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At least 343 records · Page 19

All sources NASA NTRS DOE OSTI

DOE OSTI2022

High precision real-time insertion device and monochromator synchronization at NSLS-II

We report that insertion devices have become the dominant photon source at synchrotron and free electron laser light source facilities the world over. Undulators, characterized by their small deflection parameter, exhibit a high degree of constructive interference in photon production from high energy charged particle beams leading to very high photon rates at specific harmonics of the fundamental frequency with relatively narrow spectral widths. Spectroscopic measurements of interest typically span several of these harmonic widths, which requires precision adjustment of an undulator’s magnetic gap to maintain peak flux within the much narrower bandwidth of a beamline monochromator at the desired energy. High precision insertion device controls are developed at NSLS-II including real-time linked control of monochromator hardware allowing for fast, high precision, hardware triggered, spectroscopic measurements. Furthermore, this fast fly scan method is described, compared statistically for self consistency, and shown to be far superior in both efficiency and accuracy as compared to standard step scan measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Synthesis and Characterization of Lignin-grafted-poly(ε-caprolactone) from Different Biomass Sources

Modification of lignin with poly(ε-caprolactone) is a promising approach to valorize industrial low-value lignins and to advance the bioeconomy. We have synthesized lignin grafted poly(ε-caprolactone) (lignin-g-PCL) copolymers via ring-opening polymerization of ε-caprolactone with different types of lignins of varying botanical sources (G-type pine lignin, S/G-type poplar lignin, and C-type Vanilla seeds lignin) and lignin extraction methods (Kraft and ethanol organosolv pulping). The lignin-g-PCL copolymer showed remarkably improved compatibility and dispersion in acetone, chloroform, and toluene in comparison to non-modified lignins. The structure and thermal properties of the lignin-g-PCL were investigated using Fourier-transform infrared spectroscopy (FTIR), 31 P nuclear magnetic resonance (NMR), 2D heteronuclear single quantum correlation (HSQC) NMR, gel permeation chromatography (GPC), and differential scanning calorimetry (DSC). Furthermore, we have found that all the technical lignins were reactive to the copolymerization reaction regardless of their plant source and isolation methods. The molecular weights of the synthesized lignin-g-PCL copolymers were positively correlated with the content of aliphatic lignin hydroxyls, suggesting that the copolymerization reaction tends to occur preferentially at the aliphatic hydroxyls rather than the phenolic hydroxyls of lignin. Thermal analyses of the lignin-g-PCL copolymers were studied, and in general, a reduction of melting temperature and crystallinity percentage in comparison to the neat PCL was observed. However, the thermal behavior of lignin-g-PCL copolymers varied depending on the lignin feedstocks employed in the copolymerization reaction.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

Challenges for density functional theory in simulating metal–metal singlet bonding: A case study of dimerized VO2

VO2 is renowned for its electric transition from an insulating monoclinic (M1) phase, characterized by V–V dimerized structures, to a metallic rutile (R) phase above 340 K. This transition is accompanied by a magnetic change: the M1 phase exhibits a non-magnetic spin-singlet state, while the R phase exhibits a state with local magnetic moments. Simultaneous simulation of the structural, electric, and magnetic properties of this compound is of fundamental importance, but the M1 phase alone has posed a significant challenge to the density functional theory (DFT). In this study, we show none of the commonly used DFT functionals, including those combined with on-site Hubbard U to treat 3d electrons better, can accurately predict the V–V dimer length. The spin-restricted method tends to overestimate the strength of the V–V bonds, resulting in a small V–V bond length. Conversely, the spin-symmetry-breaking method exhibits the opposite trends. Each of these two bond-calculation methods underscores one of the two contentious mechanisms, i.e., Peierls lattice distortion or Mott localization due to electron–electron repulsion, involved in the metal–insulator transition in VO2. To elucidate the challenges encountered in DFT, we also employ an effective Hamiltonian that integrates one-dimensional magnetic sites, thereby revealing the inherent difficulties linked with the DFT computations.

Chemistry↗

DOE OSTI2026

Design and Validation of a Cryogenic Dilatometer

This project focuses on the design and development of a cryogenic dilatometer capable of measuring the thermal expansion of materials at extremely low temperatures. Understanding how materials change dimension with temperature is critical for applications involving cryogenic environments, particularly laminated systems housing superconducting magnets, where small dimensional changes can significantly affect performance and reliability. To address this, a dilatometer system was designed to operate within a liquid nitrogen environment while accurately measuring displacements caused by thermal contraction. The purpose of this device is to determine the coefficient of thermal expansion (CTE) of a material. The design process involved defining functional requirements, developing mechanical and thermal concepts for the measurement apparatus, selecting appropriate materials compatible with cryogenic temperatures, and integrating sensors capable of detecting small dimensional changes. The resulting system aims to provide a practical and repeatable method for evaluating material thermal expansion at cryogenic temperatures, supporting research into composite use in superconducting applications that require accurate characterization of material behavior in low-temperature environments.

Schmitt, Nicholas [Northern Illinois U.]↗

DOE OSTI2020

DNA-assembled superconducting 3D nanoscale architectures

Studies of nanoscale superconducting structures have revealed various physical phenomena and led to the development of a wide range of applications. Most of these studies concentrated on one- and two-dimensional structures due to the lack of approaches for creation of fully engineered three-dimensional (3D) nanostructures. Here, we present a ‘bottom-up’ method to create 3D superconducting nanostructures with prescribed multiscale organization using DNA-based self-assembly methods. We assemble 3D DNA superlattices from octahedral DNA frames with incorporated nanoparticles, through connecting frames at their vertices, which result in cubic superlattices with a 48 nm unit cell. The superconductive superlattice is formed by converting a DNA superlattice first into highly-structured 3D silica scaffold, to turn it from a soft and liquid-environment dependent macromolecular construction into a solid structure, following by its coating with superconducting niobium (Nb). Through low-temperature electrical characterization we demonstrate that this process creates 3D arrays of Josephson junctions. This approach may be utilized in development of a variety of applications such as 3D Superconducting Quantum interference Devices (SQUIDs) for measurement of the magnetic field vector, highly sensitive Superconducting Quantum Interference Filters (SQIFs), and parametric amplifiers for quantum information systems.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2023

Deuteron off-resonance rotating frame relaxation for the characterization of slow motions in rotating and static solid-state proteins

Here, we demonstrate the feasibility of deuterium solid-state NMR off-resonance rotating frame relaxation measurements for studies of slow motions in biomolecular solids. The pulse sequence, which includes adiabatic pulses for magnetization alignment, is illustrated for static and magic-angle spinning conditions away from rotary resonances. We apply the measurements for three systems with selective deuterium labels at methyl groups: a) a model compound, Fluorenylmethyloxycarbonyl methionine-D 3 amino acid, for which the principles of the measurements and corresponding motional modeling based on rotameric interconversions are demonstrated; b) amyloid-β 1-40 fibrils labeled at a single alanine methyl group located in the disordered N-terminal domain. This system has been extensively studied in prior work and here serves as a test of the method for complex biological systems. The essential features of the dynamics consist of large-scale rearrangements of the disordered N-terminal domain and the conformational exchange between the free and bound forms of the domain, the latter one due to transient interactions with the structured core of the fibrils. and c) a 15-residue helical peptide which belongs to the predicted α-helical domain near the N-terminus of apolipoprotein B. The peptide is solvated with triolein and incorporates a selectively labeled leucine methyl groups. The method permits model refinement, indicating rotameric interconversions with a distribution of rate constants.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2000

Characterization of Electronic Materials HgZnSe and HgZnTe Using Innovative and Conventional Techniques

HgZnSe and HgZnTe are electronic materials of interest for potential IR detector and focal plane array applications due to their improved strength and compositional stability over HgCdTe, but they are difficult to grow on Earth and to fully characterize. Conventional contact methods of characterization, such as Hall and van der Paw, although adequate for many situations are typically labor intensive and not entirely suitable where only very small samples are available. To adequately characterize and compare properties of electronic materials grown in low earth orbit with those grown on Earth, innovative techniques are needed that complement existing methods. This paper describes the implementation and test results of a unique non-contact method of characterizing uniformity, mobility, and carrier concentration together with results from conventional methods applied to HgZnSe and HgZnTe. The innovative method has advantages over conventional contact methods since it circumvents problems of possible contamination from alloying electrical contacts to a sample and also has the capability to map a sample. Non- destructive mapping, the determination of the carrier concentration and mobility at each place on a sample, provides a means to quantitatively compare, at high spatial resolution, effects of microgravity on electronic properties and uniformity of electronic materials grown in low-Earth orbit with Earth grown materials. The mapping technique described here uses a 1mm diameter polarized beam of radiation to probe the sample. Activation of a magnetic field, in which the sample is placed, causes the plane of polarization of the probe beam to rotate. This Faraday rotation is a function of the free carrier concentration and the band parameters of the material. Maps of carrier concentration, mobility, and transmission generated from measurements of the Faraday rotation angles over the temperature range from 300K to 77K will be presented. New information on band parameters, obtained by combining results from conventional Hall measurements of the free carrier concentration with Faraday rotation measurements, will also be presented. One example of how this type of information was derived is illustrated in the following figure which shows Faraday rotation vs wavelength modeled for Hg(l-x)ZnxSe at a temperature of 300K and x=0.07. The plasma contribution, total Faraday rotation, and interband contribution to the Faraday rotation, are designated in the Figure as del(p), FR tot, and del(i) respectively. Experimentally measured values of FR tot, each indicated by + , agree acceptably well with the model at the probe wavelength of 10.6 microns. The model shows that at the probe wavelength, practically all the rotation is due to the plasma component, which can be expressed as delta(sub p)= 2pi(e(sup 3))NBL/c(sup 2)nm*(sup 2) omega(sup 2). In this equation, delta(sub p) is the rotation angle due to the free carrier plasma, N is the free carrier concentration, B the magnetic field strength, L the thickness of the sample, n the index of refraction, omega the probe radiation frequency, c the speed of light, e the electron charge, and m* the effective mass. A measurement of N by conventional techniques, combined with a measurement of the Faraday rotation angle allows m* to be accurately determined since it is an inverse square function.

Tanton, George↗

NASA NTRS2016

In-Flight Calibration Methods for Temperature-Dependent Offsets in the MMS Fluxgate Magnetometers

During the first dayside season of the Magnetospheric Multiscale (MMS) mission, the in-flight calibration process for the Fluxgate magnetometers (FGM) implemented an algorithm that selected a constant offset (zero-level) for each sensor on each orbit. This method was generally able to reduce the amplitude of residual spin tone to less than 0.2 nT within the region of interest. However, there are times when the offsets do show significant short-term variations. These variations are most prominent in the nighttime season (phase 1X), when eclipses are accompanied by offset changes as large as 1 nT. Eclipses are followed by a recovery period as long as 12 hours where the offsets continue to change as temperatures stabilize. Understanding and compensating for these changes will become critical during Phase 2 of the mission in 2017, when the nightside will become the focus of MMS science. Although there is no direct correlation between offset and temperature, the offsets are seen for the period of any given week to be well-characterized as function of instrument temperature. Using this property, a new calibration method has been developed that has proven effective in compensating for temperature-dependent offsets during phase 1X of the MMS mission and also promises to further refine calibration quality during the dayside season.

Magnetic field reconnection↗

NASA NTRS2017

In-Flight Calibration of the MMS Fluxgate Magnetometers

We present an overview of the approach to in-flight calibration, which is a coordinated effort between the University of California Los Angeles (UCLA), Space Research Institute, Graz, Austria (IWF) and the NASA Goddard Space Flight Center (GSFC). We present details of the calibration effort at GSFC. During the first dayside season of the Magnetospheric Multiscale (MMS) mission, the in-flight calibration process for the Fluxgate magnetometers (FGM) implemented an algorithm that selected a constant offset (zero-level) for each sensor on each orbit. This method was generally able to reduce the amplitude of residual spin tone to less than 0.2 nT within the region of interest. However, there are times when the offsets do show significant short-term variations. These variations are most prominent in the nighttime season (phase 1X), when eclipses are accompanied by offset changes as large as 1 nT. Eclipses are followed by a recovery period as long as 12 hours where the offsets continue to change as temperatures stabilize. Understanding and compensating for these changes will become critical during Phase 2 of the mission in 2017, when the nightside will become the focus of MMS science. Although there is no direct correlation between offset and temperature, the offsets are seen for the period of any given week to be well-characterized as function of instrument temperature. Using this property, a new calibration method has been developed that has proven effective in compensating for temperature-dependent offsets during phase 1X of the MMS mission and also promises to further refine calibration quality during the dayside season.

Magnetic field reconnection↗

DOE OSTI2023

Computed Tomography Scanning and Geophysical Measurements of the CarbonSAFE Seal Integrity Wells in the Illinois Basin

The U.S. Department of Energy’s (DOE) National Energy Technology Laboratory (NETL) researchers in Morgantown, West Virginia, utilized computed tomography (CT) facilities and the Multi-Sensor Core Logger (MSCL) to evaluate the integrity of three cores (Geophysical Monitor #2 (GM2), Verification Well #1 (VW #1), and Wabash #1 for the Illinois Basin Carbon Storage Assurance Facility Enterprise (CarbonSAFE) efforts. This work was carried out in collaboration with the Illinois State Geological Survey (ISGS) as part of their efforts to analyze cores from two field locations, including the Illinois Basin-Decatur Project (IBDP) and second stage Illinois Industrial Carbon Capture and Storage (IL-ICCS) sites at Decatur, Illinois, and the Wabash CarbonSAFE project at the Wabash Valley Resources Integrated Gasification Combined Cycle plant in Terre Haut, Indiana. The results of this study are presented in several formats and are available online on the Energy Data eXchange (EDX). The rock characterization was conducted using non-destructive techniques, allowing for future analysis of the cores. While the equipment used did not provide direct visualization of shale pore space, it allowed for detection of fractures and discontinuities. Low resolution CT imagery with the NETL medical CT scanner was performed on the entire core. Qualitative analysis of the medical CT images, coupled with x-ray fluorescence (XRF), P-wave, and magnetic susceptibility measurements from the MSCL were utilized to identify areas of interest for further study as well as fractured zones. The ability to quickly identify key areas for more detailed study with higher resolution will save time and resources in future studies. The combination of methods used provided a multi-scale analysis of this core and provided both a macro and micro description of the core that is relevant for many subsurface energy-related examinations traditionally performed at NETL.

58 GEOSCIENCES↗

DOE OSTI2021

Preface

Crystallization via nonclassical pathways is important during the formation of minerals in nature and has become a popular method to synthesize advanced materials on both laboratory and industrial scales. Unlike classical crystal growth pathways via monomer-by-monomer addition, crystallization via nonclassical pathways, such as particle-by-particle attachment, can form larger crystals more quickly. Materials prepared via nonclassical crystallization have been applied in various fields such as energy, catalysis, environment, biomedicine, optics, electrics, and magnetics. Understanding nonclassical crystallization pathways could provide new insights into synthesizing novel materials. This ACS Book series aims to provide updated information on fundamental nonclassical crystallization research, including theory and experiments. It is also intended for experienced researchers, to reinforce their knowledge of the developmental scope of new techniques–especially state-of-the-art in situ characterization tools–to understand mechanisms of crystallization via nonclassical pathways. Topics covered in this book series include: (1) nonclassical nucleation; (2) cluster assembly; (3) particle-based crystallization; (4) crystal formation from amorphous intermedium phases; (5) biomineralization via nonclassical pathways; (6) theoretical developments to simulate nonclassical crystallization; (7) observation of the nonclassical crystallization pathways via various characterization techniques; and (8) the application of nonclassical crystallization. Volume II of the Nonclassical Crystallization Book Series will cover a broad range of topics including particle-based crystallization, biomolecular self-assembly, biomineralization, nanoscale imaging, and applications of nonclassical crystallization.

Zhang, Xin↗

DOE OSTI2020

2D HSQC Chemical Shifts of Impurities from Biomass Pretreatment

Two dimensional (2D) heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) is a powerful analytical method which can be used to elucidate the structure of biomass. During processing, biomass is typically subjected to some form of chemical treatment which can be performed with a variety of compounds. The presence of these compounds, even in trace amounts, has the potential to contaminate the sample and lead to misinterpretation of the HSQC spectra. Here we report the chemical shifts of 29 compounds commonly used in biomass processing which have the potential to contaminate the biomass samples and lead to the misinterpretation of peaks associated with biomass (Populus trichocarpa ) pretreated via autohydrolysis. The identification of these chemical shifts could serve as a valuable tool in preventing errors in characterizing biomass via HSQC.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1983

Geomagnetism of earth's core

Instrumentation, analytical methods, and research goals for understanding the behavior and source of geophysical magnetism are reviewed. Magsat, launched in 1979, collected global magnetometer data and identified the main terrestrial magnetic fields. The data has been treated by representing the curl-free field in terms of a scalar potential which is decomposed into a truncated series of spherical harmonics. Solutions to the Laplace equation then extend the field upward or downward from the measurement level through intervening spaces with no source. Further research is necessary on the interaction between harmonics of various spatial scales. Attempts are also being made to analytically model the main field and its secular variation at the core-mantle boundary. Work is also being done on characterizing the core structure, composition, thermodynamics, energetics, and formation, as well as designing a new Magsat or a tethered satellite to be flown on the Shuttle.

Benton, E. R.↗

NASA NTRS2017

Highly Conductive Wire: Cu Carbon Nanotube Composite Ampacity and Metallic CNT Buckypaper Conductivity

NASA is currently working on developing motors for hybrid electric propulsion applications in aviation. To make electric power more feasible in airplanes higher power to weight ratios are sought for electric motors. One facet to these efforts is to improve (increase) the conductivity and (lower) density of the magnet wire used in motors. Carbon nanotubes (CNT) and composites containing CNT are being explored as a possible way to increase wire conductivity and lower density. Presented here are measurements of the current carrying capacity (ampacity) of a composite made from CNT and copper. The ability of CNT to improve the conductivity of such composites is hindered by the presence of semiconductive CNT (s-CNT) that exist in CNT supplies naturally, and currently, unavoidably. To solve this problem, and avoid s-CNT, various preferential growth and sorting methods are being explored. A supply of sorted 95 metallic CNT (m-CNT) was acquired in the form of thick film Buckypaper (BP) as part of this work and characterized using Raman spectroscopy, resistivity, and density measurements. The ampacity (Acm2) of the Cu-5volCNT composite was 3.8 lower than the same gauge pure Cu wire similarly tested. The lower ampacity in the composite wire is believed to be due to the presence of s-CNT in the composite and the relatively low (proper) level of longitudinal cooling employed in the test method. Although Raman spectroscopy can be used to characterize CNT, a strong relation between the ratios of the primary peaks GGand the relative amounts of m-CNT and s-CNT was not observed. The average effective conductivity of the CNT in the sorted, 95 m-CNT BP was 2.5 times higher than the CNT in the similar but un-sorted BP. This is an indication that improvements in the conductivity of CNT composites can be made by the use of sorted, highly conductive m-CNT.

wire↗

NASA NTRS2016

Carbon Nanotube Composite Ampacity and Metallic CNT Buckypaper Conductivity

yarns↗

DOE OSTI2023

Quantitative Analysis of Origin of Lithium Inventory Loss and Interface Evolution over Extended Fast Charge Aging in Li Ion Batteries

During the extreme fast charging (XFC) of lithium-ion batteries, lithium inventory loss (LLI) and reaction mechanisms at the anode/electrolyte interface are crucial factors in performance and safety. Determining the causes of LLI and quantifying them remain an essential challenge. We present mechanistic research on the evolution and interactions of aging mechanisms at the anode/electrolyte interface. We used NMC 532 /graphite pouch cells charged at rates of 1, 6, and 9 C up to 1000 cycles for our investigation. The cell components were characterized after cycling using electrochemical measurements, inductively coupled plasma optical emission spectroscopy, 7 Li solid-state nuclear magnetic resonance spectroscopy, and high-performance liquid chromatography/mass spectrometry. The results indicate that cells charged at 1 C exhibit no Li plating, and the increase of SEI thickness is the dominant source of the Li loss. In contrast, Li loss in cells charged at 9 C is related to the formation of the metallic plating layers (42%) the SEI layer (38.1%) and irreversible intercalation into the bulk graphite (19%). XPS analysis suggests that the charging rate has little influence on the evolution of SEI composition. The interactions between competing aging mechanisms were evaluated by a correlation analysis. In conclusion, the quantitative method established in this work provides a comprehensive analytical framework for understanding the synergistic coupling of anodic degradation mechanisms, forecasting SEI failure scenarios, and assessing the XFC lithium-ion battery capacity fade.

25 ENERGY STORAGE↗

DOE OSTI2026

4D beam matrix reconstruction in particle accelerators

Transverse beam parameters in particle accelerators are commonly described using the Twiss parameters, which are experimentally accessible yet inherently limited because they neglect correlations between different transverse coordinates. Such correlations frequently arise from uncompensated cathode magnetic fields or misaligned focusing quadrupoles, affecting beam quality and accelerator performance. To address this limitation, we propose and validate a novel diagnostic method for the complete four-dimensional (4D) transverse beam matrix. Our method involves passing the beam through a beamline comprising both conventional and skew quadrupole magnets, followed by downstream measurements of the resulting two-dimensional (2D) beam profiles. These measurements represent distinct 2D projections of the underlying 4D transverse phase–space distribution. By systematically varying quadrupole strengths, multiple independent projections of the beam phase space are obtained. We reconstruct the original 4D beam matrix from these measured projections using an optimization-based least-square fit, providing fast and robust reconstruction regardless of the specific beamline configuration. Through extensive numerical simulations and realistic particle-tracking studies, we demonstrate the diagnostic’s accuracy, robustness, and capability to achieve reconstruction uncertainties smaller than measurement errors, particularly when employing sufficient numbers of quadrupole scans. This method presents a powerful and flexible approach for comprehensive beam characterization and accelerator tuning.

43 PARTICLE ACCELERATORS↗

DOE OSTI2020

Thermodynamics and magnetism in the two-dimensional to three-dimensional crossover of the Hubbard model

The realization of antiferromagnetic (AF) correlations in ultracold fermionic atoms on an optical lattice is a significant achievement. Experiments have been carried out in one, two, and three dimensions, and have also studied anisotropic configurations with stronger tunneling in some lattice directions. Such anisotropy is relevant to the physics of cuprate superconductors and other strongly correlated materials. Moreover, this anisotropy might be harnessed to enhance AF order. Here we numerically investigate, using the determinant quantum Monte Carlo method, a simple realization of anisotropy in the three-dimensional (3D) Hubbard model in which the tunneling between planes, $t_⊥$, is unequal to the intraplane tunneling $\textit{t}$. This model interpolates between the three-dimensional isotropic ($t_⊥ = t$) and two-dimensional (2D;$t_⊥$ = 0) systems. In this work, we show that at fixed interaction strength to tunneling ratio ($\textit{U/t}$), anisotropy can enhance the magnetic structure factor relative to both 2D and 3D results. However, this enhancement occurs at interaction strengths below those for which the Néel temperature $T_{\text{Néel}}$ is largest, in such a way that the structure factor cannot be made to exceed its value in isotropic 3D systems at the optimal $\textit{U/t}$. We characterize the 2D-3D crossover in terms of the magnetic structure factor, real space spin correlations, number of doubly occupied sites, and thermodynamic observables. An interesting implication of our results stems from the entropy's dependence on anisotropy. As the system evolves from 3D to 2D, the entropy at a fixed temperature increases. Correspondingly, at fixed entropy, the temperature will decrease going from 3D to 2D. This suggests a cooling protocol in which the dimensionality is adiabatically changed from 3D to 2D.

74 ATOMIC AND MOLECULAR PHYSICS↗