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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 253 records · Page 14
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Focused‐beam X‐ray fluorescence and diffraction microtomographies for mineralogical and chemical characterization of unsectioned extraterrestrial samples

Abstract This study describes the application of new synchrotron X‐ray fluorescence (XRF) and diffraction (XRD) microtomographies for the 3‐D visualization of chemical and mineralogical variations in unsectioned extraterrestrial samples. These improved methods have been applied to three compositionally diverse chondritic meteorite samples that were between 300 and 400 μm in diameter, including samples prepared from fragments of the CR2 chondrite LaPaz Icefield (LAP) 02342, H5 chondrite MacAlpine Hills (MAC) 88203, and the CM2 chondrite Murchison. The synchrotron‐based XRF and XRD tomographies used are focused‐beam techniques that measure the intensities of fluorescent and diffracted X‐rays in a sample simultaneously during irradiation by a high‐energy microfocused incident X‐ray beam. Measured sinograms of the emitted and diffracted intensities were then tomographically reconstructed to generate 2‐D slices of XRF and XRD intensity through the sample, with reconstructed pixel resolution of 1–2 μm, defined by the resolution of the focused incident X‐ray beam. For sample LAP 02342, primary mineral phases that were visualized in reconstructed slices using these techniques included isolated grains of α‐Fe, orthopyroxene, and olivine. For our sample of MAC 88203, XRF/XRD tomography allowed visualization of forsteritic olivine as a primary mineral phase, a vitrified fusion crust at the sample surface, identification of localized Cr‐rich spinels at spatial resolutions of several micrometers, and imaging of a plagioclase‐rich glassy matrix. In the sample of Murchison, major identifiable phases include clinoenstatite‐ and olivine‐rich chondrules, variable serpentine matrix minerals and small Cr‐rich spinels. Most notable in the tomographic analysis of Murchison is the ability to quantitatively distinguish and visualize the complex mixture of serpentine‐group minerals and associated tochilinite–cronstedtite intergrowths. These methods provide new opportunities for spatially resolved characterization of sample texture, mineralogy, crystal structure, and chemical state in unsectioned samples. This provides researchers an ability to characterize such samples internally with minimal disruption of sample micro‐structures and chemistry, possibly without the need for sample extraction from some types of sampling and capture media.

Geochemistry & Geophysics↗
DOE OSTI2023

Experimental 4D Tracking of a Single Electron in IOTA

We present the results of the first experiments on 4-dimensional phase-space tracking of a single electron in a storage ring, using a linear multi-anode photomultiplier tube for simultaneously measuring transverse coordinates and arrival times of synchrotron-radiation pulses. During the next few months, full 6D tracking will be implemented. This technology makes it possible to characterize the motion of a single particle, i.e. simultaneously tracking of amplitudes and phases for slow synchrotron oscillations and fast betatron oscillations. Complete tracking of a single particle enables the first direct measurements of dynamical properties, including invariants, amplitude-dependent tunes, and chaotic behavior.

43 PARTICLE ACCELERATORS↗
DOE OSTI2020

Extreme ultraviolet microscope characterization using photomask surface roughness

We demonstrate a method for characterizing the field-dependent aberrations of a full-field synchrotron-based extreme ultraviolet microscope. The statistical uniformity of the inherent, atomic-scale roughness of readily-available photomask blanks enables a self-calibrating computational procedure using images acquired under standard operation. We characterize the aberrations across a 30-um field-of-view, demonstrating a minimum aberration magnitude of smaller than λ/21 rms averaged over the center 5-um area, with a measurement accuracy better than λ/180 rms. The measured field variation of aberrations is consistent with system geometry and agrees with prior characterizations of the same system. In certain cases, it may be possible to additionally recover the illumination wavefront from the same images. Our method is general and is easily applied to coherent imaging systems with steerable illumination without requiring invasive hardware or custom test objects; hence, it provides substantial benefits when characterizing microscopes and high-resolution imaging systems in situ.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Electrochemistry of Thin Films with In Situ/Operando Grazing Incidence X-Ray Scattering: Bypassing Electrolyte Scattering for High Fidelity Time Resolved Studies

Electroactive polymer thin films undergo repeated reversible structural change during operation in electrochemical applications. While synchrotron X-ray scattering is powerful for the characterization of stand-alone and ex situ organic thin films, in situ/operando structural characterization has been underutilized-in large part due to complications arising from supporting electrolyte scattering. This has greatly hampered the development of application relevant structure property relationships. Therefore, a new methodology for in situ/operando X-ray characterization that separates the incident and scattered X-ray beam path from the electrolyte is developed. As a proof of concept, the operando structural characterization of weakly-scattering, organic mixed conducting thin films in an aqueous electrolyte environment is demonstrated, accessing previously unexplored changes in the $\pi-\pi$ peak and diffuse scatter, while capturing the solvent swollen thin film structure which is inaccessible in previous ex situ studies. These in situ/operando measurements improve the sensitivity to structural changes, capturing minute changes not possible ex situ, and have multimodal potential such as combined Raman measurements that also serve to validate the true in situ/operando conditions of the cell. Finally, new directions enabled by this in situ/operando cell design are examined and state of the art measurements are compared.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Amorphous nonstoichiometric oxides with tunable room-temperature ferromagnetism and electrical transport

Material functionalities strongly depend on the stoichiometry, crystal structure, and homogeneity. Here we demonstrate an approach of amorphous nonstoichiometric inhomogeneous oxides to realize tunable ferromagnetism and electrical transport at room temperature. In order to verify the origin of the ferromagnetism, we employed a series of structural, chemical, and electronic state characterizations. Combined with electron microscopy and transport measurements, synchrotron-based grazing incident wide angle X-ray scattering, soft X-ray absorption and circular dichroism clearly reveal that the room-temperature ferromagnetism originates from the In 0.23 Co 0.77 O 1-v amorphous phase with a large tunable range of oxygen vacancies. The room-temperature ferromagnetism is tunable from a high saturation magnetization of 500 emu cm -3 to below 25 emu cm -3 , with the evolving electrical resistivity from 5 × 10 3 μΩ cm to above 2.5 × 10 5 μΩ cm. Inhomogeneous nano-crystallization emerges with decreasing oxygen vacancies, driving the system towards non-ferromagnetism and insulating regime. Our work unfolds the novel functionalities of amorphous nonstoichiometric inhomogeneous oxides, which opens up new opportunities for developing spintronic materials with superior magnetic and transport properties.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2021

Resolving the Evolution of Atomic Layer-Deposited Thin-Film Growth by Continuous In Situ X-Ray Absorption Spectroscopy

In situ synchrotron X-ray absorption near-edge structure characterization of thin-film titania growth by atomic layer deposition (ALD) over ZnO nanowires reveals persistent low-coordinated Ti motifs leading to a new picture of ALD growth. Through the design of growth and measurement cycles, Ti K-edge spectral data are continuously recorded so as to characterize the film evolution as a function of ALD cycle number and the surface changes within the time scale of the ALD cycle. A unified set of analysis tools is developed to interpret the time-series of spectral data. A prenucleation stage of growth, a transition region, and then a steady-state growth stage are observed with distinguishable features. Multivariate curve resolution analysis, that is physically constrained, demonstrates two specific spectral components with associated, time-dependent concentrations. The bulk-film component tracks the stages of growth. The surface and interface components, present throughout the stages of growth, reveal a significant coverage of relatively isolated or loosely networked tetrahedrally coordinated Ti atomic motifs. Lastly, spectral signatures for the intra-cycle growth kinetics are reconstructed at a time resolution of ~1 s and demonstrate that the transient Ti motifs on the growing surface stabilize within a few seconds of the Ti precursor pulse.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Scalable Synthesis and Characterization of Multilayer γ-Graphyne, New Carbon Crystals with a Small Direct Band Gap

γ-Graphyne is the most symmetric sp 2 /sp 1 allotrope of carbon, which can be viewed as graphene uniformly expanded through the insertion of two-carbon acetylenic units between all the aromatic rings. To date, synthesis of bulk γ-graphyne has remained a challenge. In this work, we report the synthesis of multilayer γ-graphyne through crystallization-assisted irreversible cross-coupling polymerization. A comprehensive characterization of this new carbon phase is described, including synchrotron powder X-ray diffraction, electron diffraction, lateral force microscopy, Raman spectroscopy, infrared spectroscopy, and cyclic voltammetry. Experiments indicate that γ-graphyne is a 0.48 eV band gap semiconductor, with a hexagonal a-axis spacing of 6.88 Å and an interlayer spacing of 3.48 Å, which is consistent with theoretical predictions. The observed crystal structure has an aperiodic sheet stacking. The material is thermally stable up to 240 °C but undergoes transformation at higher temperatures. While conventional 2D polymerization and reticular chemistry rely on error correction through reversibility, we demonstrate that a periodic covalent lattice can be synthesized under purely kinetic control. The reported methodology is scalable and inspires extension to other allotropes of the graphyne family.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Towards high-efficiency particle detection using superconducting microwire arrays

Here, we present a detailed study of an 8-channel 1×1 mm 2 WSi superconducting microwire single photon detector (SMSPD) array exposed to 120 GeV hadron beam and 120 GeV muon beam at the CERN Super Proton Synchrotron H6 beamline. Following up on our first detailed characterization of the efficiency and response of an SMSPD fabricated on a 3 nm WSi film, we report measurements of enhanced particle detection efficiency using a sensor fabricated from a thicker 4.7 nm-thick WSi film. We also report the first SMSPD detection efficiency measurement made for muons. Measurements are enabled by a silicon tracking telescope providing 10 μm in-situ spatial resolution. The results show a fill factor-normalized detection efficiency of 75% and a time resolution of about 130 ps across pixels. These findings represent a significant advancement toward developing high-efficiency SMSPD charged particle tracking systems with simultaneous precision timing, with potential applications in future accelerator-based experiments such as the FCC-ee and Muon Collider.

Cryogenic detectors↗
DOE OSTI2024

Orientational analysis of atomic pair correlations in nanocrystalline indium oxide thin films

The application of grazing-incidence total X-ray scattering (GITXS) for pair distribution function (PDF) analysis using >50 keV X-rays from synchrotron light sources has created new opportunities for structural characterization of supported thin films with high resolution. Compared with grazing-incidence wide-angle X-ray scattering, which is only useful for highly ordered materials, GITXS/PDFs expand such analysis to largely disordered or nanostructured materials by examining the atomic pair correlations dependent on the direction relative to the surface of the supporting substrate. A characterization of nanocrystalline In 2 O 3 -derived thin films is presented here with in-plane-isotropic and out-of-plane-anisotropic orientational ordering of the atomic structure, each synthesized using different techniques. The atomic orientations of such films are known to vary based on the synthetic conditions. Here, an azimuthal orientational analysis of these films using GITXS with a single incident angle is shown to resolve the markedly different orientations of the atomic structures with respect to the planar support and the different degrees of long-range order, and hence, the terminal surface chemistries. It is anticipated that orientational analysis of GITXS/PDF data will offer opportunities to extend structural analyses of thin films by providing a means to qualitatively determine the major atomic orientation within nanocrystalline and, eventually, non-crystalline films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Advances in High Resolution Ultrafast Scintillators for Fast timing Applications

Scintillation detectors exhibiting high spatial resolution and fast timing capabilities are of vital importance for synchrotron sources. These detectors may be exposed to a variety of X-ray energies (up to 140 keV) and used in high frame rate applications. Here, we describe the advances in the development of thin-film LuI3:Ce scintillators for higher energy X-ray imaging, with fast timing and high spatial resolution. When grown in a single crystalline form, these scintillators are bright, producing 115 000 photons/MeV. However, to achieve high spatial resolution, these scintillators are grown in thin-film form with a microcolumnar structure, controllable to column diameters of <1-30 mu m. Thus, a much thicker scintillator layer (10 mu m-3 mm or higher) may be grown, providing superior X-ray absorption while achieving high resolutions of 50 mu m or better, at the cost of reduced light yield. To study the timing characteristics of the scintillator, time-resolved X-ray excited optical luminescence (TR-XEOL) was performed on two different sets of three samples of LuI3 at the 1-BM beamline of the Advanced Photon Source at Argonne National Laboratory. Besides, we report timing measurements obtained using a photomultiplier tube (PMT) and oscilloscope at Radiation Monitoring Devices (RMD) Inc. Using the TR-XEOL, we determined the decay constants of LuI3 as a function of Ce doping, recording a fast decay component as low as 3.6 ns (39%), one of the fastest values recorded in inorganic scintillators. This fast decay opens up numerous novel applications, where ultrahigh frame rates are important using synchrotron X-rays. This article will discuss fabrication, characterization, and potential applications for this novel scintillator.

fast timing↗
DOE OSTI2024

Isotropic negative thermal expansion in ZrW 2 O 8 and HfW 2 O 8 from 1100 to 1275°C

Abstract ZrW 2 O 8 (ZrO 2 •2WO 3 ) and HfW 2 O 8 (HfO 2 •2WO 3 ) have been the focus of thermal expansion studies due to their isotropic negative thermal expansion (NTE) measured previously at temperatures below 775°C. This work presents measurements of these materials at their thermodynamically stable temperature ranges of 1105 and 1257°C for ZrW 2 O 8 and 1105–1276°C for HfW 2 O 8 , where they were characterized with in situ, powder X‐ray diffraction. The linear coefficients of thermal expansion were measured to be −5.52 × 10 −6 and −4.87 × 10 −6 °C −1 for ZrW 2 O 8 and HfW 2 O 8 , respectively. The mechanism leading to this NTE is discussed. Powder samples were synthesized by a solution‐based process called the organic–inorganic steric entrapment method. In situ characterization in air was carried out at the National Synchrotron Light Source II using a hexapole lamp, optical furnace and the Advanced Photon Source using a quadrupole lamp, optical furnace to achieve elevated temperatures.

Materials Science↗
DOE OSTI2020

Nitrogen in black phosphorus structure

Group V elements in crystal structure isostructural to black phosphorus with unique puckered two-dimensional layers exhibit exciting physical and chemical phenomena. However, as the first element of group V, nitrogen has never been found in the black phosphorus structure. Here, we report the synthesis of the black phosphorus–structured nitrogen at 146 GPa and 2200 K. Metastable black phosphorus–structured nitrogen was retained after quenching it to room temperature under compression and characterized in situ during decompression to 48 GPa, using synchrotron x-ray diffraction and Raman spectroscopy. We show that the original molecular nitrogen is transformed into extended single-bonded structure through gauche and trans conformations. Raman spectroscopy shows that black phosphorus–structured nitrogen is strongly anisotropic and exhibits high Raman intensities in two A g normal modes. Synthesis of black phosphorus–structured nitrogen provides a firm base for exploring new type of high-energy-density nitrogen and a new direction of two-dimensional nitrogen.

58 GEOSCIENCES↗
DOE OSTI2025

Towards High-Efficiency Particle Detection Using Superconducting Microwire Arrays

We present a detailed study of an 8-channel $1\times1$~mm$^{2}$ WSi superconducting microwire single photon detector (SMSPD) array exposed to 120~GeV hadron beam and 120~GeV muon beam at the CERN Super Proton Synchrotron H6 beamline. Following up on our first detailed characterization of the efficiency and response of an SMSPD fabricated on a 3~nm WSi film, we report measurements of enhanced particle detection efficiency using a sensor fabricated from a thicker 4.7~nm-thick WSi film. We also report the first SMSPD detection efficiency measurement made for muons. Measurements are enabled by a silicon tracking telescope providing 10~$\mu$m in situ spatial resolution. The results show a detection efficiency of 75\% and a time resolution of about 130~ps across pixels. These findings represent a significant advancement toward developing high-efficiency SMSPD charged particle tracking systems with simultaneous precision timing, with potential applications in future accelerator-based experiments such as the FCC-ee and Muon Collider.

Wang, Christina [Fermilab]↗
NASA NTRS1997

Relative Band Oscillator Strengths for Carbon Monoxide: Alpha (1)Pi-Chi (1)Sigma(+) Transitions

Band oscillator strengths for CO transitions between the electronic states A (l)Pi and X(1)Sigma(+) were measured via absorption with a synchrotron radiation source. When referenced to the well-characterized (5,0) band oscillator strength, our relative values for the (7,0) to (11,0) bands are most consistent with the recent experiments of Chan et al. and the theoretical predictions of Kirby & Cooper. Since the results from various laboratory techniques and theory now agree, analyses of interstellar CO based on absorption from A-X bands are no longer hindered by uncertainties in oscillator strength.

Federman, S. R.↗
DOE OSTI2023

At-wavelength characterization of X-ray wavefronts in Bragg diffraction from crystals

The advent of next-generation synchrotron radiation sources and X-ray free-electron lasers calls for high-quality Bragg-diffraction crystal optics to preserve the X-ray beam coherence and wavefront. This requirement brings new challenges in characterizing crystals in Bragg diffraction in terms of Bragg-plane height errors and wavefront phase distortions. Here, a quantitative methodology to characterize crystal optics using a state-of-the-art at-wavelength wavefront sensing technique and statistical analysis is proposed. The method was tested at the 1-BM-B optics testing beamline at the Advanced Photon Source for measuring silicon and diamond crystals in a self-referencing single-crystal mode and an absolute double-crystal mode. The phase error sensitivity of the technique is demonstrated to be at the λ/100 level required by most applications, such as the characterization of diamond crystals for cavity-based X-ray free-electron lasers.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2024

Time-resolved synchrotron light source X-ray detection with Low-Gain Avalanche Diodes

Low Gain Avalanche Diodes (LGADs) represent the state-of-the-art in timing measurements and will instrument future timing detectors at the High Luminosity Large Hadron Collider (HL-LHC) experiments. While conceived as a sensor for charged particles, the intrinsic gain of LGADs makes it possible to detect low energy X-rays with good energy resolution and excellent timing (tens of picoseconds). Here, using the Stanford Synchrotron Radiation Lightsource (SSRL) at SLAC, several LGADs designs were characterized with energies from 5 to 35 keV. The SSRL provides 10 ps pulsed X-ray bunches separated by 2.1 ns intervals, and with an energy dispersion (ΔE/E) of 1 X 10 -4 . LGADs fabricated by Hamamatsu Photonics (HPK) and Brookhaven National Laboratory (BNL) with different thicknesses ranging from 20 µm to 50 µm and different gain layer designs were read out a two stage fast amplification circuit and digitized with a high bandwidth, high sampling rate oscilloscope. PIN devices from HPK were characterized as well. A systematic and detailed characterization of the devices’ energy linearity, resolution and timing resolution as a function of X-ray energy was performed for different biasing voltages at room temperature

Charge multiplication↗
DOE OSTI2022

Non-destructive depth-resolved characterization of residual strain fields in high electron mobility transistors using differential aperture x-ray microscopy

Localized residual stress and elastic strain concentrations in microelectronic devices often affect the electronic performance, resistance to thermomechanical damage, and, likely, radiation tolerance. A primary challenge for the characterization of these concentrations is that they exist over sub-μm length-scales, precluding their characterization by more traditional residual stress measurement techniques. Here, in this study, we demonstrate the use of synchrotron x-ray-based differential aperture x-ray microscopy (DAXM) as a viable, non-destructive means to characterize these stress and strain concentrations in a depth-resolved manner. DAXM is used to map two-dimensional strain fields between the source and the drain in a gallium nitride (GaN) layer within high electron mobility transistors (HEMTs) with sub-μm spatial resolution. Strain fields at various positions in both pristine and irradiated HEMT specimens are presented in addition to a preliminary stress analysis to estimate the distribution of various stress components within the GaN layer. γ-irradiation is found to significantly reduce the lattice plane spacing in the GaN along the sample normal direction, which is attributed to radiation damage in transistor components bonded to the GaN during irradiation.

42 ENGINEERING↗