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DOE OSTI2023

Measurement of femtosecond dynamics of ultrafast electron beams through terahertz compression and time-stamping

Visualizing ultrafast dynamics at the atomic scale requires time-resolved characterization with femtosecond temporal resolution. For fully relativistic electron bunch probes, existing techniques for single-shot ultrafast electron diffraction (UED) are limited by the achievable electron probe bunch length, charge, and timing jitter. We present the first experimental demonstration of dual-fed THz-driven compression and time-stamping that enables electron probes with improved temporal resolution. This technique utilizes two counter-propagating quasi-single-cycle THz pulses generated from two OH-1 organic crystals coupled into an optimized THz compressor structure. We demonstrate electron bunch compression and time-of-arrival jitter suppression by a factor of 3 paving the way toward unique opportunities for UED time-resolved measurements.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2024

Mapping charge excitations in generalized Wigner crystals

Transition metal dichalcogenide-based moiré superlattices exhibit strong electron-electron correlations, thus giving rise to strongly correlated quantum phenomena such as generalized Wigner crystal states. Evidence of Wigner crystals in transition metal dichalcogenide moire superlattices has been widely reported from various optical spectroscopy and electrical conductivity measurements, while their microscopic nature has been limited to the basic lattice structure. Theoretical studies predict that unusual quasiparticle excitations across the correlated gap between upper and lower Hubbard bands can arise due to long-range Coulomb interactions in generalized Wigner crystal states. However, the microscopic proof of such quasiparticle excitations is challenging because of the low excitation energy of the Wigner crystal. Here, in this study, we describe a scanning single-electron charging spectroscopy technique with nanometre spatial resolution and single-electron charge resolution that enables us to directly image electron and hole wavefunctions and to determine the thermodynamic gap of generalized Wigner crystal states in twisted WS 2 moiré heterostructures. High-resolution scanning single-electron charging spectroscopy combines scanning tunnelling microscopy with a monolayer graphene sensing layer, thus enabling the generation of individual electron and hole quasiparticles in generalized Wigner crystals. We show that electron and hole quasiparticles have complementary wavefunction distributions and that thermodynamic gaps of ~50 meV exist for the 1/3 and 2/3 generalized Wigner crystal states in twisted WS 2 .

36 MATERIALS SCIENCE↗

DOE OSTI2020

Electronic Population Transfer via Impulsive Stimulated X-Ray Raman Scattering with Attosecond Soft-X-Ray Pulses

Free electron lasers provide a source of X-ray pulses short enough and intense enough to drive nonlinearities in molecular systems. Impulsive interactions driven by these X-ray pulses provide a way to create and probe valence electron motions with high temporal and spatial resolution. Observing these electronic motions is crucial to understand the role of electronic coherence in chemical processes. A simple nonlinear technique for probing electronic motion, impulsive stimulated X-ray Raman scattering (ISXRS), involves a single impulsive interaction to produce a coherent superposition of electronic states. In this work, we demonstrate electronic population transfer via ISXRS using broad bandwidth (5.5 eV full width at half maximum) attosecond X-ray pulses produced by the Linac Coherent Light Source (LCLS). The impulsive excitation is resonantly enhanced by the oxygen 1s → 2π* resonance of nitric oxide (NO), and excited state neutral molecules are probed with a time-delayed UV laser pulse.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2025

Effect of stress on Laves phase precipitation in creep ruptured Grade 92 ferritic martensitic steel characterized by a novel accessible method

At high temperature conditions relevant to fossil and nuclear energy plants, Laves phase (Fe 2 X, X=Mo, W) precipitation is observed in common ferritic martensitic (FM) structural steels, with various reported effects on creep behavior. Despite being valuable metrics to correlate with mechanical properties and other precipitate phases, the volume fraction and number density of Laves phase precipitates has been difficult to quantify accurately using common techniques such as transmission electron microscopy (TEM) due to the relatively large size (∼0.25 μm) and low number density (∼10 11 cm −3 ) of Laves precipitates. Here, to address this characterization challenge, we developed and demonstrated a high-throughput and widely accessible method to quantify the volume fraction and number density of the Laves phase based on scanning electron microscope (SEM) images with a backscattered electron signal and the information depth (ID) of backscattered electrons. We applied this new technique in creep ruptured Grade 92 FM steel to study the effect of Laves phase on creep properties and determine the influence of stress on Laves phase precipitation. The quantitative accuracy of the SEM-based volume fraction and number density values was verified using synchrotron high energy X-ray diffraction and serial sectioning tomography. Stress did not significantly affect the Laves phase size or volume fraction during creep testing at 550 – 650°C and stress levels of 90 – 260 MPa (vs. unstressed conditions). Conversely, a moderate but statistically significant stress-enhanced increase in Laves phase number density, corresponding to an increase in nucleation rate, occurred during creep exposure above 110 MPa.

Creep↗

DOE OSTI2020

Improved modeling of β electronic recoils in liquid xenon using LUX calibration data

We report here methods and techniques for creating and improving a model that reproduces the scintillation and ionization response of a dual-phase liquid and gaseous xenon time-projection chamber. Starting with the recent release of the Noble Element Simulation Technique (NEST v2.0), electronic recoil data from the $\beta$ decays of ${}^3$H and ${}^{14}$C in the Large Underground Xenon (LUX) detector were used to tune the model, in addition to external data sets that allow for extrapolation beyond the LUX data-taking conditions. This paper also presents techniques used for modeling complicated temporal and spatial detector pathologies that can adversely affect data using a simplified model framework. The methods outlined in this report show an example of the robust applications possible with NEST v2.0, while also providing the final electronic recoil model and detector parameters that will used in the new analysis package, the LUX Legacy Analysis Monte Carlo Application (LLAMA), for accurate reproduction of the LUX data. As accurate background reproduction is crucial for the success of rare-event searches, such as dark matter direct detection experiments, the techniques outlined here can be used in other single-phase and dual-phase xenon detectors to assist with accurate ER background reproduction.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2026

Probing Dynamic Phase Changes in Electrochemical Systems with Cryogenic and in Situ Analytical Electron Microscopy (Final Technical Report)

In this project, we focus on the advancement of our newly developed, unique in situ and cryogenic analytical electron microscopy (AEM) techniques and the development of additional high-end capabilities to quantitatively elucidate the mechanisms of resistive state changes in solid-state electrochemical materials for non-volatile, neuromorphic memory. The objectives of the proposed research are (1) to characterize and elucidate the mechanisms by which electronic state changes occur in various solid-state devices to build guiding principles for electrochemically activated smart materials; (2) to advance our understanding of such mechanisms by coupling cryogenic and in situ techniques to control kinetics of the observed mechanisms while mitigating probe-induced damage; and (3) to utilize additional advanced techniques including electron-beam induced current and quantum mechanical simulations in order to identify the underlying fundamental science of such processes, including roles of defect formation and its effect on phase nucleation, as well as dynamics of these processes in the electrochemical systems at the nanometer scale.

25 ENERGY STORAGE↗

DOE OSTI2022

Current Status of Developing Ultrafast Mega-electron-volt Electron Microsope

Recent studies of ultrafast electron microscopy (UEM) techniques show the use of short bunches of relativistic electrons is promising for the development of a new instrument for imaging various materials. Compared to conventional electron microscopes, the main advantage of UEMs with the electron energy of a few MeV is the possibility to study thick samples. We will discuss the progress of UEM design to date, the principal challenges on the way to a high resolution, and possible methods for their mitigation including the design of low-aberration magnetic optics, RF and mechanical subsystems with high stability, and precise collimation of electrons scattered in the samples.

43 PARTICLE ACCELERATORS↗

DOE OSTI2024

MicroBooNE Electron-Neutrino Cross-Section Results

Measurement of the electron-neutrino cross-section with argon ($\nu$-Ar) is crucial for current and future neutrino experiments. Results from MicroBooNE detector, a liquid argon time projection chamber (LArTPC) based at Fermilab, provide the most extensive and precise determination of these electron-neutrino cross-sections. MicroBooNE is situated on both on-axis and off-axis beams: the Booster Neutrino Beam (BNB) and Neutrinos at the Main Injector (NuMI) beam, respectively. The background for both beams is dominated by showers from neutral pion decay, necessitating an electron-photon separation technique. In this proceeding, we review three recent electron-neutrino cross-section results from MicroBooNE using NuMI and BNB.

Guzzo, Marina [Edinburgh U.]↗

DOE OSTI2025

Microbead Encapsulation for Protection of Electronic Components

Here, this study investigates the application of microbeads as an innovative encapsulation technique to protect electronic components from harsh mechanical strain. Traditional encapsulation methods using hard epoxy provide substantial mechanical support but create thermal expansion mismatch issues, potentially leading to electronic component failure. We explore the use of finely powdered microbeads to achieve protective structures combining stiffness and energy absorption. The research focuses on key variables, including microbead size, microbead roughness, compaction of microbeads, and circuit board mounting in the encapsulation, all of which influence the encapsulation’s effectiveness. Experimental setups and testing protocols were developed to assess the performance of various microbead materials under different impact conditions. Results demonstrate that microbead encapsulation significantly reduces strain on circuit boards, minimizing the risk of damage during mechanical shocks. However, challenges remain, such as optimizing microbead characteristics and modeling their behavior within large-scale circuit board assemblies. Despite these challenges, the findings suggest that microbead encapsulation offers a promising alternative to conventional methods, enhancing the durability and reliability of electronic components in high-stress environments.

42 ENGINEERING↗

DOE OSTI2021

Excited states in variational Monte Carlo using a penalty method

Here, in this article, the authors present a technique using variational Monte Carlo to solve for excited states of electronic systems. This technique is based on enforcing orthogonality to lower energy states, which results in a simple variational principle for the excited states. Energy optimization is then used to solve for the excited states. This technique is applied to the well-characterized benzene molecule, in which ~10 000 parameters are optimized for the first 12 excited states. Agreement within ~0.2 eV is obtained with higher scaling coupled cluster methods; small disagreements with experiment are likely due to vibrational effects.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Determination of the mean energy of fast electron losses and anisotropies through thick-target emission on WEST

Abstract A new method to obtain the mean energy of fast electron losses in fusion plasmas using a versatile multi-energy hard x-ray (HXR) detector is presented. The method is based on measuring the thick-target emission of tungsten in the divertor region produced by fast electron losses interacting with the target and modeling the tungsten spectra by a Monte Carlo code which simulates the interaction between a beam of electrons and a solid target. The mean energy of the fast electron losses is determined through the comparison between the experimental and synthetic emission. The results show that fast electron losses during lower hybrid current drive discharges at WEST have a mean energy of 90–140 keV and represent only 2% of the total heat flux at the target. Additionally, anisotropic HXR emission has been detected for the first time at the WEST core and edge plasma, with opposite directions. It is due to the forward-peak emission of two distinctive populations of fast electrons: co-current fast electrons in the core and counter-current fast electron losses at the inner strike point. In view of future experiments like ITER where electron cyclotron current drive will generate a fast electron population, this technique could serve as a real-time monitor of fast electron losses and eventually feed an actuator on the current drive generation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Biopolymer‐assisted Synthesis of P‐doped TiO 2 Nanoparticles for High‐performance Lithium‐ion Batteries: A Comprehensive Study

Abstract TiO 2 material has gained significant attention for large‐scale energy storage due to its abundant, low‐cost, and environmentally friendly properties, as well as the availability of various nanostructures. Phosphorus doping has been established as an effective technique for improving electronic conductivity and managing the slow ionic diffusion kinetics of TiO 2 . In this study, non‐doped and phosphorus doped TiO 2 materials were synthesized using sodium alginate biopolymer as chelating agent. The prepared materials were evaluated as anode materials for lithium‐ion batteries (LIBs). The electrodes exhibit remarkable electrochemical performance, including a high reversible capacity of 235 mAh g −1 at 0.1 C and excellent first coulombic efficiency of 99 %. An integrated approach, combining operando XRD and ex‐situ XAS, comprehensively investigates the relationship between phosphorus doping, material structure, and electrochemical performance, reinforced by analytical tools and first principles calculations. Furthermore, a full cell was designed using 2 %P‐doped TiO 2 anode and LiFePO 4 cathode. The output voltage was about 1.6 V with high initial specific capacity of 148 mAh g −1 , high rate‐capability of 120 mAh g −1 at 1 C, and high‐capacity retention of 96 % after 1000 cycles at 1 C.

El Halya, Nabil↗

DOE OSTI2020

Reconstruction and uncertainty quantification of lattice Hamiltonian model parameters from observations of microscopic degrees of freedom

The emergence of scanning probe and electron beam imaging techniques has allowed quantitative studies of atomic structure and minute details of electronic and vibrational structure on the level of individual atomic units. These microscopic descriptors, in turn, can be associated with local symmetry breaking phenomena, representing the stochastic manifestation of the underpinning generative physical model. In this work, we explore the reconstruction of exchange integrals in the Hamiltonian for a lattice model with two competing interactions from observations of microscopic degrees of freedom and establish the uncertainties and reliability of such analysis in a broad parameter-temperature space. In contrast to other approaches, we specifically specify a loss function inherent to thermodynamic systems and utilize it to estimate uncertainty in simulated realizations of different models. As an ancillary task, we develop a machine learning approach based on histogram clustering to predict phase diagrams efficiently using a reduced descriptor space. We further demonstrate that reconstruction is possible well above the phase transition and in the regions of parameter space when the macroscopic ground state of the system is poorly defined due to frustrated interactions. This suggests that this approach can be applied to the traditionally complex problems of condensed matter physics such as ferroelectric relaxors and morphotropic phase boundary systems, spin and cluster glasses, and quantum systems once the local descriptors linked to the relevant physical behaviors are known.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Enabling phase quantification of anhydrous cements via Raman imaging

The phase composition of Portland cements is typically determined using conventional techniques like X-ray Diffraction (XRD) Rietveld analysis, optical microscopy point counting, and electron microscopy. However, these techniques have several limitations that may affect their accuracy in certain sample-specific scenarios. Here, we report a highly accurate phase quantification of 11 different types of commercial, anhydrous cements using a new and complementary technique: Raman imaging. Specifically, for the 4 principal phases, composition from our extensive data (250,000 Raman spectra per sample, error < 0.71%) and those obtained from XRD Rietveld and supplier data have high coefficients of determination (R{sup 2} > 0.98, mean deviation <2%). Additionally, we also quantify 8 secondary phases present in cement clinkers (gypsum, anhydrite, bassanite, syngenite, dolomite, calcite, quartz, and portlandite) with a high degree of confidence, thereby demonstrating that Raman imaging is a highly versatile tool for anhydrous phase quantification in a broad variety of cements.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Bayesian inference of electron density and ion temperature profiles from neutral beam and halo Balmer- α emission at Wendelstein 7-X

By employing Bayesian inference techniques, the full electron density profile from the plasma core to the edge of Wendelstein 7-X (W7-X) is inferred solely from neutral hydrogen beam and halo Balmer- α (H α ) emission data. The halo is a cloud of neutrals forming in the vicinity of the injected neutral beam due to multiple charge exchange reactions. W7-X is equipped with several neutral hydrogen beam heating sources and an H α spectroscopy system that views these sources from different angles and penetration depths in the plasma. As the beam and halo emission form complex spectra for each spatial point that are non-linearly dependent on the plasma density profile and other parameters, a complete model from the neutral beam injection and halo formation through to the spectroscopic measurements is required. The model is used here to infer electron density profiles for a range of common W7-X plasma scenarios. The inferred profiles show good agreement with profiles determined by the Thomson scattering and interferometry diagnostics across a broad range of absolute densities without any changes to the input or fitting parameters. The time evolution of the density profile in a discharge with continuous core density peaking is successfully reconstructed, demonstrating sufficient spatial resolution to infer strongly shaped profiles. Furthermore, it is shown as a proof of concept that the model is also able to infer the main ion temperature profile using the same data set.

forward modeling↗

DOE OSTI2025

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↗

DOE OSTI2020

Source size measurement options for low-emittance light sources

Radiation-based techniques for measuring electron source sizes are widely used as emittance diagnostics at existing synchrotron sources. Three of these techniques, namely, pinhole imaging, double-slit interferometry, and a K-edge filter-based beam position and size monitor system (ps-BPM), are evaluated for measuring source sizes at low-emittance storage rings. Each technique is reviewed with a detailed system description, design optimization, and practical considerations targeted for small source sizes. Pinhole imaging has the simplest setup and gives the beam profile in both transverse dimensions but with limited resolution. Double-slit interferometry has the highest resolution but with a limited detectable size range. The ps-BPM system shows reasonable resolution for monitoring small source sizes and divergence and can give real-time information of the source position and angle. New facilities may consider an integrated system that combines some or all of these techniques.

43 PARTICLE ACCELERATORS↗

DOE OSTI2021

IMS Rapid Response FY21 Summary Report for: Integrating Patterned Probes with Four-Dimensional Scanning Transmission Electron Microscopy for Unrivaled Crystallographic Structure Determination in Nanomaterials

The initial goal of our 4-dimensional scanning transmission electron microscopy (4D-STEM)-based project was to develop strain resolution two orders of magnitude better than what is now currently possible with electron-based scattering techniques, all while collecting scattering information from 7 different tilt axes at one time [multi-beam electron diffraction (MBED)1 ] through the development of a new electron probe-forming aperture with non-circular features (patterned probes 2 ). We set out to accomplish this through a collaboration with Drs. Colin Ophus and Ben Savitsky at Lawrence Berkeley Laboratory (they are the world-leading experts in developing the complex computational codes required to perform orientation analysis and quantitative strain mapping on our 4D-STEM data sets. We are motivated to invest in this area as it will be the only technique sensitive enough to perform three- dimensional automated crystallographic orientation mapping (ACOM) and strain mapping for materials exposed to external stimulus (a focus of our larger efforts).

36 MATERIALS SCIENCE↗