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DOE OSTI2020

Charged-Current Electron Neutrino Measurement with the MicroBooNE Detector

MicroBooNE is the first phase of Fermilab’s Short Baseline Neutrino (SBN) Liquid Argon Time Projection Chamber (LArTPC) programme.This proceeding outlays the first characterisation of electron neutrinos in a muon neutrino beam with the LArTPC detector technology. The Booster Neutrino Beam has an energy peaking around 1GeV and an electron content of approximately 0.5%. The analysis investigates electrons produced in charged-current electron neutrino interactions. The kinematics of the electrons are measured along with comparisons to simulation. Most of the systematic uncertainties are constrained using a data-driven sample of charged-current muon neutrino events. The measurement of electron neutrinos originating from the Booster Neutrino Beam is a crucial component to understand the nature of the observed excess of low energy electromagnetic-like events at MiniBooNE.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2023

Tuning MXene Surface Terminations for Strategic Control of Physical Properties

Scientific Achievement • Ti3C2Tx surfaces with a higher hydroxyl group concentration play a pivotal role in surface properties and were found to be thermodynamically stable. • From the electronic bonding analysis, the charge density difference and electron localization function demonstrated a significant electron localization at the hydroxyl group, which results in a locally induced dipole on the surface. • A large tunability in the work function is found from different concentrations of functional groups on the surface which can be controlled by the concentration of HF used for etching of the MAX phase to produce the resulting MXene. Research Details • The influence of termination group distribution on the surface of Ti3C2Tx MXenes from various etching concentrations of HF was evaluated • The work functions of Ti3C2Tx MXenes with differing concentrations of functional groups were determined • The influence of termination group clustering on the surface of Ti3C2Tx MXenes was investigated by visualization of the electron localization function and charge density difference

Ward, Patrick A.↗

DOE OSTI2022

Fabrication and Characterization of Iron-Based Catalysts for the Dehydrogenation of Fossil Fuels

For a prosperous and sustainable future, hydrogen is an encouraging solution due to its simple transition for industrial decarbonization and synergy for economic development. Paradoxically, current hydrogen production pathways release substantial amount of greenhouse gases into the atmosphere contributing to climate change. To keep up with increasing demand, hydrogen could be produced through microwave-assisted thermocatalytic dehydrogenation of fossil fuels without emitting carbon dioxide. This requires specified catalysts to meet the requirements of hydrogen yield and selectivity. The objective of the present research is to fabricate, characterize, and compare iron-based alumina (FeAlxOy) catalysts produced via solution combustion synthesis and iron-based catalysts on silicon carbide support (Fe/SiC) produced via incipient wetness impregnation. Heat mode, fuel type, and oxidizer mole ratio were varied for FeAlxOy catalysts, and metal loading was varied for Fe/SiC catalysts. Each resultant product was characterized by X-ray diffraction analysis, scanning electron microscopy, laser diffraction particle size analysis, and Brunauer-Emmett-Teller (BET) surface area analysis. Characterization suggests that fabrication of iron-based alumina nanocomposites through solution combustion synthesis in a muffle furnace using citric acid as the fuel yields the most promising catalyst.

Reyes, Victoria Isabel↗

DOE OSTI2025

Quantitative approaches for multiscale structural analysis with atomic resolution electron microscopy

Atomic-resolution imaging with scanning transmission electron microscopy is a powerful tool for characterizing the nanoscale structure of materials, in particular features such as defects, local strains, and symmetry-breaking distortions. In addition to advanced instrumentation, the effectiveness of the technique depends on computational image analysis to extract meaningful features from complex datasets recorded in experiments, which can be complicated by the presence of noise and artifacts, small or overlapping features, and the need to scale analysis over large representative areas. Here, we present image analysis approaches which synergize real and reciprocal space information to efficiently and reliably obtain meaningful structural information with picometer scale precision across hundreds of nanometers of material from atomic-resolution electron microscope images. Damping superstructure peaks in reciprocal space allows symmetry-breaking structural distortions to be disentangled from other sources of inhomogeneity and measured with high precision. Real-space fitting of the wavelike signals resulting from Fourier filtering enables absolute quantification of lattice parameter variations and strain, as well as the uncertainty associated with these measurements. Implementations of these algorithms are made available as an open source python package.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Structural analysis of Gd 6 FeBi 2 from single-crystal X-ray diffraction methods and electronic structure calculations

The crystal structure of the gadolinium iron bismuthide Gd 6 FeBi 2 has been characterized by single-crystal X-ray diffraction data and analyzed in detail using first-principles calculations. The structure is isotypic with the Zr 6 CoAl 2 structure, which is a variant of the ZrNiAl structure and its binary prototype Fe 2 P (Pearson code hP 9, Wyckoff sequence g f d a ). As such, the structure is best viewed as an array of tricapped trigonal prisms of Gd atoms centered alternately by Fe and Bi. The magnetic-ordering temperature of this compound ( ca 350 K) is much higher than that of other rare-earth metal-rich phases with the same or related structures. It is also higher than the ordering temperature of many other Gd-rich ternary phases, where the magnetic exchange is typically governed by Ruderman–Kittel–Kasuya–Yosida (RKKY) interactions. First-principles calculations reveal a larger than expected Gd magnetic moment, with the additional contribution arising from the Gd 5 d electrons. The electronic structure analysis suggests strong Gd 5 d –Fe 3 d hybridization to be the cause of this effect, rather than weak interactions between Gd and Bi. These details are of importance for understanding the magnetic response and explaining the high ordering temperature in this material.

Chemistry↗

DOE OSTI2026

Ion-Electron Coupling-Driven Redox Behavior in Metal–Organic Frameworks

Redox-active metal–organic frameworks (MOFs) have long been proposed as electronic transport platforms, yet the microscopic origin of their conductivity remains debated. A theoretical demonstration reveals charge transport in a Zn(pyrazole–naphthalene diimide (NDI)) MOF arising not from delocalized band-like states but from redox hopping between discrete linker sites. Using ab initio molecular dynamics simulations combined with electronic structure analysis, we established a direct link among electron injection, structural reorganization, and transport. Electron accumulation proceeds sequentially and site-selectively from imide and carbonyl groups of the NDI core progressively involving pyrazole N atoms at higher reduction states, through a hierarchy of redox-active sites. In contrast, Zn nodes remain essentially redox-inactive, which confirms their structural role. Density-of-states analysis corroborates a transport regime dominated by linker-centered states with evolving p-character upon reduction, resulting in dynamically reconfigured conduction networks. Real-time trajectories reveal anisotropic linker-to-linker electron transfer modulated by counterion coordination. This cooperative ion–electron regime emerges from potential energy surface collapse into a single low-barrier transition (ΔG ‡ ≈ 45 meV), where ionic and electronic motions evolve adiabatically on the same free-energy landscape. Elucidating redox conductivity in Zn(pyrazole–NDI) MOFs provides a theoretical framework for use in neuromorphic computing and related technologies.

Charge transfer↗

DOE OSTI2018

Interplay between bulk and edge-bound topological defects in a square micromagnet

A field-driven transformation of a domain pattern in a square micromagnet, defined in a thin film of La 0.7 Sr 0.3 MnO 3 , is discussed in terms of creation and annihilation of bulk vortices and edge-bound topological defects with half-integer winding numbers. The evolution of the domain pattern was mapped with soft x-ray photoemission electron microscopy and magnetic force microscopy. Micromagnetic modeling, permitting detailed analysis of the spin texture, accurately reproduces the measured domain state transformation. The simulations also helped stipulate the energy barriers associated with the creation and annihilation of the topological charges and thus to assess the stability of the domain states in this magnetic microstructure.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Relation between sampling, sensitivity and precision in strain mapping using the Geometric Phase Analysis method in Scanning Transmission Electron Microscopy

The sensitivity and the precision of the Geometric Phase Analysis (GPA) method for strain characterization is a topic widely discussed in the literature and is usually difficult to quantify. Indeed, the GPA precision is intricately linked to the resolution of the strain maps defined when masking the periodic reflections in Fourier space. In this study an additional parameter, sampling, is proposed to be analyzed regarding the precision of GPA by developing the concept of a phase noise in the GPA equations. Both experimentally and theoretically, the following article demonstrates how the precision, and the sensitivity of the GPA method is improved when using a larger pixel spacing to record an electron micrograph in Scanning Transmission Electron Microscopy (STEM). In conclusion, the counterintuitive concept of increasing the field of view to improve the GPA precision results in an extension of the application of strain characterization methods in STEM towards low deformation levels.

47 OTHER INSTRUMENTATION↗

DOE OSTI2020

Correlative electron and ion beam analysis of the electrochemical performances of LiV 3 O 8 cathode films as a function of microstructures

Degradation mechanisms in LiV 3 O 8 cathode films (~500 nm) with different initial microstructures i.e., globular nanocrystals in amorphous matrix and needle-like nanocrystals, synthesized by annealing the cathodes at 150 °C and 300 °C for 6 h are studied by Transmission Electron Microscopy (TEM) and Auger Electron Spectroscopy (AES). In addition, a unique in-situ combination of TEM and Secondary Ion Mass Spectrometry (SIMS) imaging techniques, namely Parallel Ion and Electron beam Spectrometry (PIES) is carried out to measure the 3D distribution of V and Li with nanoscale resolution. These characterization studies focus on correlating the pre- and post-cycling microstructure to observed electrochemical performance. The LiV 3 O 8 cathode film with needle-like nanocrystals (300 °C) shows a higher initial capacity but it degrades rapidly compared to the film with globular nanocrystals embedded in amorphous matrix (150 °C). We observed that LiV 3 O 8 films with needle-like nanocrystals are more susceptible to cathode decohesion and vanadium dissolution than the films with globular nanocrystals embedded in amorphous matrix, explaining the differences in their electrochemical performance. The findings from this study have relevance to the development of thin film electrode microstructures for high capacity and cyclic stability.

25 ENERGY STORAGE↗

DOE OSTI2022

Universal signal scaling in microwave impedance microscopy

Microwave impedance microscopy (MIM) is an emerging scanning probe technique that measures the local complex dielectric function using near-field microwave. Although it has made significant impacts in diverse fields, a systematic, quantitative understanding of the signal's dependence on various important design parameters is lacking. Here, we show that for a wide range of MIM implementations, given a complex tip-sample admittance change ΔΥ, the MIM signal—the amplified change in the reflected microwave amplitude—is –G · ΔΥ/2Υ 0 · η 2 · V in , where η is the ratio of the microwave voltage at the probe to the incident microwave amplitude, Y o is the system admittance, and G is the total voltage gain. For linear circuits, η is determined by the circuit design and does not depend on V in . We show that the maximum achievable signal for different designs scales with η 2 or η when limited by input power or sample perturbation, respectively. Furthermore, this universal scaling provides guidance on diverse design goals, including maximizing narrow-band signal for imaging and balancing bandwidth and signal strength for spectroscopy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

3D electron tomographic and biochemical analysis of ER, Golgi and trans Golgi network membrane systems in stimulated Venus flytrap (Dionaea muscipula) glandular cells

The insect-trapping leaves of Dionaea muscipula provide a model for studying the secretory pathway of an inducible plant secretory system. The leaf glands were induced with bovine serum albumin to secrete proteases that were characterized via zymogram activity gels over a 6-day period. The accompanying morphological changes of the endoplasmic reticulum (ER) and Golgi were analyzed using 3D electron tomography of glands preserved by high-pressure freezing/freeze substitution methods. Secretion of multiple cysteine and aspartic proteases occurred biphasically. The majority of the Golgi was organized in clusters consisting of 3–6 stacks surrounded by a cage-like system of ER cisternae. In these clusters, all Golgi stacks were oriented with their cis-most C1 cisterna facing an ER export site. The C1 Golgi cisternae varied in size and shape consistent with the hypothesis that they form de novo. Following induction, the number of ER-bound polysomes doubled, but no increase in COPII vesicles was observed. Golgi changes included a reduction in the number of cisternae per stack and a doubling of cisternal volume without increased surface area. Polysaccharide molecules that form the sticky slime cause swelling of the trans and trans Golgi network (TGN) cisternae. Peeling of the trans-most cisternae gives rise to free TGN cisternae. One day after gland stimulation, the free TGNs were frequently associated with loose groups of oriented actin-like filaments which were not seen in any other samples. These findings suggest that the secretory apparatus of resting gland cells is “overbuilt” to enable the cells to rapidly up-regulate lytic enzyme production and secretion in response to prey trapping.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2021

Electron diffraction radial distribution function analysis of amorphous boron carbide synthesized by ion beam irradiation and chemical vapor deposition

Amorphous boron carbide (a-BxC) networks consist of light elements, and their low atomic scattering factors makes structural analysis by x-ray diffraction difficult. Electron diffraction has an advantage of detecting the light elements, because of the strong interaction between the matter and electrons. In this work, we prepared a-BxC by ion beam technologies and plasma-enhanced chemical vapor deposition, and characterized their structures via atomic pair-distribution functions derived from electron diffraction intensity profiles. It was found that a pentagonal pyramid is the most favorable cluster in a-B4C generated by ion irradiation, while C—C homonuclear bonds were formed in the deposited a-B x C thin film. X-ray photoemission spectroscopy revealed that the a-BxC thin film possesses more carbon than B 4 C, which is responsible for the formation of the homonuclear bonds.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Bridging Zirconia Nodes within a Metal–Organic Framework via Catalytic Ni-Hydroxo Clusters to Form Heterobimetallic Nanowires

Metal-organic frameworks (MOFs), with their well-ordered pore networks and tunable surface chemistries, offer a versatile platform for preparing well-defined nanostructures wherein functionality such as catalysis can be incorporated. We resolved the atomic structure of Ni-oxo species deposited in the MOF NU-1000 through atomic layer deposition using local and long-range structure probes, including X-ray absorption spectroscopy, pair distribution function analysis and difference envelope density analysis, with electron microscopy imaging and computational modeling.

Environmental Molecular Sciences Laboratory↗

DOE OSTI2017

A Manufacturing Cost and Supply Chain Analysis of SiC Power Electronics Applicable to Medium-Voltage Motor Drives

Wide bandgap (WBG) semiconductor devices are increasingly being considered for use in certain power electronics applications, where they can improve efficiency, performance, footprint, and, potentially, total system cost compared to systems using traditional silicon (Si) devices. Silicon carbide (SiC) devices in particular -- which are currently more mature than other WBG devices -- are poised for growth in the coming years. Today, the manufacturing of SiC wafers is concentrated in the United States, and chip production is split roughly equally between the United States, Japan, and Europe. Established contract manufacturers located throughout Asia typically carry out manufacturing of WBG power modules. We seek to understand how global manufacturing of SiC components may evolve over time by illustrating the regional cost drivers along the supply chain and providing an overview of other factors that influence where manufacturing is sited. We conduct this analysis for a particular case study where SiC devices are used in a medium-voltage motor drive.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2018

Microstructure and Mechanical Properties of Spray-Formed 7075 Alloy During Retrogression

The mechanical properties, conductivity, microstructure, precipitation behavior and evolution process of elements and phases of spray-formed 7075 alloy during retrogression are studied by the tensile test, electric test, hardness test, transmission electron microscope (TEM), x-ray diffraction (XRD) analysis, electron-dispersive spectroscopy (EDS) and lattice parameter measurements. The results show that the mechanical properties and conductivity of the alloy can be effectively improved when treated at a suitable retrogression temperature and time. According to the TEM observations, XRD analysis, EDS and an accurate measurement of the lattice parameter, the redissolution of elements and precipitated phases can be readily observed. From the optimization selection of the RRA treatment for the 7075 alloy, the regularity of redissolution and precipitation of the elements and phases are evaluated. The ultimate tensile strength, yield strength, hardness, elongation and conductivity of the spray-formed 7075 alloy after preaging at 120 °C for 16 h, retrogression at 200 °C for 8 min and reaging at 120 °C for 24 h are 791, 736 MPa, 181 HBW, 8.5% and 22.6 MS/m, respectively.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Constraints on dark photons and axionlike particles from the SuperCDMS Soudan experiment

We present an analysis of electron recoils in cryogenic germanium detectors operated during the SuperCDMS Soudan experiment. The data are used to set new constraints on the axioelectric coupling of axion-like particles and the kinetic mixing parameter of dark photons, assuming the respective species constitutes all of the galactic dark matter. This study covers the mass range from 40 eV/$c^2$ to 500 eV/$c^2$ for both candidates, excluding previously untested parameter space for masses below ~1 keV/$c^2$. For the kinetic mixing of dark photons, values below $10^{-15}$ are reached for particle masses around 100 eV/$c^2$; for the axioelectric coupling of axion-like particles, values below $10^{-12}$ are reached for particles with masses in the range of a few-hundred eV/$c^2$.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Viscosities and working region predictions for bismuth aluminoborosilicate glasses

Bismuth aluminoborosilicate glasses were prepared using a standard melt-quench technique, and the viscosity and thermal properties were measured and analyzed. Electron microprobe analysis was used to examine glass homogeneity. Fragility was calculated based on Mauro–Yue–Ellison–Gupta–Allan model fits to the viscosity curves. The system is characterized by an open structure with high fragility (44-59). Based on microanalysis and differential scanning calorimetry results, the addition of network intermediate Al2O3 appears to mitigate both phase separation and crystallization. From thermal property data, mixture models were created to predict the glass transition temperatures and softening temperatures as functions of composition. Based on K-fold validation findings, the first-order mixture model predictions of glass transition and softening appear to approximate actual values better than models with any additional second-order terms.

Gardner, Levi↗

DOE OSTI2019

Performance of Laser-Based Electronic Devices for Structural Analysis of Amazonian Terra-Firme Forests

Tropical vegetation biomass represents a key component of the carbon stored in global forest ecosystems. Estimates of aboveground biomass commonly rely on measurements of tree size (diameter and height) and then indirectly relate, via allometric relationships and wood density, to biomass sampled from a relatively small number of harvested and weighed trees. Recently, however, novel in situ remote sensing techniques have been proposed, which may provide nondestructive alternative approaches to derive biomass estimates. Nonetheless, we still lack knowledge of the measurement uncertainties, as both the calibration and validation of estimates using different techniques and instruments requires consistent assessment of the underlying errors. To that end, we investigate different approaches estimating the tropical aboveground biomass in situ. We quantify the total and systematic errors among measurements obtained from terrestrial light detection and ranging (LiDAR), hypsometer-based trigonometry, and traditional forest inventory. We show that laser-based estimates of aboveground biomass are in good agreement (<10% measurement uncertainty) with traditional measurements. However, relative uncertainties vary among the allometric equations based on the vegetation parameters used for parameterization. We report the error metrics for measurements of tree diameter and tree height and discuss the consequences for estimated biomass. Despite methodological differences detected in this study, we conclude that laser-based electronic devices could complement conventional measurement techniques, thereby potentially improving estimates of tropical vegetation biomass.

54 ENVIRONMENTAL SCIENCES↗