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At least 37 records · Page 2

Pattern-enhanced Resonant Soft X-ray Scattering for Operando monitoring of electrochemical solid-liquid interfaces

Unveiling interfaces at sub-nanometer scales is essential for advancing the understanding of complex chemical transformations. However, characterizing solid-liquid interfaces with high dimensional sensitivity and temporal resolution remains challenging, due to their dynamic nature and inaccessibility by conventional probes. Here we present an approach, Pattern-enhanced Resonant Soft X-ray Scattering, to overcome the challenges. Rooted in a “sample-as-optics” philosophy, this technique utilizes precisely engineered line-grating nanopatterns to modulate near-field X-ray illumination, coherently enhancing scattering signals from the line-gratings. We implement the method using Ni line-grating nanopatterns in electrochemical water oxidation. The periodic nanostructures serve as diffractive optical elements to reveal the Ni oxidation gradients and structural dynamics at the electrode-electrolyte interfaces. Finite-element simulations corroborate the observed trends by modeling variations in compositions and structures during electrocatalysis. Through integrating advanced sample design with coherent wave nature of soft X-rays, our approach opens accessible pathways to operando exploring chemical evolution and sub-nanometer dimensional variations simultaneously in electrochemical systems. This non-destructive method is efficient and element-specific, making it valuable for probing chemical and dimensional dynamics with appropriate modeling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Quantifying uncertainty in uranium concentration measurements via K-edge densitometry

This study quantifies the uncertainty in uranium concentration predictions of fluoride and chloride-based salts within a steel pipe using K-edge densitometry. Modeling and simulation was conducted with the Monte Carlo N-Particle Transport (MCNP) code. The quality of of this technique’s prediction in a pipe requires proper characterization of the pipe’s thickness, which is dependent on the source size and axial offset from the pipe centerline. The thickness was determined as either the center-line thickness seen by the X-ray source or an average value determined through random sampling. Generally, the predicted concentrations were slightly better at lower offset with the random sampling thickness and using the center-line thickness for the highest offsets. For a line-beam source and varying axial offsets, the relative error of concentration was within 1% of the true value but uncertainty increased by 2 orders of magnitude. Similarly, for no axial offset, the relative error was significantly less than 1% while no trend for uncertainty was found. However, at the largest possible offset for a given source size, the concentrations become erroneous and greater than the allowable 1% relative error. Furthermore, high offsets tended to increase the variance of the transmission spectra by 3 orders of magnitude.

Characterization and Analytical Technique

A quantitative comparison of the fingerprint of twinned microstructures through surface and three-dimensional techniques

Assessing the fingerprint of a material’s microstructure is key for supporting materials design. With the emergence of a wide range of 3D characterization techniques, it is critical to understand the main differences in fingerprints reconstructed from 2D and 3D datasets. To this end, we introduce a graph-based microstructure reconstruction framework that enables structural comparisons of twin domain networks in high purity Ti using 3D and 2D electron backscatter diffraction. Insights into the structure of the twin networks are facilitated by combining statistical analysis of twin crystallography with visual and graphical analysis of the novel graph abstractions of the twins. We demonstrate that compared to 3D reconstructions, conventional 2D views of twinning miss key aspects of the microstructure including the high interconnectivity of domains into networks that span the full reconstruction volume. The reduced cross-grain and in-grain twin connectivity typically observed in 2D has notable implications on our understanding of how twinning mediates the plastic response of microstructures and how twin networks evolve. It is thus clear that 3D characterization is critical for accurately inferring both twin network morphologies as well as the key unit processes facilitating network formation.

36 MATERIALS SCIENCE

Detecting isolated resonance curves using fixed frequency voltage control tests

Isolated resonance curves, or isolas, are resonance branches of the harmonically forced system that exist separately from the main nonlinear forced response curve, leading to excessive vibrations. Traditional stepped or swept sine simulations and tests rely on continuation along the frequency parameter, typically resulting in a jump phenomenon along the primary resonance branch, prior to the disconnected isola. The main objective of this research is to propose an approach to identify isolated resonance curves by performing continuation along the input amplitude that initializes the response from a low-amplitude solution in the linear regime. Furthermore, this is achieved with the open-loop fixed frequency voltage control method that continues along the shaker voltage parameter and measures the so-called S-curves, which are theoretically a continuous solution branch that connect to the isola. The methodology is demonstrated on a fixture-wing-pylon assembly with a vibro-impact nonlinearity localized in a pylon subcomponent attachment. Multi-harmonic balance simulations are deployed to compute both the nonlinear forced response curves and S-curves to demonstrate the isola detection strategy on a reduced-order finite element model of the nonlinear system. Swept sine and fixed frequency voltage control tests are then conducted on the physical structure to demonstrate the isola detection experimentally, revealing the existence of the large amplitude vibrations that are undetected in the forces levels and frequencies measured with traditional frequency sweeping.

Characterization and Analytical Technique

Transforming jet flavour tagging at ATLAS

Jet flavour tagging enables the identification of jets originating from heavy-flavour quarks in proton–proton collisions at the Large Hadron Collider, playing a critical role in its physics programmes. This paper presents GN2, a transformer-based flavour tagging algorithm deployed by the ATLAS Collaboration that represents a different methodology compared to previous approaches. Designed to classify jets based on the flavour of their constituent particles, GN2 processes low-level tracking information in an end-to-end architecture and incorporates physics-informed auxiliary training objectives to enhance both interpretability and performance. Its performance is validated in both simulation and collision data. The measured c-jet (light-jet) rejection in data is improved by a factor of 3.5 (1.8) for a 70% b-jet tagging efficiency, compared to the previous algorithm. GN2 provides substantial benefits for physics analyses involving heavy-flavour jets, such as measurements of Higgs boson pair production and the couplings of bottom and charm quarks to the Higgs boson, and demonstrates the impact of advanced machine learning methods in experimental particle physics.

Characterization and analytical techniques

Formation, chemical evolution and solidification of the dense liquid phase of calcium (bi)carbonate

Metal carbonates, which are ubiquitous in the near-surface mineral record, are a major product of biomineralizing organisms and serve as important targets for capturing anthropogenic CO 2 emissions. However, pathways of carbonate mineralization typically diverge from classical predictions due to the involvement of disordered precursors, such as the dense liquid phase (DLP), yet little is known about DLP formation or solidification processes. Using in situ methods we report that a highly hydrated bicarbonate DLP forms via liquid–liquid phase separation and transforms into hollow hydrated amorphous CaCO 3 particles. Acidic proteins and polymers extend DLP lifetimes while leaving the pathway and chemistry unchanged. Molecular simulations suggest that the DLP forms via direct condensation of solvated Ca 2+ •(HCO 3 – ) 2 complexes that react due to proximity effects in the confined DLP droplets. Furthermore, our findings provide insight into CaCO 3 nucleation that is mediated by liquid–liquid phase separation, advancing the ability to direct carbonate mineralization and elucidating an often-proposed complex pathway of biomineralization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

The structure of liquid carbon elucidated by in situ X-ray diffraction

Carbon has a central role in biology and organic chemistry, and its solid allotropes provide the basis of much of our modern technology. However, the liquid form of carbon remains nearly uncharted, and the structure of liquid carbon and most of its physical properties are essentially unknown. But liquid carbon is relevant for modelling planetary interiors and the atmospheres of white dwarfs, as an intermediate state for the synthesis of advanced carbon materials, inertial confinement fusion implosions, hypervelocity impact events on carbon materials and our general understanding of structured fluids at extreme conditions. Here we present a precise structure measurement of liquid carbon at pressures of around 1 million atmospheres obtained by in situ X-ray diffraction at an X-ray free-electron laser. Our results show a complex fluid with transient bonding and approximately four nearest neighbours on average, in agreement with quantum molecular dynamics simulations. The obtained data substantiate the understanding of the liquid state of one of the most abundant elements in the universe and can test models of the melting line. The demonstrated experimental abilities open the path to performing similar studies of the structure of liquids composed of light elements at extreme conditions.

74 ATOMIC AND MOLECULAR PHYSICS

LumaCam: a novel class of position-sensitive event mode particle detectors using scintillator screens

A new type of position-sensitive detectors is gaining attention in the neutron community. They are scintillator based detectors that detect the scintillation light on an individual photon basis via an image intensifier and a fast image sensor. Their readout operates in event mode i.e. it produces information about individual neutron interactions, reconstructed from the sensor data, thus enabling to achieve superior spatial and temporal resolutions compared to regular detectors. Although the development of current detectors is focused on neutrons, the concept is also applicable to the detection of other particles such as high-energy photons. This document provides a description on how these detectors are built, how they operate, and what their characteristics are. An example of a detector implementation based on a Timepix3 chip is described to illustrate the detector concept. This includes a detailed description of the algorithm that reconstructs the neutron interactions from the sensor data, one of the core components that sets it apart from established scintillator-based imaging detectors. Energy-resolved epithermal neutron radiography was performed at the ISIS EMMA beamline with this detector, illustrating some of the fundamental differences in the data that can be produced with the new type of detector compared to more established types of scintillator based neutron detectors. The term LumaCam is proposed to refer to this new class of position-sensitive event-mode detectors.

47 OTHER INSTRUMENTATION

Creation and characterization of warm dense matter isochorically heated by an intense laser-driven proton beam to temperatures exceeding 100 eV

The warm dense matter (WDM) is an exotic state of matter encountered in inertial confinement implosions for fusion energy, as well as the interiors of giant planets like Jupiter, brown dwarfs, the atmospheres of white dwarfs, neutron star crusts, and newly discovered exo-planets. One efficient way to create WDM is to use protons accelerated by a high-intensity short-pulse laser to isochorically heat dense samples to WDM states. Despite its importance, direct temperature measurements within WDM targets are scarce. This study utilizes an intense proton beam generated by the kilojoule EP laser further focused and guided by a curved foil and cone structure to efficiently heat a thin copper sample. A high-resolution streaked spectrometer tuned to copper K α fluorescence lines provided bulk temperature measurements every ~2 ps, revealing temperatures exceeding 100 eV in under 50 ps. Particle-in-cell simulations of proton transport and energy deposition closely matched the observed heating dynamics, including transverse temperature gradients revealed by the broadening of K α lines.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY

Time-domain thermoreflectance

Time-domain thermoreflectance (TDTR) has been instrumental in measuring the heat transfer properties of bulk and nanostructured materials over the past two decades. In this Primer, we describe the optical and thermal aspects of TDTR, with an in-depth discussion on the theory, apparatus design and implementation. We present examples that illustrate the ability of TDTR to measure thermal conductivity tensors, thermal conductance across material interfaces, and volumetric heat capacity of thin films, 2D materials and bulk materials. The ability of TDTR to spatially resolve thermal properties is useful for studying heterogeneous material systems, such as materials processed in or subjected to extreme environments. We consider current limitations of pump–probe metrologies and discuss recent advancements of TDTR, such as time-resolved magneto-optic Kerr effect (TR-MOKE), beam-offset TDTR/TR-MOKE, steady-state thermoreflectance, frequency-domain thermoreflectance and laser-flash TDTR. Lastly, we present an outlook on anticipated technological developments to further expand the ability of TDTR to measure nanoscale thermal properties.

42 ENGINEERING

Complete Initial Studies in Microstructural Studies of Nuclear Graphite

Nuclear graphite is a critical material for the performance and safety of high-temperature reactors, making its study essential for the successful deployment of next-generation reactors in the United States. During the past year, Oak Ridge National Laboratory (ORNL) has contributed extensively to advancing the understanding of nuclear graphite’s properties, behavior, and applications; particular focus has been given to irradiation effects, oxidation mechanisms, thermal and mechanical performance, and long-term stability under reactor conditions. This report provides an update on the ongoing publications being prepared at ORNL. These studies are collectively intended to build a comprehensive knowledge base on nuclear graphite. The studies focus on key aspects such as microstructural characterization, oxidation behavior, advanced analytical techniques, molten salt infiltration, technique development, and billet-to-billet variability. By summarizing the progress of these publications, this report outlines ORNL’s contributions to the field, identifies knowledge gaps, and proposes future research directions. The findings presented in these studies will help enhance the understanding of nuclear graphite’s behavior, support the qualification of nuclear graphite materials, further the development of new techniques and guidelines for using microscopy techniques, and improve reactor safety and performance.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Interfaces in polymer, ceramic, and metal matrix composites; Proceedings of the Second International Conference on Composite Interfaces (ICCI-II), Cleveland, OH, June 13-17, 1988

The present conference on interfacial factors in advanced composite materials discusses such topics in their development status and properties as silane coupling, the electrochemical and plasma-surface treatment of carbon fibers, fiber surface-analytical techniques, polymer molecular scale characterization by atom-probe field-ion microscopy, the study of carbon fiber-epoxy resin interface interactions by means of labeling techniques, and the surface tailoring of SiC by ion implantation. Also discussed are developments in laser light-scattered photoelasticity, microstructural evolutions under heat treatment and radiation damage, TEM for composites, the interfaces of carbon fiber-reinforced Al composites, the influence of the interface on macroscopic composite properties, and the status of the theoretical understanding of composite interfaces.

Ishida, Hatsuo

LDEF polymeric materials: A summary of Langley characterization

The NASA Long Duration Exposure Facility (LDEF) enabled the exposure of a wide variety of materials to the low earth orbit (LEO) environment. This paper provides a summary of research conducted at the Langley Research Center into the response of selected LDEF polymers to this environment. Materials examined include graphite fiber reinforced epoxy, polysulfone, and additional polyimide matrix composites, films of FEP Teflon, Kapton, several experimental high performance polyimides, and films of more traditional polymers such as poly(vinyl toluene) and polystyrene. Exposure duration was either 10 months or 5.8 years. Flight and control specimens were characterized by a number of analytical techniques including ultraviolet-visible and infrared spectroscopy, thermal analysis, scanning electron and scanning tunneling microscopy, x-ray photoelectron spectroscopy, and, in some instances, selected solution property measurements. Characterized effects were found to be primarily surface phenomena. These effects included atomic oxygen-induced erosion of unprotected surfaces and ultraviolet-induced discoloration and changes in selected molecular level parameters. No gross changes in molecular structure or glass transition temperature were noted. The intent of this characterization is to increase our fundamental knowledge of space environmental effects as an aid in developing new and improved polymers for space application. A secondary objective is to develop benchmarks to enhance our methodology for the ground-based simulation of environmental effects so that polymer performance in space can be more reliably predicted.

Young, Philip R.

Marine Algae Polysaccharides: An Overview of Characterization Techniques for Structural and Molecular Elucidation

Polysaccharides make up a large portion of the organic material from and in marine organisms. However, their structural characterization is often overlooked due to their complexity. With many high-value applications and unique bioactivities resulting from the polysaccharides’ complex and heterogeneous structures, dedicated analytical efforts become important to achieve structural elucidation. Because algae represent the largest marine resource of polysaccharides, the majority of the discussion is focused on well-known algae-based hydrocolloid polymers. The native environment of marine polysaccharides presents challenges to many conventional analytical techniques necessitating novel methodologies. We aim to deliver a review of the current state of the art in polysaccharide characterization, focused on capabilities as well as limitations in the context of marine environments. This review covers the extraction and isolation of marine polysaccharides, in addition to characterizations from monosaccharides to secondary and tertiary structures, highlighting a suite of analytical techniques.

09 BIOMASS FUELS

Real-time neutron multiplicity and source localization for criticality safety during fuel debris removal

Advancing neutron detection and analysis techniques for complex radiation environments is an ongoing focus in nuclear instrumentation and monitoring. This proposal presents research and development of a generalized real-time neutron monitoring and analysis system, applicable to any detector capable of producing time-tagged neutron count data. While the work is demonstrated using the Neutron Multiplication Analysis Detector (NoMAD), a modular 15-tube helium-3 (He-3) array, due to its availability, spatial resolution, and flexible deployment, the methods developed are extensible to other systems, including organic scintillators and fast digital detectors. This research investigates two complementary analytical techniques for real-time characterization of neutron emitting sources: neutron multiplicity estimation based on the Hage-Cifarelli formalism and spatial localization using supervised machine learning applied to spatial count rate patterns. These methods are designed to operate under dynamic, evolving conditions such as fuel debris retrieval or reactor startup, where neutron-emitting material geometries may be partially unknown or changing over time. By integrating statistical neutron emission data with spatial localization, this research aims to develop and evaluate methods for real time neutron monitoring, source characterization, and material verification. Key contributions include implementation of a low-latency data pipeline for continuous neutron multiplicity analysis, development and validation of machine learning models for spatial inference, and experimental evaluation of system performance under variable measurement conditions. The outcomes are intended to support applications in nuclear safeguards, verification, emergency response, and reactor startup.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

Tribological evaluation and analysis of coating materials

A physical characterization of coating materials by analytical techniques such as XPS, AES, ellipsometry, and nuclear reaction analysis can contribute to the understanding of adhesion and friction of the coatings and can partially predict the tribological properties of the coatings. This two-part paper describes the tribological properties and physical characteristics of (1) diamondlike carbon (DLC) films and (2) silicon nitride (SiN(x)) films. Emphasis is to relate plasma deposition conditions to the film chemistry and composition and to the adhesion and friction of the films. With the DLC films, the higher the plasma deposition power, the less the hydrogen concentration and the greater the film density and the hardness. The friction behavior of DLC films deposited at higher deposition powers (200 to 300 W) is similar to that of bulk diamond. Even in a vacuum, the DLC films effectively lubricate ceramic surfaces (Si3N4) at temperatures to 500 C. With SiN(x) films, the silicon to nitrogen ratios and the amount of amorphous silicon depend on deposition frequency. The presence of rich amorphous silicon in the high-frequency plasma-deposited SiN(x) films increases their adhesion and friction above 500 C in vacuum.

Miyoshi, Kazuhisa

Resin transfer molding of textile preforms for aircraft structural applications

The NASA LaRC is conducting and supporting research to develop cost-effective fabrication methods that are applicable to primary composite aircraft structures. One of the most promising fabrication methods that has evolved is resin transfer molding (RTM) of dry textile material forms. RTM has been used for many years for secondary structures, but has received increased emphasis because it is an excellent method for applying resin to damage-tolerant textile preforms at low cost. Textile preforms based on processes such as weaving, braiding, knitting, stitching, and combinations of these have been shown to offer significant improvements in damage tolerance compared to laminated tape composites. The use of low-cost resins combined with textile preforms could provide a major breakthrough in achieving cost-effective composite aircraft structures. RTM uses resin in its lowest cost form, and storage and spoilage costs are minimal. Near net shape textile preforms are expected to be cost-effective because automated machines can be used to produce the preforms, post-cure operations such as machining and fastening are minimized, and material scrap rate may be reduced in comparison with traditional prepreg molding. The purpose of this paper is to discuss experimental and analytical techniques that are under development at NASA Langley to aid the engineer in developing RTM processes for airframe structural elements. Included are experimental techniques to characterize preform and resin behavior and analytical methods that were developed to predict resin flow and cure kinetics.

Hasko, Gregory H.