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At least 1,279 records · Page 71

Scanning transmission election microscopy observations of twisted epitaxial gold nanodiscs in twisted molybdenum disulfide bilayers

Atomic scale, scanning transmission electron microscopy (STEM) analysis of the moiré structures in twisted epitaxial gold nanodiscs encapsulated in twisted bilayer molybdenum disulfide is presented. High angle annular dark field STEM imaging reveals that the period of the moiré patterns between gold and molybdenum disulfide varies with different twist angles of the bilayer molybdenum disulfide, ranging from 1.80 nm (epitaxial alignment of gold) to 1.53 nm (twisted epitaxial alignment of gold). Additionally, bright field STEM imaging reveals a faint, larger "moiré of moiré" structure in cases where the bilayer molybdenum disulfide twist angle is small (~6°), arising from the overlapping three-layers, which is not visible in conventional transmission electron microscopy images. In conclusion, our experiments indicate that scanning transmission electron microscopy as a suitable tool for moiré analysis of twisted multilayer planar heterostructures, complementary to information provided by conventional transmission electron microscopy and diffraction.

Au↗

Quantitative Electron Beam‐Single Atom Interactions Enabled by Sub‐20‐pm Precision Targeting

The ability to probe and control matter at the picometer scale is essential for advancing quantum and energy technologies. Scanning transmission electron microscopy offers powerful capabilities for materials analysis and modification, but sample damage, drift, and scan distortions hinder single atom analysis and deterministic manipulation. Materials analysis and modification via electron–solid interactions can be transformed by precise delivery of electrons to a specified atomic location, maintaining the beam position despite drift, and minimizing collateral dose. Here a fast, low-dose, sub-20-pm precision electron beam positioning technique is developed, “atomic lock-on,” (ALO), which offers the ability to position the beam on a specific atomic column without previously irradiating that column. This technique is used to lock onto a single selected atomic location to repeatedly measure its weak electron energy loss signal despite sample drift. Moreover, electron beam-matter interactions in single atomic events are measured with μ s time resolution. This enables observation of single-atom dynamics, such as atomic bistability, revealing partially bonded atomic configurations and recapture phenomena. This opens prospects for using electron microscopy for high-precision measurements and deterministic control of matter for quantum technologies.

2D materials↗

Microscopy of hierarchically organized TiO{sub 2} photoelectrode for dye solar cells

Research on improving the performance of dye solar cells has various aspects of the device being investigated. This paper analyzes the deliberately hierarchized photoelectrode configuration for DSC applications to improve the performance of DSCs. Multiple layers of differently composed TiO{sub 2} particle types namely aggregates and nanoparticles were deposited to form a photoelectrode with thickness of about 12 µm. The photoelectrodes were assembled into working DSCs with an active area of 1 cm{sup 2}. Measurement for solar power conversion performance was measured under 1 sun at AM1.5 spectrum simulated sunlight. Electron microscopy for photoelectrode analysis was conducted using Field Emission Scattering Electron Microscopy with enhanced resolution. External Quantum Efficiency was measured using a purpose built instrument. Kinetics were investigated using the Electrochemical Impedance Spectroscopy (EIS) measurement with a potentiostat. The best performing DSC is of the hierarchically organized photoelectrode with a photoconversion efficiency of 4.58%, an increase of 14% in comparison to the reference samples with fully aggregates configuration. Short circuit current density, Jsc increases by about 2.223 mA cm{sup −2} relative to the blanks. The electron microscopy confirmed expected thickness at around 10 µm and layers forming the photoelectrode being hierarchically deposited with ∼20 nm TiO{sub 2} nanoparticles and 450 nm TiO{sub 2} aggregates mixture composition. EQE improved especially for visible region of 500-550 nm light wavelengths with 12 % increase in the response of in that region. Improvement to the diffusion coefficient as measured by the EIS contributed to the performance increase of the photoelectrode configuration under investigation.

14 SOLAR ENERGY↗

Characterization study of polycrystalline tin oxide surfaces before and after reduction in CO

Polycrystalline tin oxide surfaces have been examined before and after reduction in 40 Torr of CO at 100 and 175 C using Auger electron spectroscopy (AES), electron spectroscopy for chemical analysis (ESCA), ion scattering spectroscopy (ISS) and electron stimulated desorption (ESD). The changes in the surface composition and chemical states of the surface species generally are subtle for the reductive conditions used. However, significant changes do occur with regard to the amounts and the chemical forms of the hydrogen-containing species remaining after both the 100 and 175 C reductions.

Drawdy, Jean E.↗

Gamma Irradiation of NaCl-UCl 3 Salt for the Molten Chloride Fast Reactor

This report documents the results of the gamma ray irradiation of NaCl-UCl 3 eutectic salt in the Advanced Test Reactor (ATR) spent fuel pool gamma tube and subsequent analysis of capsules utilizing the Gas Assay Sample and Recharge (GASR) system. NaCl-UCl 3 salt capsules at four different temperatures, 75C, 150C, 300C and 600C, were irradiated shortly after the core internal changeout (CIC) of the ATR, beginning April 28 th of 2021, and ending on August 18 th of 2021. Re-positioning of the fuel elements in the spent fuel pool to move more fresh fuel elements around the gamma tube occurred on May 11 th of 2021, resulting in an approximate 20% increase in the dose rate and consequently the total absorbed dose. In total, the salt-filled capsules underwent 2638 hours of gamma irradiation from the adjacent freshly discharged ATR spent fuel. Capsule internal pressure measurements were taken via the Gas Assay Sample and Recharge (GASR) system in the INL Hot Fuels Examination Facility (HFEF) following completion of the irradiation. Based on the GASR analysis results, the primary conclusion from this experiment to-date is that radiolytic generation of chlorine gas is insignificant for the dose rates and total absorbed dose that these samples experienced. To elucidate more detailed effects of radiolysis on NaCl-UCl 3 eutectic salts and reach a more definitive conclusion, further advanced analyses such as electron microscopy, simultaneous thermal analysis, and electron paramagnetic resonance are recommended to analyze the capsule wall and salt samples.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Thermal Analysis of the Advanced Modular Power Systems (AMPS) Power Electronic Modules

In an effort to transform future space power system architectures and operations, the Advanced Modular Power Systems (AMPS) project is currently developing an interface standard for power electronic modules to enable modular architectures for space power systems. Each architecture would consist of one or more modular electronic units (MEU) that would comprise of a tailored combination of modules. The standard currently comprises modules enabling switchgear, power conversion, and data interfacing. The objective of the AMPS project is to enable the modularity and interchangeability of different architectures using these standardized modules in hopes of reducing complexity and cost, increasing inherent redundancy and reliability, and minimizing power system redesign for future programs. A key enabler to these future modular architectures will be the thermal management system, which has to contend with acquiring heat from the electronics modules at the card level and then transporting that heat to the radiator of the larger system. The focus of this paper, therefore, will be the thermal design and analysis of multiple AMPS power electronics modules and the development of their thermal-vacuum test.

Modular Power Electronics↗

Synthesis of magnesiowüstite nanocrystallites embedded in an amorphous silicate matrix via low energy multiple ion implantations

The synthesis process is presented for experimentally simulating modifications in cosmic dust grains using sequential ion implantations or irradiations followed by thermal annealing. Cosmic silicate dust analogues were prepared via implantation of 20–80 keV Fe - , Mg - , and O - ions into commercially available p-type silicon (100)wafers. The as-implanted analogues are amorphous with a Mg/(Fe+Mg) ratio of 0.5 tailored to match theoretical abundances in circumstellar dusts. Before the ion implantations were performed, Monte-Carlo-based ion-solid interaction codes were used to model the dynamic redistribution of the implanted atoms in the silicon substrate. 600 keV helium ion irradiation was performed on one of the samples before thermal annealing. Two samples were thermally annealed at a temperature appropriate for an M-class stellar wind, 1000 K, for 8.3 h in a vacuum chamber with a pressure of 1 x 10 -7 torr. The elemental depth profiles were extracted utilizing Rutherford Backscattering Spectrometry (RBS) in the samples before and after thermal annealing. X-ray diffraction (XRD)analysis was employed for the identification of various phases in crystalline minerals in the annealed analogues. Transmission electron microscopy (TEM) analysis was utilized to identify specific crystal structures. RBS analysis shows redistribution of the implanted Fe, Mg, and O after thermal annealing due to incorporation into the crystal structures for each sample type. XRD patterns along with TEM analysis showed nanocrystalline Mg and Fe oxides with possible incorporation of additional silicate minerals.

79 ASTRONOMY AND ASTROPHYSICS↗

Spontaneous synchrotron emission from a plasma with an energetic runaway electron tail

The emissivity of spontaneous synchrotron radiation is computed for a plasma consisting of a background thermal plasma in addition to an energetic runaway electron component. The analysis is performed for both the ordinary and extraordinary modes, for frequencies in the vicinity of the electron plasma frequency and the higher harmonics of the electron gyrofrequency, and for the case when the electron plasma frequency is approximately the same as or smaller than the cyclotron frequency. The relativistic gyroresonance with the runaway electrons is found to result in a level of spontaneous emission which, for frequencies in the neighborhood of the electron plasma frequency, is significantly enhanced over the thermal radiation.

Freund, H. P.↗

Enhancement of two dimensional electron gas concentrations due to Si{sub 3}N{sub 4} passivation on Al{sub 0.3}Ga{sub 0.7}N/GaN heterostructure: strain and interface capacitance analysis

Enhancement of two dimensional electron gas (2DEG) concentrations at Al{sub 0.3}Ga{sub 0.7}N/GaN hetero interface after a-Si{sub 3}N{sub 4} (SiN) passivation has been investigated from non-destructive High Resolution X-ray Diffraction (HRXRD) analysis, depletion depth and capacitance-voltage (C-V) profile measurement. The crystalline quality and strained in-plane lattice parameters of Al{sub 0.3}Ga{sub 0.7}N and GaN were evaluated from double axis (002) symmetric (ω-2θ) diffraction scan and double axis (105) asymmetric reciprocal space mapping (DA RSM) which revealed that the tensile strain of the Al{sub 0.3}Ga{sub 0.7}N layer increased by 15.6% after SiN passivation. In accordance with the predictions from theoretical solution of Schrödinger-Poisson’s equations, both electrochemical capacitance voltage (ECV) depletion depth profile and C-V characteristics analyses were performed which implied effective 9.5% increase in 2DEG carrier density after passivation. The enhancement of polarization charges results from increased tensile strain in the Al{sub 0.3}Ga{sub 0.7}N layer and also due to the decreased surface states at the interface of SiN/Al{sub 0.3}Ga{sub 0.7}N layer, effectively improving the carrier confinement at the interface.

36 MATERIALS SCIENCE↗

A new technique for Auger analysis of surface species subject to electron-induced desorption.

A method is presented to observe surface species subject to electron-induced desorption by Auger electron spectroscopy. The surface to be examined is moved under the electron beam at constant velocity, establishing a time-independent condition and eliminating the time response of the electron spectrometer as a limiting factor. The dependence of the Auger signal on the sample velocity, incident electron current, beam diameter, and desorption cross section is analyzed. It is shown that it is advantageous to analyze the moving sample with a high beam current, in contrast to the usual practice of using a low beam current to minimize desorption from a stationary sample. The method is illustrated by the analysis of a friction transfer film of PTFE, in which the fluorine is removed by electron-induced desorption. The method is relevant to surface studies in the field of lubrication and catalysis.

Pepper, S. V.↗

Rheology, Mechanical Properties and Morphology of Poly(lactic acid)/Ethylene Vinyl Acetate Blends

In this work, the effect of ethylene vinyl acetate (EVA) content on the rheology, mechanical properties, and morphology of poly (lactic acid) (PLA)/EVA blends was investigated. Differential Scanning Calorimetry (DSC) showed that the addition of EVA to PLA decreased the degree of crystallinity of PLA. Dynamic Mechanical Thermal Analysis (DMTA) results showed that the presence of EVA copolymer increased the cold crystallization temperature (T{sub cc}) of PLA. The addition of 10% of EVA to PLA substantially increased the impact strength. Morphology analysis by Scanning Electron Microscopy (SEM) indicated the immiscibility between PLA and EVA phases and an in increase the EVA average dispersed phase domains size with the increase in EVA content. Rheological measurements under oscillatory shear flow showed that storage modulus (G′) increased with the increase in the EVA content at low frequencies and is related to the increase in the EVA dispersed phase domains size, as also observed by relaxation spectrum analysis. Cole–Cole plots of imaginary viscosity (η″) versus real viscosity (η′) and Han plots of storage modulus (G′) versus loss modulus (G″) indicated that PLA and EVA phases are immiscible, as also observed by SEM.

36 MATERIALS SCIENCE↗

Machine learning for automated experimentation in scanning transmission electron microscopy

Abstract Machine learning (ML) has become critical for post-acquisition data analysis in (scanning) transmission electron microscopy, (S)TEM, imaging and spectroscopy. An emerging trend is the transition to real-time analysis and closed-loop microscope operation. The effective use of ML in electron microscopy now requires the development of strategies for microscopy-centric experiment workflow design and optimization. Here, we discuss the associated challenges with the transition to active ML, including sequential data analysis and out-of-distribution drift effects, the requirements for edge operation, local and cloud data storage, and theory in the loop operations. Specifically, we discuss the relative contributions of human scientists and ML agents in the ideation, orchestration, and execution of experimental workflows, as well as the need to develop universal hyper languages that can apply across multiple platforms. These considerations will collectively inform the operationalization of ML in next-generation experimentation.

36 MATERIALS SCIENCE↗

Improving Electronic Conductivity of Layered Oxides through the Formation of Two-Dimensional Heterointerface for Intercalation Batteries

Synthetic strategies for the improvement in electronic conductivities and electrochemical stabilities of transition metal oxide cathodes, which are limiting factors in the performance of commercial intercalation batteries, are required for next-generation, high-performance battery systems. Furthermore, the chemical preintercalation approach, consisting of a combined sequence of a sol–gel process, extended aging, and a hydrothermal treatment, is a versatile, wet synthesis technique that allows for the incorporation of a polar species between the layers of transition metal oxides. Here, formation of a layered 2D δ-C x V 2 O 5 · n H 2 O heterostructure occurs via chemical preintercalation of dopamine molecules between bilayers of vanadium oxide followed by the hydrothermal treatment of the precipitate, leading to carbonization of the organic molecules. The presence of carbon layers within the structure has been confirmed via a combined analysis of scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, Raman spectroscopy, X-ray photoelectron spectroscopy, electrochemical impedance spectroscopy, four-probe conductivity measurements, and scanning transmission electron microscopy characterization. 2D δ-C x V 2 O 5 · n H 2 O heterostructure electrodes demonstrated significantly improved electrochemical performance, particularly at higher current densities, in Li-ion cells. The heterostructure electrodes exhibited 75% of the capacity retention when the current was changed from 20 mA g –1 (206 mAh g –1 ) to 300 mA g –1 (155 mAh g –1 ), while the reference δ-V 2 O 5 · n H 2 O electrodes exhibited only 10% capacity retention in the same experiment. Remarkably, 2D δ-C x V 2 O 5 · n H 2 O heterostructure electrodes demonstrated significantly improved capacity retention (94% after 30 cycles) for bilayered vanadium oxide electrodes in Li-ion cells during galvanostatic cycling at 20 mA g –1 . The improved electrochemical performance, in both extended cycling and rate capability studies, of the 2D δ-C x V 2 O 5 · n H 2 O heterostructure electrodes in the Li-ion system is ascribed to the intermittent formation of carbon layers within the bilayered structure, which leads to increased electronic conductivity and improved structural stability of the heterostructure compared to the reference δ-V 2 O 5 · n H 2 O electrodes.

25 ENERGY STORAGE↗

Designing Antifouling and Antimicrobial Interfaces: Structural Characterization using CryoEM, Automated Microscopy, and AI Image Segmentation

The design of functionalized surfaces for interactions with biological systems is critical across sectors such as healthcare, energy, and agriculture. Tailoring materials for specific applications, such as antifouling and antimicrobial surfaces, demands a comprehensive understanding of topology and chemistry across multiple length and time scales on both biological and materials systems. This work presents the development and characterization of nanostructured surfaces with controlled topographies and chemistries that enhance bacterial membrane disruption, reduce biofilm formation, and improve antimicrobial and antifouling capabilities. Two specific use cases will be presented - the use of cellulose nanocrystals (CNCs) for bacterial growth inhibition and the development of antifouling surfaces to prevent protein and bacterial adsorption [1-4]. By leveraging large language models (LLMs) for image segmentation and training [5], we enable automated analysis of terabyte-scale cryogenic electron microscopy (cryoEM) datasets. This analysis provides statistical insights into the biotic/abiotic interface and facilitates automated electron microscopy experiments to mitigate time and dose. The integration of cryogenic electron tomography (cryoET) and cryogenic focused ion beam (cryoFIB) milling enables high-resolution, near-native-state imaging and 3D reconstructions of bio/material interfaces [6]. Orthogonal characterization techniques and computational modeling further enhances our understanding, offering a robust platform for the design and optimization of next-generation functional surfaces [7].

Williams, Alexis [ORNL] (ORCID:0000000252835822)↗

Adsorption Efficiency of Polyaspartate-Montmorillonite Composite Towards the Removal of Pb(II) and Cd(II) from Aqueous Solution

The selective modification of sodium montmorillonite (Na{sup +}-Mt) surface with polyionene followed by poly (succinimde-co-aspartate) has been considered. Na{sup +}-Mt was allowed to react with well characterized polyionene in two fold excess. The resulting polyionene/Mt (IC) was further modified with poly (succinimide-co-aspartate) through an ion exchange process. The obtained polyaspartate/Mt (IPS) composite was characterized by elemental analysis, X-ray diffraction, FTIR spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and BET surface analyzer. The adsorption efficiency of IPS composite was investigated for the removal of Pb(II) and Cd(II) from aqueous solution under different experimental conditions including initial metal ions concentration, temperature and single and binary mixture systems of metal ions. The experimental data were analyzed by Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich models. Langmuir model reveals that the monolayer adsorption capacity of IPS was 92.59 and 67.57 mg/g for Pb(II) and Cd(II), respectively. The modification of parent Na{sup +}-Mt enhanced their adsorption capacity by about 87.91 and 29.84% for Pb(II) and Cd(II), respectively, due to inclusion of extra active sites of polyaspartate. The mean sorption energy, E calculated from Dubinin–Radushkevich isotherm were 2.75 and 1.98 kJ/mol for the adsorption of Pb(II) and Cd(II), respectively, indicating physical adsorption process. Also, The thermodynamic parameters were calculated and indicated that the adsorption was spontaneous and exothermic process. The mechanism of cation exchange and complexation of metal ions was suggested. IPS composite has a considerable potential for the removal of heavy metal ions from aqueous solution and wastewater stream.

36 MATERIALS SCIENCE↗

Using nonequilibrium dynamics to probe competing orders in a Mott-Peierls system

Competition between ordered phases, and their associated phase transitions, are significant in the study of strongly correlated systems. Here, we examine one aspect, the nonequilibrium dynamics of a photoexcited Mott-Peierls system, using an effective Peierls-Hubbard model and exact diagonalization. Near a transition where spin and charge become strongly intertwined, we observe antiphase dynamics and a coupling-strength-dependent suppression or enhancement in the static structure factors. The renormalized bosonic excitations coupled to a particular photoexcited electron can be extracted, which provides an approach for characterizing the underlying bosonic modes. The results from this analysis for different electronic momenta show an uneven softening due to a stronger coupling near k F . As a result, this behavior reflects the strong link between the fermionic momenta, the coupling vertices, and ultimately, the bosonic susceptibilities when multiple phases compete for the ground state of the system.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Relativistic electron acceleration and decay time scales in the inner and outer radiation belts: SAMPEX

High-energy electrons have been measured systematically in a low-altitude (520 x 675 km), nearly polar (inclination = 82 deg) orbit by sensitive instruments onboard the Solar, Anomalous, and Magnetospheric Particle Explorer (SAMPEX). Count rate channels with electron energy thresholds ranging from 0.4 MeV to 3.5 MeV in three different instruments have been used to examine relativistic electron variations as a function of L-shell parameter and time. A long run of essentially continuous data (July 1992 - July 1993) shows substantial acceleration of energetic electrons throughout much of the magnetosphere on rapid time scales. This acceleration appears to be due to solar wind velocity enhancements and is surprisingly large in that the radiation belt 'slot' region often is filled temporarily and electron fluxes are strongly enhanced even at very low L-values (L aprroximately 2). A superposed epoch analysis shows that electron fluxes rise rapidly for 2.5 is approximately less than L is approximately less than 5. These increases occur on a time scale of order 1-2 days and are most abrupt for L-values near 3. The temporal decay rate of the fluxes is dependent on energy and L-value and may be described by J = Ke-t/to with t(sub o) approximately equals 5-10 days. Thus, these results suggest that the Earth's magnetosphere is a cosmic electron accelerator of substantial strength and efficiency.

Baker, D. N.↗

Miniature Time-of-Flight Mass Spectrometer

Major advances must occur to protect astronauts from prolonged periods in near-zero gravity and high radiation associated with extended space travel. The dangers of living in space must be thoroughly understood and methods developed to reverse those effects that cannot be avoided. Six of the seven research teams established by the National Space Biomedical Research Institute (NSBRI) are studying biomedical factors for prolonged space travel to deliver effective countermeasures. To develop effective countermeasures, each of these teams require identification of and quantitation of complex pharmacological, hormonal, and growth factor compounds (biomarkers) in humans and in experimental animals to develop an in-depth knowledge of the physiological changes associated with space travel. At present, identification of each biomarker requires a separate protocol. Many of these procedures are complicated and the identification of each biomarker requires a separate protocol and associated laboratory equipment. To carry all of this equipment and chemicals on a spacecraft would require a complex clinical laboratory; and it would occupy much of the astronauts time. What is needed is a small, efficient, broadband medical diagnostic instrument to rapidly identify important biomarkers for human space exploration. The Miniature Time-Of- Flight Mass Spectrometer Project in the Technology Development Team is developing a small, high resolution, time-of-flight mass spectrometer (TOFMS) to quantitatively measure biomarkers for human space exploration. Virtues of the JHU/APL TOFMS technologies reside in the promise for a small (less than one cubic ft), lightweight (less than 5 kg), low-power (less than 50 watts), rugged device that can be used continuously with advanced signal processing diagnostics. To date, the JHU/APL program has demonstrated mass capability from under 100 to beyond 10,000 atomic mass units (amu) in a very small, low power prototype for biological analysis. Further, the electronic nature of the TOFMS output makes it ideal for rapid telemetry to earth for in-depth analysis by ground support teams.

Potember, Richard S.↗