Surface Reaction Layer Research Articles

Effect on albumin and fibronectin adsorption of silver doping via ionic exchange of a silica-based bioactive glass

Protein adsorption is a crucial step in the life of biomaterials for bone application, such as bioactive glasses. The investigation of adsorption mechanisms is a difficult task per se, which is even more complex on bioactive glasses due to surface reactivity. Here, the effect of silver doping by ionic exchange on the interaction of a silica-based bioactive glass with albumin and fibronectin, serum proteins related to osseointegration, is reported. The presence of silver does not change relevant surface properties such as topography, surface energy, wettability, or surface ζ potential. Nevertheless, the interactions with proteins are much different. The presence of silver significantly increases the adsorption of albumin and fibronectin and leads to a higher loss of secondary structure compared to the undoped surface, as a consequence of the interactions and bonding between silver and thiols in the cysteine residues. Selectivity of silver-doped glass is discovered: Ag enhances more adsorption and denaturation of albumin since it has more cysteines than fibronectin. It is also here observed that due to the formation of a hydrated silica gel layer during adsorption, proteins are not only present on the surface of the bioactive glasses, but also embedded inside the surface reaction layer.

Effect of yttrium on intergranular embrittlement behavior of GH3535 alloy induced by tellurium

The influence of yttrium (Y) addition on the tellurium (Te) induced intergranular embrittlement of Ni-16Mo-7Cr alloy was investigated. The results show that the addition of Y remarkedly reduces the diffusion depth of Te into the alloy, and thus improves the intergranular cracking resistance of the alloy. The YTe phases on the surface reaction layer and near-surface grain boundaries, plays an important role in fixing Te and slowing down the Te diffusion. Adding more than 0.05 wt% Y into the alloy does not continuously improve the intergranular embrittlement resistance, and even damages the mechanical properties.

Tapered Cross Section Photoelectron Spectroscopy Provides Insights into the Buried Interfaces of III‐V Semiconductor Devices

AbstractInterfaces are key elements that define electronic properties of the final device. Inevitably, most of the active interfaces of III–V semiconductor devices are buried and it is therefore not straightforward to characterize them. The Tapered Cross Section Photoelectron Spectroscopy (TCS‐PES) approach is promising to address such a challenge. That the TCS‐PES can be used to study the relevant heterojunction in epitaxial III–V architectures prepared by metalorganic chemical vapor deposition is demonstrated here. A MULTIPREP polishing system that enables controlling the angle between the sample holder and the polishing plate has been employed to improve the reproducibility of the polishing procedure. With this procedure, that preparing the TCS of III–V semiconductor devices with tapering angles lower than 0.02° is possible is demonstrated. The PES provides then information about the buried interfaces of Ge|GaInP and GaAs|GaInP layer stacks. Both, chemical and electronic properties have been measured by PES. It evidences that the preparation of the TCSs under an uncontrolled atmosphere modifies the pristine properties of the critical buried heterointerfaces. Surface states and reaction layers are created on the TCS surface, which restrict unambiguous conclusions on buried interface energetics.

Effect of temperature, oxygen partial pressure and calcium lignosulphonate on chalcopyrite dissolution in sulfuric acid solution

The pressure leaching mechanism of chalcopyrite was studied by both leaching tests and in-situ electrochemical measurements. The effects of leaching temperature, oxygen partial pressure, and calcium lignosulphonate, on copper extraction and iron extraction of chalcopyrite pressure leaching were investigated. The leaching rate is accelerated by increasing the leaching temperature from 120 to 150 °C and increasing oxygen partial pressure to 0.7 MPa. The release of iron is faster than that of copper due to the formation of iron-depleted sulfides. Under the optimal leaching conditions without calcium lignosulphonate, the copper and iron extraction rates are 79% and 81%, respectively. The leaching process is mixedly controlled by surface reaction and product layer diffusion with an activation energy of 36.61 kJ/mol. Calcium lignosulphonate can effectively remove the sulfur passive layer, and the activation energy is 45.59 kJ/mol, suggesting that the leaching process with calcium lignosulphonate is controlled by surface chemical reactions. Elemental sulfur is the main leaching product, which is mixed with iron-depleted sulfides and leads to the passivation of chalcopyrite. Electrochemical studies suggest that increasing the oxygen partial pressure leads to increasing the cathodic reaction rate and weakening the passivation of chalcopyrite.

Structural and elemental characterization of glass and ceramic particles for bone surgery

ObjectiveClinically used bioceramics have been characterized previously with different kinds of methods and comparison of results have proven to be difficult due to varieties of the material properties of interest. Therefore, in this study we compared clinically commonly used bioceramics of hydroxyapatite and carbonate apatite, two bioactive glasses 45S5 and S53P4, and alumina with respect of properties which according to the present knowledge are significant for bone biology. MethodsPhysicochemical properties of the materials were characterized by various methods. Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) was used to analyze the material vibrational features. X-ray Power Diffraction (XRD) was used to characterize the material crystal structure and scanning electron microscopy-energy-dispersive x-ray analysis (SEM-EDXA) was used to evaluate the morphology and size of the materials and to calculate their oxide content. The dissolution behavior of the materials, ion release and pH changes in Tris buffer in a continuous flow-through reaction for 24-hours were determined. The change of the surface of the bioactive glasses by interfacial reaction during the Tris immersion was examined and the thickness of the surface reaction layer of the materials was studied. ResultsSEM examination showed that the particle morphology of BG 45S5, BG S53P4 and alumina particle’s surface was smooth. The surface of HAP was porous, but also CAP showed some surface porosity. An increase in the pH of the immersion solution was observed especially for BG 45S5 and BG S53P4. HAP, CAP and alumina caused only a minor increase in pH. BGs 45S5 and S53P4 showed a rapid initial release of sodium and calcium ions, followed by the release of silicon species. Minor release of sodium ions was registered for HAP, CAP and alumina. Calcium ion release was low but constant over the experimental time while only a minor initial dissolution was measured for HAP. SignificanceThe in vitro study showed differences in the materials’ properties, which are considered to be important for biological suitability and in clinical applications, such as materials tomography, ion release and pH changes.

Selective atomic layer reaction between GaN and SiN in HBr neutral beam etching

We investigated higher selective etching between SiN and GaN using an HBr neutral beam (NB) and found that it exhibited a more selective reaction compared to Cl2 NB. The etching rate of GaN mainly depended on the desorption rate of the etching product (GaClx or GaBrx) assisted by the bombardment of NB. As a result, in the case of the HBr neutral beam, the GaN etching rate was drastically decreased at the atomic layer level because the vapor pressure of the etching product, GaBrx, was much lower than that of GaClx. On the other hand, the dominant etching progression of SiN was mainly caused by neutral beam bombardment energy, and the desorption of the etching products (SiClx or SiBrx) was almost the same in both cases because the vapor pressures of the etching product, SiClx and SiBrx. In particular, in the case of the HBr neutral beam, the neutral beam energy dependence of the surface reaction layer of SiN was larger than that of Cl2 NB. As a result, the etching selectivity between SiN and GaN in HBr NB improved to 2.1 at 10 W of bias power, whereas that with Cl2 NB was saturated at 0.41 at more than 10 W of bias power. We found that the surface atomic layer etching reaction could precisely control the desorption rate of the etching product by optimizing the neutral beam bombardment energy and gas chemistry. The HBr neutral beam process can achieve atomic layer level selective reactions on the SiN/GaN structure.

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.

Thermal oxidation of PEPA-terminated polyimide

The thermal oxidative stability of a 4-phenylethynyl phthalic anhydride (PEPA) endcapped polyimide (PI) was investigated. A surface reaction layer formed due to oxidization during thermal aging and grew in thickness with increasing aging time. Analysis of the surface layer revealed a partial loss of aromatic ring, ether linkage, and imide linkage in the aged polymer. The partial loss of the imide linkage and ether linkage in the surface layer was corroborated by the observed release of carbon monoxide and carbon dioxide reaction products. The oxidized layer exhibited discoloration and an increase in glass transition temperature. The surface discoloration was attributed to the formation of the conjugated unsaturated or aromatic carbonyl groups and/or the charge transfer complex. Interior regions of the oxidized samples were largely unaffected, except for a more compact molecular configuration. Compared with aging at high temperatures (288°C, 316°C), aging at 204°C produced similar chemical changes in the cured polymer, albeit with a low degradation rate. The oxidative stability of the imide polymer surpassed that of conventional nadic-endcapped PIs due to the greater intrinsic thermal stability of the PEPA endcap. The unusual oxidative stability of the PI, combined with superior mechanical properties, warrant consideration as a composite matrix for future applications in high-temperature service conditions.

Thermochemical calculations of the oxidation behavior of Nb2AlC MAX phase in ZrO2–matrix composites

The oxidation behavior of Y-TZP/Nb2AlC composite was explored by thermo-chemical phase equilibrium calculations and experimental oxidation studies at 1200 °C. Growth of a compact surface reaction layer requires migration of oxygen from the surface to the reaction front and a gradient of oxygen content is likely to develop. The results of phase equilibria calculations show that at low oxygen concentration preferential oxidation of Al favors thermal degradation of Nb2AlC which yields Al2O3 and Nb-carbides. With increasing oxygen content various Nb-oxides are formed and finally a mixture of NbAlO4 and Nb2O5 is present after full oxidation of a Nb2AlC particle. Experimental measurements confirmed the formation of a compact oxidation reaction layer at 1200 °C composed mainly of NbAlO4 and a co-doped (Nb,Y)-TZP matrix.

The effect of wall flow velocity on compatibility of high-purity SiC materials with liquid Pb-Li alloy by rotating disc testing for 3000 h up to 900 °C

The lead-lithium (Pb-Li) alloy is considered as a coolant and a tritium breeder for fusion reactor blanket systems. One of the critical requirements in realization of the systems is the compatibility of silicon carbide (SiC) and its composites, as structural and/or functional materials of the blanket, with liquid Pb-Li flow at high temperatures. This study aims to clarify the corrosion process of high-purity SiC materials under flow condition of liquid Pb-Li for 3000 h at 700 and 900 °C, respectively, by using the rotating disc corrosion equipment. Furthermore, the effect of wall flow velocity on the compatibility was specifically evaluated. For that purpose the decrease rate (about 32–37%) of the wall flow velocity on disc type’s sample by the dragging effect by fluidic viscosity was first calculated by numerical analysis of the rotating flow condition. The wall flow velocity dependence on the reaction layer’s thickness was then evaluated for both high purity SiC and SiC/SiC composites. The test results show that the formation process of the surface reaction layer mainly depends on both the time required for the chemical reaction and the wall flow velocity in the initial stage but the reaction layer thickness tended to approach to the constant regardless of the wall flow velocity with increasing exposed time. In short, no accelerated corrosion was found for about 3000 h. It was also found that there was no significant difference of the temperatures between 700 and 900 °C. Finally the key corrosion mechanism, i.e., the reaction of oxide impurities, e.g., Li2O, in liquid Pb-Li with the Si-oxide layer over SiC, was identified.

Corrosion Behavior of Pipeline Carbon Steel under Different Iron Oxide Deposits in the District Heating System

The corrosion behavior of pipeline steel covered by iron oxides (α-FeOOH; Fe3O4 and Fe2O3) was investigated in simulated district heating water. In potentiodynamic polarization tests; the corrosion rate of pipeline steel is increased under the iron oxide but the increaseing rate is different due to the differnet chemical reactions of the covered iron oxides. Pitting corrosion was only observed on the α-FeOOH-covered specimen; which is caused by the crevice corrosion under the α-FeOOH. From Mott-Schottky and X-ray diffraction results; the surface reaction and oxide layer were dependent on the kind of iron oxides. The iron oxides deposit increases the failure risk of the pipeline and localized corrosion can be occurred under the α-FeOOH-covered region of the pipeline. Thus, prevention methods for the iron oxide deposit in the district pipeline system such as filtering or periodic chemical cleaning are needed.

In-situ generated tribomaterial in metal/metal contacts: Current understanding and future implications for implants

Artificial hip joints operate in aqueous biofluids that are highly reactive towards metallic surfaces. The reactivity at the metal interface is enhanced by mechanical interaction due to friction, which can change the near-surface structure of the metal and surface chemistry. There are now several reports in the literature about the in-situ generation of reaction films and tribo-metallurgical transformations on metal-on-metal hip joints. This paper summarizes current knowledge and provides a mechanistic interpretation of the surface chemical and metallurgical phenomena. Basic concepts of corrosion and wear are illustrated and used to interpret available literature on in-vitro and in-vivo studies of metal-on-metal hip joints. Based on this review, three forms of tribomaterial, characterized by different combinations of oxide films and organic layers, can be determined. It is shown that the generation of these tribofilms can be related to specific electrochemical and mechanical phenomena in the metal interface. It is suggested that the generation of this surface reaction layer constitutes a way to minimize (mechanical) wear of MoM hip implants.

Influence of the coating level on the heterogeneous ozonolysis kinetics and product yields of chlorpyrifos ethyl adsorbed on sand particles

Heterogeneous oxidation of chlorpyrifos ethyl (CLP) coated sand particles by gaseous ozone was studied. Mono-size sand was coated with CLP at different coating levels between 10 and 100 μg g−1 and exposed to ozone. Results were analyzed thanks to Gas Surface Reaction and Surface Layer Reaction Models. Kinetic parameters derived from these models were analyzed and led to several conclusions. The equilibrium constant of O3 between the gas phase and the CLP-coated sand was independent on the sand contamination level. Ozone seems to have similar affinity for coated or uncoated sand surface. Meanwhile, the kinetic parameters decreased with an increasing coating level. Chlorpyrifos Oxon, (CLPO) has been identified and quantified as an ozonolysis product. The product yield of CLPO remains constant (53 ± 10%) for the different coating level.The key parameter influencing the CLP reactivity towards ozone was the CLP-coating level. This dependence had a great influence on the lifetime of the CLP coated on sand particles, with respect to ozone, which could reach several years at high contamination level.

Relationship between formation of surface-reaction layers and flux of dissociated species in C4F8/Ar plasma for SiO2 etching using pulsed-microwave plasma

The mechanism of highly selective etching of SiO2 using pulsed-microwave electron-cyclotron-resonance plasma was investigated by analyzing the relationship between plasma dissociations and fluorocarbon layers formed on surfaces during etching with a cyclo-C4F8/Ar gas mixture. Dissociated molecules of CxFy and CFx species were measured without fragmentations using ion attachment mass spectrometry, and both thicknesses and atomic concentrations of reaction layers formed on etched surfaces were analyzed using x-ray photoelectron spectroscopy. Thus, the impact of CxFy molecules on the formation of fluorocarbon layers were analyzed using this measurement system. The authors found that the process window of highly selective etching of SiO2 over Si was enlarged by using pulsed-microwave plasma because a thinner fluorocarbon layer was formed by controlling C4F8 dissociation by changing the duty cycle of the pulsed-microwaves. With conventional continuous plasma, an etch stop occurred at low wafer bias conditions because a thicker fluorocarbon layer, which protects the SiO2 surface from the ion bombardment, was formed on the SiO2 surface. The thicker fluorocarbon layer was formed from a large amount of CxFy species, such as C2F2, which were generated in the highly dissociated continuous plasma. On the contrary, with pulsed plasma, a thinner fluorocarbon layer was formed due to the lower flux of CxFy species because the dissociation of C4F8 was controlled by reducing the duty cycle of the pulsed-microwave plasma. As a result, the process window was enlarged to the low wafer bias conditions using the pulsed-microwave plasma.

Role of surface-reaction layer in HBr/fluorocarbon-based plasma with nitrogen addition formed by high-aspect-ratio etching of polycrystalline silicon and SiO2 stacks

The etching of polycrystalline silicon (poly-Si)/SiO2 stacks by using VHF plasma was studied for three-dimensional NAND fabrication. One critical goal is achieving both a vertical profile and high throughput for multiple-stack etching. While the conventional process consists of multiple steps for each stacked layer, in this study, HBr/fluorocarbon-based gas chemistry was investigated to achieve a single-step etching process to reduce process time. By analyzing the dependence on wafer temperature, we improved both the etching profile and rate at a low temperature. The etching mechanism is examined considering the composition of the surface reaction layer. X-ray photoelectron spectroscopy (XPS) analysis revealed that the adsorption of N–H and Br was enhanced at a low temperature, resulting in a reduced carbon-based-polymer thickness and enhanced Si etching. Finally, a vertical profile was obtained as a result of the formation of a thin and reactive surface-reaction layer at a low wafer temperature.

Effect of Laser Surface Treatment on the Corrosion Behavior of FeCrAl-Coated TZM Alloy

The current study involves the coating of Titanium-Zirconium-Molybdenum (TZM) alloy with FeCrAl through plasma thermal spraying which proved effective in improving the oxidation resistance of the substrate. A post-laser surface melting treatment further enhanced the surface protection of the TZM alloy. Oxidation tests conducted at 1100 °C in air indicated that some Mo oxides were formed at the surface but a relatively small amount of weight reduction was observed for FeCrAl-coated TZM alloys up to 60 min of treatment. The post-laser surface treatment following the plasma thermal spray process apparently delayed the severe oxidation process and surface spalling of the alloy. It was suggested that the slow reduction in weight in the post-laser-treated specimen was related to fewer defects in the coating layer. It was also found that a surface reaction layer formed through the diffusion of Fe into the Mo alloy substrate at high temperature. The layer mainly consisted of Fe-saturated Mo and FeMo intermetallic compounds. In order to observe the corrosion behavior of the laser-treated alloy in 3.5% NaCl solution, electrochemical characteristics were also investigated. A proposed equivalent circuit model for the specimen indicated localized corrosion of coated alloy with some permeable defects in the coating layer.

Analysis of surface-reaction layers formed by etching Si3N4 with pulsed-microwave plasma

The mechanism of highly selective etching of Si3N4 by a pulsed-microwave electron-cyclotron-resonance plasma was investigated by analyzing surface-reaction layers formed by etching using a CH3F/O2/Ar gas chemistry. A hydrofluorocarbon (HFC) layer formed not only on nonpatterned materials (Si3N4 and others) but also at the bottoms of line-and-space patterns were analyzed by X-ray photoelectron spectroscopy. Thermal reactivity between the HFC layer and the Si3N4 layer was also investigated by thermal-desorption spectroscopy. The investigation results show that nitrogen contained in the Si3N4 layer thermally reacted with the HFC layer to form NH3 or HCN, and silicon contained in Si3N4 had high reactivity with fluorine contained in the HFC layer. Owing to the high reactivity between the fluorine-rich HFC layer and the Si3N4 layer in the pulsed-microwave plasma, the HFC layer became thin, even at a low wafer bias, and thus promoted ion-assisted etching. A wide process window was provided by the formation of the fluorine-rich thin HFC layer using the pulsed-microwave plasma.

Investigation of post-annealing enhancement effect of passivation quality of hydrogenated amorphous silicon

The excellent surface passivation scheme for suppression of surface recombination is a basic prerequisite to obtain high efficiency solar cells. Particularly, the HIT (heterojunction with intrinsic thin-layer) solar cell, which possesses an abrupt discontinuity of the crystal network at an interface between the crystalline silicon (c-Si) surface and the hydrogenated amorphous silicon (a-Si:H) thin film, usually causes a large density of defects in the bandgap due to a high density of dangling bonds, so it is very important for high energy conversion efficiency to obtain millisecond (ms) range of minority carrier lifetime (i. e. 2 ms). The a-Si:H, due to its excellent passivation properties obtained at low deposition temperatures and also mature processing, is still the best candidate materials for silicon HIT solar cell. Deposition of a transparent conductive oxide (TCO), such as indium tin oxide (ITO), has to be used to improve the carrier transport, since the lateral conductivity of a-Si:H is very poor. Usually, ITO is deposited by magnetron sputtering, but damage of a-Si:H layers by sputtering-induced ion bombardment inevitably occurs, thus triggering the serious degradation of the minority carrier lifetime, i. e., a loss in wafer passivation. Fortunately, this damage can be often recovered by some post-annealing. In this paper, however, the situation is different, and it is found that the minority carrier lifetime of ITO/a-Si:H/c-Si/a-Si:H heterojunction has been drastically enhanced by post-annealing after sputtering ITO on a- Si:H/c-Si/a-Si:H heterojunction (from 1.7 ms to 4.0 ms), not just recovering. It is very important to investigate how post-annealing enhances the lifetime and its physics nature. Combining the two experimental ways of HF treatment and vacuum annealing, three possible reasons for this enhancement effect (the field effect at the ITO/a-Si:H interface, the surface reaction-layer resulting from annealing in air, and the optimization of a-Si:H material itself) have been studied, suggesting this is irrelevant to the first two. The influence of post-annealing on a-Si:H/c-Si/a-Si:H heterojunction deposited at different temperatures has also been investigated. It is found that the remarkable enhancement effect of post-annealing is for low growth temperature(175 ℃) and not for high growth temperature(200 ℃), with the confirmation of an effective way for high quality passivation using growth at low temperature and then annealed at high temperature. Moreover, the configuration of a-Si:H at different growth temperatures between afore and after annealing has been discussed by an application of Fourier transform infrared (FTIR) spectroscopy. It is shown that the large increase of the lifetime of the heterojunction after annealing results from the improvement of microstructure of a-Si:H itself, which is essentially a competitive balance of the dominant role of some micro-factors, including hydrogen content, hydrogen bonding and network disorder in amorphous silicon film determined by the optimized matching between the growth temperature of a-Si:H materials and the annealing temperature of the heterojunction. An optimum control for this balance point is the essential cause of lifetime enhancement.

X‐Ray Photoelectron Spectroscopy Investigations of the Surface Reaction Layer and its Effects on the Transformation Properties of Nanoscale Ti51Ni38Cu11 Shape Memory Thin Films

The depth‐dependent chemical constitution of Ti51Ni38Cu11 thin films of different total film thickness from 400 to 50 nm was characterized using X‐ray photoelectron spectroscopy (XPS). It was analyzed how reaction layers, which form on the surface of the film significantly change the chemical composition of the transforming phase, which leads in turn to altered phase transformation properties. For thinner films, the deviation from the nominal chemical composition increases. For a film thickness of 50 nm, a Ti loss of ≈9 at% is observed. The Ni content is increased by ≈5 at%, whereas the Cu content stays relatively constant for films of different thickness. The results are summarized in a layer model, which supports designing nanoscale shape memory thin films.

Chemical and structural stability of lithium-ion battery electrode materials under electron beam.

The investigation of chemical and structural dynamics in battery materials is essential to elucidation of structure-property relationships for rational design of advanced battery materials. Spatially resolved techniques, such as scanning/transmission electron microscopy (S/TEM), are widely applied to address this challenge. However, battery materials are susceptible to electron beam damage, complicating the data interpretation. In this study, we demonstrate that, under electron beam irradiation, the surface and bulk of battery materials undergo chemical and structural evolution equivalent to that observed during charge-discharge cycling. In a lithiated NiO nanosheet, a Li2CO3-containing surface reaction layer (SRL) was gradually decomposed during electron energy loss spectroscopy (EELS) acquisition. For cycled LiNi0.4Mn0.4Co0.18Ti0.02O2 particles, repeated electron beam irradiation induced a phase transition from an layered structure to an rock-salt structure, which is attributed to the stoichiometric lithium and oxygen removal from 3a and 6c sites, respectively. Nevertheless, it is still feasible to preserve pristine chemical environments by minimizing electron beam damage, for example, using fast electron imaging and spectroscopy. Finally, the present study provides examples of electron beam damage on lithium-ion battery materials and suggests that special attention is necessary to prevent misinterpretation of experimental results.