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At least 127 records · Page 7

Mapping Electron Beam-Induced Radiolytic Damage in Molecular Crystals

Every electron crystallography experiment is fundamentally constrained by radiation damage [1]. Despite its crucial importance, little is understood about the onset and progression of radiolysis in beam-sensitive molecular crystals [2]. Since the typical metric used for monitoring the degradation induced by radiolysis is the attenuation of Bragg reflections in electron diffraction patterns [3], the scope of previous analyses [2-6] has mostly been limited to indirect observation via the back focal plane. Here, a simultaneous visualization of the effects of electron beam-induced radiolysis—in both real space and reciprocal space—remains elusive.

74 ATOMIC AND MOLECULAR PHYSICS↗

Chemical and Structural Stability of Lithium-Ion Battery Electrode Materials under Electron Beam

Our 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. But, 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 LiNi 0.4 Mn 0.4 Co 0.18 Ti 0.02 O 2 particles, repeated electron beam irradiation induced a phase transition from an R$\bar{3}$m layered structure to an rock-salt structure, which is attributed to the stoichiometric lithium and oxygen removal from R$\bar{3}$m 3a and 6c sites, respectively. Nevertheless, it is still feasible to preserve pristine chemical environments by minimizing electron beam damage, for example, in 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.

25 ENERGY STORAGE↗

Strain Field Analysis in Electronic Components by ESPI: Bad Thermal Contact and Damage Evaluation

Designing electronic components and devices is a complex task that must include also considerations about thermo-mechanical behavior of the component itself. This aspect, in fact, can affect the reliability of the device as a consequence of the thermal stresses that are introduced in the component while it is working. Stress concentration can arise, in fact, due to different thermal expansion coefficients of the materials involved. Determining the thermo-mechanical response by numerically methods is not simple and not always possible so that experimental methods are preferable. In this paper, specifically, the electronic speckle pattern interferometry technique was adopted to measure full-field strain of the component during exercise. By using an optical technique it is possible to get information about the behavior of the component without being in contact with the component itself so that the dissipation coefficient is not altered. The system was able to detect gradients of deformation in the component itself connected to the different distribution of internal current in the component. Moreover, it was observed, that the presence of bad thermal contact between the package and the heat sink can be revealed because it results in a different thermos-mechanical behavior of the component. Finally, a critical defect was introduced in the component and it was observed the way the presence of damage affects the in-plane displacement of the component. Very huge differences were observed leading to the consideration that this kind of approach could be conveniently adopted also as a damage detection tool.

42 ENGINEERING↗

Effects of electron–phonon coupling on damage accumulation in molecular dynamics simulations of irradiated nickel

The role of the electronic system in high energy displacement cascades is explored. The energy exchange between the electronic and the atomic subsystem is described by the electron–phonon coupling. The electronic effects on the damage accumulation due to 100 keV Ni ion cascades in nickel, a prototype system to a large group of nickel-based high entropy alloys, are investigated for overlapping cascades. It is shown that the energy exchange between the two subsystems affects microstructure evolution, resulting in the formation of smaller clusters and more isolated defects. This effect is more significant for the vacancy cluster formation and size distribution.

36 MATERIALS SCIENCE↗

Study of fretting wear in titanium, Monel-400, and cobalt-25 percent molybdenum using scanning electron microscopy.

Damage scar volume measurements taken from like metal fretting pairs, combined with scanning electron microscopy observations, showed that three sequentially operating mechanisms result in the fretting of titanium, Monel-400, and cobalt-25% molybdenum. Initially, adhesion and plastic deformation on the surface played an important role. This was followed after a few hundred cycles by a fatigue mechanism, producing spall-like pits in the damage scar. Finally, an oxidation-related mechanism became most significant. Damage scar measurements made on several elemental metals after 600,000 fretting cycles suggested that the ratio of oxide hardness to metal hardness was a measure of the susceptibility of a metal to progressive damage by fretting.

Bill, R. C.↗

Fretting wear in titanium, Monel-400, and cobalt 25-percent-molybdenum using scanning electron microscopy

Damage scar volume measurements taken from like metal fretting pairs combined with scanning electron microscopy observations showed that three sequentially operating mechanisms result in the fretting of titanium, Monel-400, and cobalt - 25-percent molybdenum. Initially, adhesion and plastic deformation of the surface played an important role. This was followed after a few hundred cycles by a fatigue mechanism which produced spall-like pits in the damage scar. Finally, a combination of oxidation and abrasion by debris particles became most significant. Damage scar measurements made on several elemental metals after 600,000 fretting cycles suggested that the ratio of oxide hardness to metal hardness was a measure of the susceptibility of a metal to progressive damage by fretting.

Bill, R. C.↗

High‐Resolution Electron Tomography of Ultrathin Boerdijk–Coxeter–Bernal Nanowire Enabled by Superthin Metal Surface Coating

Abstract The rapid advancement of transmission electron microscopy has resulted in revolutions in a variety of fields, including physics, chemistry, and materials science. With single‐atom resolution, 3D information of each atom in nanoparticles is revealed, while 4D electron tomography is shown to capture the atomic structural kinetics in metal nanoparticles after phase transformation. Quantitative measurements of physical and chemical properties such as chemical coordination, defects, dislocation, and local strain have been made. However, due to the incompatibility of high dose rate with other ultrathin morphologies, such as nanowires, atomic electron tomography has been primarily limited to quasi‐spherical nanoparticles. Herein, the 3D atomic structure of a complex core–shell nanowire composed of an ultrathin Boerdijk–Coxeter–Bernal (BCB) core nanowire and a noble metal thin layer shell deposited on the BCB nanowire surface is discovered. Furthermore, it is demonstrated that a new superthin noble metal layer deposition on an ultrathin BCB nanowire could mitigate electron beam damage using an in situ transmission electron microscope and atomic resolution electron tomography. The colloidal coating method developed for electron tomography can be broadly applied to protect the ultrathin nanomaterials from electron beam damage, benefiting both the advanced material characterizations and enabling fundamental in situ mechanistic studies.

Song, Xiaohui↗

Effects of recoil spectra and electronic energy dissipation on defect survival in 3C-SiC

The coincidence of electronic and damage energy dissipation from energetic ions to an atomic lattice can significantly affect damage production along the ion trajectory due to spatial overlap of inelastic and elastic processes. Damage production and disordering in single crystal 3C-SiC from 5 MeV Si and 10 MeV Au ions is investigated using ion-channeling experiments. While defects are created by damage energy dissipation via elastic scattering, electronic energy dissipation via electron-phonon coupling decreases defect survival along the ion trajectory for Si ions. Finally, the more energetic recoil spectrum for 10 MeV Au ions leads to weaker spatial coupling of electronic and damage energy dissipation processes, and damage production is only weakly affected.

36 MATERIALS SCIENCE↗

FreeDam – A webtool for free-electron laser-induced damage in femtosecond X-ray crystallography

Over the last decade X-ray free-electron laser (XFEL) sources have been made available to the scientific community. One of the most successful uses of these new machines has been protein crystallography. When samples are exposed to the intense short X-ray pulses provided by the XFELs, the sample quickly becomes highly ionized and the atomic structure is affected. Here we present a webtool dubbed FreeDam based on non-thermal plasma simulations, for estimation of radiation damage in free-electron laser experiments in terms of ionization, temperatures and atomic displacements. The aim is to make this tool easily accessible to scientists who are planning and performing experiments at XFELs.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Track damage and erosion of insulators by ion-induced electronic processes

Track damage and the associated ejection of atoms and molecules from insulators, which occur as a result of ion-induced electronic excitation, are of interest both in their own right and because of the mechanisms through which the energy in the excited electrons is transformed into atomic motion. In this paper an overview is given of the phenomena that are observed. We show that there is a remarkable similarity between the damage profile along the ion's track in the solid and the yield of ejected atoms at the energy that corresponds to each point on the track. It is also seen that the density of extended defects (or, correspondingly, the ejected particle yield) appears to have a 'universal' form that is weakly dependent on the type of material. In the model presented this is a consequence of the inner-shell ionization of light elements in the solid by the incident ion; the resulting Auger decay produces an intense ionization spike that locally triggers the track formation/erosion process. This model allows the estimation of erosion yields/damage profiles for different ions and materials.

Tombrello, T. A.↗

Gallium arsenide solar cell radiation damage study

A thorough analysis has been made of electron- and proton- damaged GaAs solar cells suitable for use in space. It is found that, although some electrical parametric data and spectral response data are quite similar, the type of damage due to the two types of radiation is different. An I-V analysis model shows that electrons damage the bulk of the cell and its currents relatively more, while protons damage the junction of the cell and its voltages more. It is suggested that multiple defects due to protons in a strong field region such as a p/n junction cause the greater degradation in cell voltage, whereas the individual point defects in the quasi-neutral minority-carrier-diffusion regions due to electrons cause the greater degradation in cell current and spectral response.

Maurer, R. H.↗

Effect of electron flux on radiation damage in GaAs solar cells

The objective of this work was to evaluate the effect of electron flux and temperature on radiation damage in GaAs solar cells. The defect levels and the power ratio of the GaAs solar cells under various irradiation conditions are compared. In a 200 C continuous annealing experiment, the GaAs solar cells which were irradiated at a flux of 2 x 10 to the 9th e/sq cm s suffered less power degradation than the cells which were irradiated at the same temperature at a higher flux of 4 x 10 to the 10th e/sq cm s. After the continuous annealing experiment, a single-step post annealing at 200 C was performed for 40 hr on these irradiated cells. An additional improvement in power recovery was observed only on those cells irradiated at the high flux of 4 x 10 to the 10th e/sq cm s. DLTS data indicate that the defect density decreases with lower electron flux. Both of these observations strongly suggest that the continuous annealing in GaAs cells can be effective at temperatures as low as 150 C, or even less in a space environment such as geosynchronous orbit.

Loo, R. Y.↗

Structural Complexities in Sodium Ion Conductive Antiperovskite Revealed by Cryogenic Transmission Electron Microscopy

Here we use low-dose cryogenic transmission electron microscopy (cryo-TEM) to investigate the atomic-scale structure of antiperovskite Na 2 NH 2 BH 4 crystals by preserving the room-temperature cubic phase and carefully monitoring the electron dose. Via quantitative analysis of electron beam damage using selected area electron diffraction, we find cryogenic imaging provides 6-fold improvement in beam stability for this solid electrolyte. Cryo-TEM images obtained from flat crystals revealed the presence of a new, long-range-ordered supercell with a cubic phase. The supercell exhibits doubled unit cell dimensions of 9.4 Å × 9.4 Å as compared to the cubic lattice structure revealed by X-ray crystallography of 4.7 Å × 4.7 Å. The comparison between the experimental image and simulated potential map indicates the origin of the supercell is a vacancy ordering of sodium atoms. This work demonstrates the potential of using cryo-TEM imaging to study the atomic-scale structure of air- and electron-beam-sensitive antiperovskite-type solid electrolytes.

36 MATERIALS SCIENCE↗