRT, the [001] direction was observed to be the most prevalent crack direction; however, cracks were also observed in the [100] direction. In uncracked regions of the films, XRT revealed the alignment of threading dislocations along the [001] direction. Cross-sectional imaging of the crack geometry and propagation was performed using BF-STEM, and it was observed that the cracks in the [001] direction extended through the thickness of the β-(AlxGa1−x)2O3 film (∼205 nm) and a further ∼100–200 nm into the β-Ga2O3 substrate. Experimental data for critical film thickness showed good agreement with previous theoretical calculations based on the Griffith criterion for crack propagation.

Direct imaging of local atomic structures in zeolite using optimum bright-field scanning transmission electron microscopy.

Zeolites are used in industries as catalysts, ion exchangers, and molecular sieves because of their unique porous atomic structures. However, direct observation of zeolitic local atomic structures via electron microscopy is difficult owing to low electron irradiation resistance. Subsequently, their fundamental structure-property relationships remain unclear. A low-electron-dose imaging technique, optimum bright-field scanning transmission electron microscopy (OBF STEM), has recently been developed. It reconstructs images with a high signal-to-noise ratio and a dose efficiency approximately two orders of magnitude higher than that of conventional methods. Here, we performed low-dose atomic-resolution OBF STEM observations of two types of zeolite, effectively visualizing all atomic sites in their frameworks. In addition, we visualized the complex local atomic structure of the twin boundaries in a faujasite (FAU)-type zeolite and Na+ ions with low occupancy in eight-membered rings in a Na-Linde Type A (LTA) zeolite. The results of this study facilitate the characterization of local atomic structures in many electron beam-sensitive materials.

Decoding the Atomic-Scale Structural Origin of Large Strain Performance in BNT-6BT Based Relaxor Ferroelectrics.

The relationship between matter properties and their atomic-scale structures is a challenging investigation. For relaxor ferroelectrics, correlating the relaxor mechanisms on the atomic scale to properties is still ambiguous. Here, the correlation between the atomic-scale structure and strain performance of 0.94 Bi0.5Na0.5TiO3-0.06BaTiO3 (94BNT-6BT) and 0.93 Bi0.5Na0.5TiO3-0.06BaTiO3-0.01BaZrO3 (93BNT-6BT-1BZ) is reported. The δTi-Bi/Na displacement vector map based on the annular dark field (ADF) scanning transmission electron microscopy (STEM) image demonstrates the coexistence of tetragonal (T) and rhombohedral (R) phases of the resulting ceramics, and BZ doping increases the proportion of the T phase. Furthermore, the enhanced annular bright field (eABF) STEM image demonstrates that BZ doped ceramics exhibit obvious oxygen octahedral tilt. The oxygen octahedral tilt increased gradually from the domain wall to the inner place of the nanodomain, indicating a regional consistency, which results in enhancement of the relaxor performance and stain property. This study opens exciting opportunities to the design of relaxor ferroelectrics with large strain for high-displacement actuator applications.

PEI-Schiff base-modified mesoporous silica materials SBA-12, 15 and 16 for toxic metal ions capture (Co(II), Ni(II) and Cu(II)): Effect of morphology, post-synthetic modification and kinetic study

A series of SBA materials (SBA-12, SBA-15, and SBA-16) with polyethyleneimine (PEI) and its Schiff base variants with salicylaldehyde-modified samples (PS) have been successfully prepared and characterized. The synthesized materials were investigated by infrared spectroscopy (FT-IR), and quantification of the organic part coated on the surface was studied using thermogravimetric analysis (TGA). Nitrogen adsorption/desorption analysis at − 196 °C (N2), bright field scanning transmission electron microscopy (BF-STEM) and small angle X-ray scattering (SAXS) measurements were used to study textural properties, structure and morphology. Confirmation of heavy metal ions capture in pores of prepared materials was proved by X-ray fluorescence analysis (XRF), and nitrate anions were confirmed by FT-IR spectroscopy. Kinetic studies were performed by conductometric analysis (CA) and showed that the mathematical models could be applied to adsorption processes with a non-linear decreasing trend. This trend appeared in PS-modified SBA systems and some non-modified samples. The best overall adsorption properties were observed for material SBA-12 and its modified types. In this case, material SBA-12-PS can trap 54.38 mg g−1 of Cu(NO3)2 or 18.42 mg of Cu(II) ions, 112.84 mg g−1 of Ni(NO3)2 corresponding to 36.24 mg of Ni(II) cations, and 39.56 mg g−1 of Co(NO3)2 representing 12.74 mg of Co(II) ions. Non-modified materials show morphological effects where 2D ordered pores with hexagonal symmetry and the biggest mesopores (5.5 nm) have the best overall results in adsorption capacity of metal ions (Cu(II): 11.95 mg g−1) calculated from pseudo-second order. SBA-12 with a cubic framework and 3D ordered pores (3.8 nm) has a lower adsorption capacity than SBA-15 (Cu(II): 7.85 mg g−1), and SBA-16 with the smallest spherical pores (under 2 nm) showed the lowest overall adsorption capacity (Cu(II): 4.65 mg g−1). Kinetic rates of non-modified samples have opposite trend SBA-12 (Cu(II): 0.009 mg g−1 min−1) > SBA-15 (Cu(II): 0.002 mg g−1 min−1) > SBA-16 (Cu(II): 0.001 mg g−1 min−1). In the case of SBA-16, small pore entrances have a negative effect on the kinetic rate. For modified samples, SBA-12 with the largest surface area (896 m2 g−1) provides more space for binding of polyethyleneimine molecules (and also salicylaldehyde), which affects the best results in ion capture (Cu(II): 16.64 mg g−1). Bigger mesopores give more adsorption capacity, but capillarity makes the kinetic rate slow. SBA-16, with tiny entrance mesopores, has the lowest kinetic rate and adsorption capacity. This phenomenon was also observed in cobalt(II) adsorption, and similar results were obtained in nickel(II) adsorption. Kinetic studies point to two types of mechanisms given by the pseudo-second-order model in the case of non-modified materials, and Elovich kinetic model describes chemisorption at modified samples. These mechanisms are influenced by the significant effect of intraparticle diffusion, described by the Weber-Morris model.

Low-energy scanning transmission electron microscopy applied to ice-embedded biological macromolecules.

In this report, we applied annular bright-field and annular dark-field low-energy (30 keV) scanning transmission electron microscopy imaging to a vitreous ice-embedded biological macromolecule, T4 phage, to investigate the applicability of these methods for morphological investigation and sample screening. Multiple camera lengths were examined to find the optimal acceptance angle for both modes. Image clarity differed substantially between the modes, with the presence of ice also strongly influencing the quality of acquired micrographs. In annular dark-field mode, the proper discrimination of electrons scattered by the specimen from those scattered by the background ice was found to be difficult due to the severe overlap of the scattered electrons. The resulting micrographs lacked clarity, and the ice-embedded phage particles could only be discerned after post-processing image adjustment. However, in annular bright-field mode, despite similar overlapping of the scattered electrons, it was possible to assess the morphology and intactness of the specimen in the embedding ice, suggesting that this mode may find utility in low-energy cryo-scanning transmission electron microscopy imaging methods.

Large (anti)ferrodistortive NaNbO3-based lead-free relaxors: Polar nanoregions embedded in ordered oxygen octahedral tilt matrix

Relaxor ferroelectric perovskites have experienced a revival of interest in recent years accompanying the deeply exploration of the fine local structure of polar nanoregions, which are thought to be the structure root for unique electrical properties. Interestingly, a new type of low-tolerance relaxor ferroelectric, which exhibits both cation displacement and large oxygen octahedral tilt, exhibiting anomalous microdomains were found in NaNbO3-based lead-free perovskites, breaking through the limits of the relaxor ferroelectric models proposed from classical relaxors. Atomic-scale annular bright-field scanning transmission electron microscopy images indicate that the microdomains are formed by long-range ordered oxygen octahedral tilt. At the same time, substructure of randomly embedded nanoregions with inhomogeneous polarization vectors can be mapped, being the main reason for relaxor behavior. Based on this special ferroelectric-improper ferroelastic state, delayed polarization saturation can be obtained under strong electric field, providing an opportunity for generating excellent energy storage properties. The results found in this work not only open up a new kind of relaxor ferroelectrics but also will lead to the reconstruction of relaxor models and theories built for more than half a century.

Automated calculations for computing the sample-limited spatial resolution in (scanning) transmission electron microscopy

MATLAB scripts were designed to compute the sample-limited spatial resolution in transmission electron microscopy (TEM) and scanning TEM (STEM) as a function of different microscopy parameters including the electron dose eD, sample geometry, and materials parameters. The scripts can be used to select the optimum microscopy modality and optimize the experimental conditions to achieve the best possible resolution considering the limitations set by both the electron optics and the examined sample. The resolution can be computed as function of the objective opening semi-angle α for TEM and detector opening semi-angle β for STEM. Optional code for computing a range over the sample thickness t or eD are provided as well, whereby the opening angle is optimized for each data point. The spatial resolution depends on the type of material of the nanoscale object (for example, gold or carbon nanoparticles), the type of matrix holding the objects (for example, water or ice), the depth of the nanoscale object inside the matrix, and eD. The optimization is consistent with the typical situation that carbon nanoparticles are best examined with TEM embedded in a thin matrix (t = 0.1 µm), while STEM is better suited for high atomic number objects such as gold nanoparticles in water, irrespective of t. The script also calculates the reduction of beam broadening in thick samples (t > 1 µm) using bright field STEM.

Strategy for optimizing experimental settings for studying low atomic number colloidal assemblies using liquid phase scanning transmission electron microscopy

Observing processes of nanoscale materials of low atomic number is possible using liquid phase electron microscopy (LP-EM). However, the achievable spatial resolution (d) is limited by radiation damage. Here, we examine a strategy for optimizing LP-EM experiments based on an analytical model and experimental measurements, and develop a method for quantifying image quality at ultra low electron dose De using scanning transmission electron microscopy (STEM). As experimental test case we study the formation of a colloidal binary system containing 30 nm diameter SiO2 nanoparticles (SiONPs), and 100 nm diameter polystyrene microspheres (PMs). We show that annular dark field (DF) STEM is preferred over bright field (BF) STEM for practical reasons. Precise knowledge of the material's density is crucial for the calculations in order to match experimental data. To calculate the detectability of nano-objects in an image, the Rose criterion for single pixels is expanded to a model of the signal to noise ratio obtained for multiple pixels spanning the image of an object. Using optimized settings, it is possible to visualize the radiation-sensitive, hierarchical low-Z binary structures, and identify both components.

Atomic-scale mapper for superlattice photodetectors analysis.

In this work, a new Python-based tool for atomic-scale mapping of high-angle annular dark-field (HAADF) and annular bright-field (ABF) scanning transmission electron microscopy (STEM) images using the Z-contrast method is introduced, aimed to help in the analysis of superlattice layers' composition, and in the determination of material of interfaces. The operation principle of the program, as well as specific examples of use, are explained in many details. Good customization flexibility using the user-friendly graphical user interface (GUI), allows the processing of a wide range of images, demonstrating a decent accuracy of coordinates extraction and performance.

Elevated barrier height originated from electric dipole effect and improved breakdown characteristics in PtOx/β-Ga2O3 Schottky barrier diodes

The higher Schottky barrier height of PtOx/β-Ga2O3 Schottky barrier diode (SBD) was derived from the electric dipole effect of PtOx Schottky electrode. And the higher Schottky barrier height effectively improved the reverse breakdown characteristics of β-Ga2O3 SBD. In this work, PtOx/β-Ga2O3 and Pt/β-Ga2O3 SBDs were fabricated, and the Schottky barrier height of PtOx SBD increased with the increment of oxygen element component in PtOx electrode, which were all higher than the Schottky barrier height of Pt SBD. Kelvin probe force microscope measurement indicated that Fermi level pinning effect and the variation in work functions of Schottky electrodes were irrelevant to the higher barrier height. Moreover, with the increment of inserting PtOx layer thickness in Pt/PtOx/β-Ga2O3 SBDs, the Schottky barrier height increased from 1.32 eV to 1.82 eV. Bright-field scanning transmission electron microscopy image demonstrated that PtOx was mainly polycrystal with layer structure near the Schottky interface. The layer structure composed of Pt ions and O ions induced electric dipole effect, and the electric dipole effect led to the increase of Schottky barrier height for PtOx SBD. Lower leakage current density, higher breakdown voltages and more concentrated breakdown voltage distribution were obtained for PtOx SBDs. Furthermore, the barrier heights of PtOx SBDs gradually increased as the temperature raised, resulting in their reverse leakage current increased much more slowly with temperature than that of Pt SBD. The above results demonstrated that PtOx/β-Ga2O3 SBD had great potential in enhancing reverse blocking characteristics and high-temperature environment applications.

Comparison of ion irradiation effects in PM-HIP and forged alloy 625

The nuclear industry has growing interest in replacing forgings with structural components fabricated by powder metallurgy with hot isostatic pressing (PM-HIP), owing to their chemical homogeneity, uniform grain structure, and near-net shape production. This study compares the ion irradiation response of PM-HIP and forged Alloy 625, over 50 and 100 dpa, 400 °C and 500 °C. Microstructure is characterized using down-zone bright-field scanning transmission electron microscopy (DZBFSTEM), and hardening is characterized using nanoindentation. PM-HIP Alloy 625 has a lower initial dislocation line density, resulting in a more rapid onset of dislocation loop growth and unfaulting than the forged material. But the total defect population (i.e. loop line length plus dislocation density) is insensitive to fabrication method. This finding shows promise for the eventual qualification of PM-HIP alloys for nuclear applications.

Coupled Compositional and Displacive Modulations in KLaMnWO6 Revealed by Atomic Resolution Imaging.

Complex compositional and displacive modulations of the crystal structure of KLaMnWO6 are imaged with atomic resolution by means of scanning transmission electron microscopy (STEM). This oxide is stabilized by cation vacancies leading to a La1+x/3K1-xMnWO6 stoichiometry. Compositional modulation on both the K and La layers are revealed in the high-angle annular dark-field STEM (HAADF-STEM) images. The compositional modulation within the La layer is coupled with the modulation of the octahedral tilting, which is exposed by imaging of the anion sublattice in annular bright-field STEM (ABF-STEM) images. These complex modulations are accommodated in a 5√2ap × 5√2ap × 2ap perovskite-type structure.

In Situ Resolving the Atomic Reconstruction of SnO2 (110) Surface.

Understanding surface reconstruction of nanocrystals is of great importance to their applications, however it is still challenging due to lack of atomic-level structural information under reconstruction conditions. Herein, through in situ spherical aberration corrected scanning transmission electron microscopy (STEM), the reconstruction of nanocrystalline SnO2 (110) surface was studied. By identifying the precise arrangements of surface/subsurface Sn and O columns through both in situ bright-field and high-angle annular dark-field STEM images, an unexpected added Sn2O model was determined for SnO2 (110)-(1 × 2) surface. The protruded Snδ+ of this surface could act as the active sites for activating O2 molecules according to our density functional theory (DFT) calculations. On the basis of in situ observation of atomic-level reconstruction behaviors and DFT calculations, an energy-driven reconstruction process was also revealed. We anticipate this work would help to clarify the long-standing debate regarding the reconstruction of SnO2 (110) surface and its intrinsic property.

Determination of Dy substitution site in Nd2\u2212xDyxFe14B by HAADF-STEM and illustration of magnetic anisotropy of \u201cg\u201d and \u201cf\u201d sites, before and after substitution

Nd2Fe14B and Nd2−xDyxFe14B (x = 0.25, 0.50) particles were prepared by the modified co-precipitation followed by reduction–diffusion process. Bright field scanning transmission electron microscope (BF-STEM) image revealed the formation of Nd–Fe–B trigonal prisms in [− 101] viewing zone axis, confirming the formation of Nd2Fe14B/Nd2−xDyxFe14B. Accurate site for the Dy substitution in Nd2Fe14B crystal structure was determined as “f” site by using high-angle annular dark field scanning transmission electron microscope (HAADF-STEM). It was found that all the “g” sites are occupied by the Nd, meanwhile Dy occupied only the “f” site. Anti-ferromagnetic coupling at “f” site decreased the magnetic moment values for Nd1.75Dy0.25Fe14B (23.48 μB) and Nd1.5Dy0.5Fe14B (21.03 μB) as compared to Nd2Fe14B (25.50 μB). Reduction of magnetic moment increased the squareness ratio, coercivity and energy product. Analysis of magnetic anisotropy at constant magnetic field confirmed that “f” site substitution did not change the patterns of the anisotropy. Furthermore, magnetic moment of Nd2Fe14B, Nd2−xDyxFe14B, Nd (“f” site), Nd (“g” site) and Dy (“f” site) was recorded for all angles between 0° and 180°.

Robust Ruthenium Catalysts Supported on Mesoporous Cyclodextrin-Templated TiO2-SiO2 Mixed Oxides for the Hydrogenation of Levulinic Acid to γ-Valerolactone.

In this paper, we present a versatile template-directed colloidal self-assembly method for the fabrication in aqueous phase of composition-tuned mesoporous RuO2@TiO2-SiO2 catalysts. Randomly methylated β-cyclodextrin/Pluronic F127 supramolecular assemblies were used as soft templates, TiO2 colloids as building blocks, and tetraethyl orthosilicate as a silica source. Catalysts were characterized at different stages of their synthesis using dynamic light scattering, N2-adsorption analysis, powder X-ray diffraction, temperature programmed reduction, high-resolution transmission electron microscopy, high-angle annular bright-field and dark-field scanning transmission electron microscopy, together with EDS elemental mapping. Results revealed that both the supramolecular template and the silica loading had a strong impact on the pore characteristics and crystalline structure of the mixed oxides, as well as on the morphology of the RuO2 nanocrystals. Their catalytic performance was then evaluated in the aqueous phase hydrogenation of levulinic acid (LA) to γ-valerolactone (GVL) under mild conditions (50 °C, 50 bar H2). Results showed that the cyclodextrin-derived catalyst displayed almost quantitative LA conversion and 99% GVL yield in less than one hour. Moreover, this catalyst could be reused at least five times without loss of activity. This work offers an effective approach to the utilization of cyclodextrins for engineering the surface morphology of Ru nanocrystals and pore characteristics of TiO2-based materials for catalytic applications in hydrogenation reactions.

Epitaxy from a Periodic Y–O Monolayer: Growth of Single-Crystal Hexagonal YAlO3 Perovskite

The role of an atomic-layer thick periodic Y–O array in inducing the epitaxial growth of single-crystal hexagonal YAlO3 perovskite (H-YAP) films was studied using high-angle annular dark-field and annular bright-field scanning transmission electron microscopy in conjunction with a spherical aberration-corrected probe and in situ reflection high-energy electron diffraction. We observed the Y–O array at the interface of amorphous atomic layer deposition (ALD) sub-nano-laminated (snl) Al2O3/Y2O3 multilayers and GaAs(111)A, with the first film deposition being three cycles of ALD-Y2O3. This thin array was a seed layer for growing the H-YAP from the ALD snl multilayers with 900 °C rapid thermal annealing (RTA). The annealed film only contained H-YAP with an excellent crystallinity and an atomically sharp interface with the substrate. The initial Y–O array became the bottom layer of H-YAP, bonding with Ga, the top layer of GaAs. Using a similar ALD snl multilayer, but with the first film deposition of three ALD-Al2O3 cycles, there was no observation of a periodic atomic array at the interface. RTA of the sample to 900 °C resulted in a non-uniform film, mixing amorphous regions and island-like H-YAP domains. The results indicate that the epitaxial H-YAP was induced from the atomic-layer thick periodic Y–O array, rather than from GaAs(111)A.

Triangular Single Shockley Stacking Fault Analyses on 4H-SiC PiN Diode with Forward Voltage Degradation

The structure of partial dislocations (PDs), which surround triangular single Shockley stacking faults (1SSFs) expanded during electroluminescence observation in a 4H-SiC PiN diode, is investigated by photoluminescence (PL) imaging, PL spectroscopy, plan-view transmission electron microscopy (TEM) imaging, g·b analysis, cross-sectional bright-field scanning TEM (BF-STEM) imaging, and high-resolution high-angle annular dark-field (HAADF)-STEM imaging. The zigzag configuration is found on the upstanding side of the triangular 1SSF by plan-view TEM imaging, while it is observed as a single line by PL imaging. Using g·b analysis, the zigzag line is confirmed to be constructed by 30° and 90° PDs. Cross-sectional BF-STEM observation proved that the expanding 1SSF penetrates through the p–n interface whose position was estimated from secondary-ion mass spectrometry (SIMS) depth profile measurements of the aluminum and nitrogen concentrations. This provides experimental evidence that the 1SSF loses its driving force for recombination-enhanced dislocation glide when it stops somewhere in the p-layer where sufficient electrons no longer exist. Using cross-sectional HAADF-STEM observation, core species of the PDs were analyzed and the Burgers vector for the dislocation loop uniquely determined. Also, the first experimental observation of a 90° silicon-core PD, reported so far, is confirmed. According to these PD analyses, the possible atomic arrangement around the 1SSF is examined and the way tetrahedrons face across each PD is summarized, based on HAADF-STEM analysis of the 1SSF line.

Imaging of polymer:fullerene bulk-heterojunctions in a scanning electron microscope: methodology aspects and nanomorphology by correlative SEM and STEM

Scanning transmission electron microscopy (STEM) at low energies (≤ 30 keV) in a scanning electron microscope is well suited to distinguish weakly scattering materials with similar materials properties and analyze their microstructure. The capabilities of the technique are illustrated in this work to resolve material domains in PTB7:PC71BM bulk-heterojunctions, which are commonly implemented for light-harvesting in organic solar cells. Bright-field (BF-) and high-angle annular dark-field (HAADF-) STEM contrast of pure PTB7 and PC71BM was first systematically analyzed using a wedge-shaped sample with well-known thickness profile. Monte-Carlo simulations are essential for the assignment of material contrast for materials with only slightly different scattering properties. Different scattering cross-sections were tested in Monte-Carlo simulations with screened Rutherford scattering cross-sections yielding best agreement with the experimental data. The STEM intensity also depends on the local specimen thickness, which can be dealt with by correlative STEM and scanning electron microscopy (SEM) imaging of the same specimen region yielding additional topography information. Correlative STEM/SEM was applied to determine the size of donor (PTB7) and acceptor (PC71BM) domains in PTB7:PC71BM absorber layers that were deposited from solution with different contents of the processing additive 1,8-diiodooctane (DIO).

Transition Metals Ion Behavior of Cathode Materials for Li Ion Battery By Electron Beam Irradiation in Scanning Transmission Electron Microscopy

Investigating the structural properties of Li-ion batteries (LIBs) and, if possible, determining the overall structure is important in understanding the physical and chemical properties. Understanding the structural properties and the electrochemical properties of the arranged atoms of cathode materials is therefore essential for new battery material design and system optimization. Particularly, cathode materials such as LiNixMnyCo1-x-yO2 (NMC), lithium-rich Li(LiyNix-yMnxCo1-2x)O2, lithium-rich / manganese-rich xLi2MnO3 (1-x)LiMO2 are analyzed by the scanning transmission electron microscopy (STEM) techniques to identify structural characteristics, leading to the conversion of the layer structure to the spinel and/or salt structure, leading to increased impedance, voltage reduction and capacity of the LIBs. The atomic behavior of Li ion in the cathode materials that determines LiBs performance is hardly characterized by transmission electron microscopy (TEM) owing to its weak electron-scattering power. In this sense, annular bright-field (ABF) STEM, in which the contrast has a low scaling rate with the atomic number, has been proven to be a robust technique for simultaneous imaging of light and heavy elements. However, it is very important to understand the damage mechanism of cathode materials by electron-beam irradiation in STEM and to develop this technique. In this study, we investigated the effect of electron-beam irradiation damage on the surface reaction layer and LiNi0.6Co0.2Mn0.2O2 material during STEM data acquisition. This electron-beam irradiation damage process is similar to the lattice reconstruction and chemical evolution caused by the charge-discharge cycle. Furthermore, based on the phase transition phenomenon by the electron-beam irradiation, it is examined whether the electron beam irradiation damage in the lattice structure substituted by Al and Ti affects the phase transition phenomenon.