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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 361 records · Page 20
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Solvent-dependent complex reaction pathways of bromoform revealed by time-resolved X-ray solution scattering and X-ray transient absorption spectroscopy

The photochemical reaction pathways of CHBr3 in solution were unveiled using two complementary X-ray techniques, time-resolved X-ray solution scattering (TRXSS) and X-ray transient absorption spectroscopy, in a wide temporal range from 100 ps to tens of microseconds. By performing comparative measurements in protic (methanol) and aprotic (methylcyclohexane) solvents, we found that the reaction pathways depend significantly on the solvent properties. In methanol, the major photoproducts are CH3OCHBr2 and HBr generated by rapid solvolysis of iso-CHBr2-Br, an isomer of CHBr3. In contrast, in methylcyclohexane, iso-CHBr2-Br returns to CHBr3 without solvolysis. In both solvents, the formation of CHBr2 and Br is a competing reaction channel. From the structural analysis of TRXSS data, we determined the structures of key intermediate species, CH3OCHBr2 and iso-CHBr2-Br in methanol and methylcyclohexane, respectively, which are consistent with the structures from density functional theory calculations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Optical and x-ray characterization of the Daedalus ultrafast x-ray imager

The Daedalus ultrafast x-ray imager is the latest generation in Sandia’s hybrid CMOS detector family. With three frames along an identical line of sight, 1 ns minimum integration time, a higher full well than Icarus, and added features, Daedalus brings exciting new capabilities to diagnostic applications in inertial confinement fusion and high energy density science. In this work, we present measurements of time response, dynamic range, spatial uniformity, pixel cross-talk, and absolute x-ray sensitivity using pulsed optical and x-ray sources. Here, we report a measured 1.5 Me — full well, pixel sensitivity at 9.58 × 10 —7 V/e — , and an estimate of spatial uniformity at ~5% across the sensor array.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

The Effect of Intensity Fluctuations on Sequential X-ray Photon Correlation Spectroscopy at the X-ray Free Electron Laser Facilities

How materials evolve at thermal equilibrium and under external excitations at small length and time scales is crucial to the understanding and control of material properties. X-ray photon correlation spectroscopy (XPCS) at X-ray free electron laser (XFEL) facilities can in principle capture dynamics of materials that are substantially faster than a millisecond. However, the analysis and interpretation of XPCS data is hindered by the strongly fluctuating X-ray intensity from XFELs. Here we examine the impact of pulse-to-pulse intensity fluctuations on sequential XPCS analysis. We show that the conventional XPCS analysis can still faithfully capture the characteristic time scales, but with substantial decrease in the signal-to-noise ratio of the g2 function and increase in the uncertainties of the extracted time constants. We also demonstrate protocols for improving the signal-to-noise ratio and reducing the uncertainties.

36 MATERIALS SCIENCE↗
NASA NTRS2023

Discovery of Strongly Variable X-Ray Polarization in the Neutron Star Low-Mass X-Ray Binary Transient XTE J1701−462

Context. After about 16 years since its first outburst, the transient neutron star low-mass X-ray binary XTE J1701−462 turned on again in September 2022, allowing for the first study of its X-ray polarimetric characteristics by a dedicated observing program with the Imaging X-ray Polarimeter Explorer (IXPE). Aims. Polarimetric studies of XTE J1701−462 have been expected to improve our understanding of accreting weakly magnetized neutron stars, in particular, the physics and the geometry of the hot inner regions close to the compact object. Methods. The IXPE data of two triggered observations were analyzed using time-resolved spectroscopic and polarimetric techniques, following the source along its Z-track of the color–color diagram. Results. During the first pointing on 2022 September 29, an average 2–8 keV polarization degree of (4.6 ± 0.4)% was measured, the highest value found up to now for this class of sources. Conversely, only a ∼0.6% average degree was obtained during the second pointing ten days later. Conclusions. The polarimetric signal appears to be strictly related to the higher energy blackbody component associated with the boundary layer (BL) emission and its reflection from the inner accretion disk, and it is as strong as 6.1% and 1.2% (> 95% significant) above 3–4 keV for the two measurements, respectively. The variable polarimetric signal is apparently related to the spectral characteristics of XTE J1701−462, which is the strongest when the source was in the horizontal branch of its Z-track and the weakest in the normal branch. These IXPE results provide new important observational constraints on the physical models and geometry of the Z-sources. Here, we discuss the possible reasons for the presence of strong and variable polarization among these sources.

XTEJ1701↗
DOE OSTI2020

X-ray and gamma-ray tomographic imaging of fuel relocation inside sodium fast reactor test assemblies during severe accidents

The present work reports on x-ray and gamma-ray high-spatial resolution computerized tomography measurements of the Pin Bundle Metallic Fuel Relocation (PBR) assemblies tested in the Metallic Uranium Safety Experiment (MUSE) facility at Argonne National Lab (ANL). The aim of the study was to characterize fuel relocation structures that develop during severe core accidents pertaining to SFR assemblies; these include but are not limited to advanced core disruption recreated in the PBR-1 assembly, and cladding breach recreated in the PBR-2 assembly. We report the x-ray tomography measurements were able to resolve small quantities of relocation fuel; with increased presence of relocation fuel, the x-ray 1measurements spatially mapped the material but could not resolve the inner regions of these. The gamma-tomography measurements showed improved results, resolving the relocation structures in great detail. The upper plenum of the PBR-1 assembly where the molten uranium was initially inserted presented high structural damage, reflected by the partial and complete disintegration of the central rods. Relocation fuel filled the subchannels, adhering to surviving cladding walls and the assembly casing. In the lower portion of the measured section, the tomogram degrades due to photon starvation effects hinting at the increased amount of relocation fuel potentially plugging the assembly; flow blockage in this section was difficult to determine due to the tomogram’s degradation from photon starvation. Small fragments were observed further down the assembly, dislodged from the initial insertion of the molten material. This section was used as an unperturbed assembly reference, with a calculated blockage of less than 1% from the present fragments. The PBR-2 assembly was characterized by columnar relocation structures propagating through the subchannels. Three of the relocation structures were captured in the measured section, with evidence of cross migration on to adjacent subchannels. The measured section in this assembly captures the leading edge of two structures. The calculated flow blockage was 16% in the planes where the three relocation structures are present, but this quickly decreases to approximately 5% past the leading edge of two of the structures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Time-Resolved X-ray Emission Spectroscopy and Resonant Inelastic X-ray Scattering Spectroscopy of Laser Irradiated Carbon

The existence of liquid carbon as an intermediate phase preceding the formation of novel carbon materials has been a point of contention for several decades. Experimental observation of such a liquid state requires nonthermal melting of solid carbon materials at various laser fluences and pulse properties. Reflectivity experiments performed in the mid-1980s reached opposing conclusions regarding the metallic or insulating properties of the purported liquid state. Time-resolved X-ray absorption studies showed shortening of C–C bonds and increasing diffraction densities, thought to evidence a liquid or glassy carbon state, respectively. Nevertheless, none of these experiments provided information on the electronic structure of the proposed liquid state. Herein, we report the results of time-resolved resonant inelastic X-ray scattering (RIXS) and time-resolved X-ray emission spectroscopy (XES) studies on amorphous carbon (a-C) and ultrananocrystalline diamond (UNCD) as a function of delay time between the irradiating pulse and X-ray probe. For both a-C and UNCD, we attribute decreases in RIXS or XES signals to transition blocking, relaxation, and finally, ablation. Increased signal at 20 ps following the irradiation of the UNCD is attributed to the probable formation of nanoscale structures in the ablation plume. Further, differences in the amount of signal observed between a-C and UNCD are explained by the difference in sample thickness and, specifically, incomplete melting of the UNCD film. Comparisons to spectral simulations based on MD trajectories at extreme conditions indicate that the carbon state in our experiments is crystalline. Normal mode analysis confirmed that symmetrical bending or stretching of the C–C bonds in the diamond lattice results in XES spectra with small intensity differences. Overall, we observed no evidence of melting to a liquid state, as determined by the lack of changes in the spectral properties for up to 100 ps delays following the melting pulses.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Simultaneous bright- and dark-field X-ray microscopy at X-ray free electron lasers

Abstract The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, dark field X-ray microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the $$10^{12}$$ 10 12 photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Single-shot X-ray absorption spectroscopy at X-ray free electron lasers

X-ray Absorption Spectroscopy (XAS) is a widely used X-ray diagnostic method for studying electronic and structural properties of matter. At first glance, the relatively narrow bandwidth and the highly fluctuating spectral structure of X-ray Free Electron Lasers (XFEL) sources seem to require accumulation over many shots to achieve high data quality. To date the best approach to implementing XAS at XFEL facilities has been using monochromators to scan the photon energy across the desired spectral range. While this is possible for easily reproducible samples such as liquids, it is incompatible with many important systems. Here, we demonstrate collection of single-shot XAS spectra over 10s of eV using an XFEL source, with error bars of only a few percent. We additionally show how to extend this technique over wider spectral ranges towards Extended X-ray Absorption Fine Structure measurements, by concatenating a few tens of single-shot measurements. Our results pave the way for future XAS studies at XFELs, in particular those in the femtosecond regime. This advance is envisioned to be especially important for many transient processes that can only be initiated at lower repetition rates, for difficult to reproduce excitation conditions, or for rare samples, such as those encountered in high-energy density physics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

X-ray microscopy and talbot imaging with the matter in extreme conditions X-ray imager at LCLS

The last decade has shown the great potential that X-ray Free Electron Lasers (FEL) have to study High Energy Density (HED) physics. Experiments at FELs have made significant breakthroughs in Shock Physics and Dynamic Diffraction, Dense Plasma Physics and Warm Dense Matter Science, using techniques such as isochoric heating, inelastic scattering, small angle scattering and X-ray diffraction. In addition, and complementary to these techniques, the coherent properties of the FEL beam can be used to image HED samples with high fidelity. We present new imaging diagnostics and techniques developed at the Matter in Extreme Conditions (MEC) instrument at Linac Coherent Light Source (LCLS) over the last few years. We show results in Phase Contrast Imaging geometry, where the X-ray beam propagates from the target to a camera revealing its phase, as well as in Direct Imaging geometry, where a real image of the sample plane is produced in the camera with a spatial resolution down to 200 nm. Last, we show an implementation of the Talbot Imaging method allowing both X-ray phase and intensity measurements change introduced by a target with sub-micron resolution.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Characterizing electronic and atomic structures for amorphous and molecular metal oxide catalysts at functional interfaces by combining soft X-ray spectroscopy and high-energy X-ray scattering

Amorphous thin film materials and heterogenized molecular catalysts supported on electrode and other functional interfaces are widely investigated as promising catalyst formats for applications in solar and electrochemical fuels catalysis. However the amorphous character of these catalysts and the complexity of the interfacial architectures that merge charge transport properties of electrode and semiconductor supports with discrete sites for multi-step catalysis poses challenges for probing mechanisms that activate and tune sites for catalysis. This minireview discusses advances in soft X-ray spectroscopy and high-energy X-ray scattering that provide opportunities to resolve interfacial electronic and atomic structures, respectively, that are linked to catalysis. This review discusses how these techniques can be partnered with advances in nanostructured interface synthesis for combined soft X-ray spectroscopy and high-energy X-ray scattering analyses of thin film and heterogenized molecular catalysts. Further, these combined approaches enable opportunities for the characterization of both electronic and atomic structures underlying fundamental catalytic function, and that can be applied under conditions relevant to device applications.

14 SOLAR ENERGY↗
DOE OSTI2024

Early-time γ -ray constraints on cosmic-ray acceleration in the core-collapse SN 2023ixf with the Fermi Large Area Telescope

Context. While supernova remnants (SNRs) have been considered the most relevant Galactic cosmic ray (CR) accelerators for decades, core-collapse supernovae (CCSNe) could accelerate particles during the earliest stages of their evolution and hence contribute to the CR energy budget in the Galaxy. Some SNRs have indeed been associated with TeV γ -rays, yet proton acceleration efficiency during the early stages of an SN expansion remains mostly unconstrained. Aims. The multi-wavelength observation of SN 2023ixf, a Type II supernova (SN) in the nearby galaxy M 101 (at a distance of 6.85 Mpc), opens the possibility to constrain CR acceleration within a few days after the collapse of the red super-giant stellar progenitor. With this work, we intend to provide a phenomenological, quasi-model-independent constraint on the CR acceleration efficiency during this event at photon energies above 100 MeV. Methods. We performed a maximum-likelihood analysis of γ -ray data from the Fermi Large Area Telescope up to one month after the SN explosion. We searched for high-energy, non-thermal emission from its expanding shock, and estimated the underlying hadronic CR energy reservoir assuming a power-law proton distribution consistent with standard diffusive shock acceleration. Results. We do not find significant γ -ray emission from SN 2023ixf. Nonetheless, our non-detection provides the first limit on the energy transferred to the population of hadronic CRs during the very early expansion of a CCSN. Conclusions. Under reasonable assumptions, our limits would imply a maximum efficiency on the CR acceleration of as low as 1%, which is inconsistent with the common estimate of 10% in generic SNe. However, this result is highly dependent on the assumed geometry of the circumstellar medium, and could be relaxed back to 10% by challenging spherical symmetry. Consequently, a more sophisticated, inhomogeneous characterisation of the shock and the progenitor’s environment is required before establishing whether or not Type II SNe are indeed efficient CR accelerators at early times.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2020

Soft x-ray absorption spectroscopy and magnetic circular dichroism as operando probes of complex oxide electrolyte gate transistors

Electrolyte-based transistors utilizing ionic liquids/gels have been highly successful in the study of charge-density-controlled phenomena, particularly in oxides. Experimental probes beyond transport have played a significant role, despite challenges in their application in electric double-layer transistors. Here, we demonstrate the application of synchrotron soft x-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism (XMCD) as operando probes of the charge state and magnetism in ion-gel-gated ferromagnetic perovskite films. Electrochemical response via oxygen vacancies at positive gate bias in LaAlO 3 (001)/La 0.5 Sr 0.5 CoO 3-δ is used as a test case. XAS/XMCD measurements of 4–25 unit-cell-thick films first probe the evolution of hole doping (from the O K-edge pre-peak) and ferromagnetism (at the Co L-edges), to establish a baseline. Operando soft XAS/XMCD of electrolyte-gated films is then demonstrated, using optimized spin-coated gels with a thickness of ~1 μm and a specific composition. The application of gate voltages up to +4 V is shown to dramatically suppress the O K-edge XAS pre-peak intensity and Co L-edge XMCD, thus enabling the Co valence and ferromagnetism to be tracked upon gate-induced reduction. Soft XAS and XMCD, with appropriate electrolyte design, are thus established to be viable for the operando characterization of electrolyte-gated oxides.

Yu, Biqiong↗
DOE OSTI2020

IRIXS: a resonant inelastic X-ray scattering instrument dedicated to X-rays in the intermediate energy range

A new resonant inelastic X-ray scattering (RIXS) instrument has been constructed at beamline P01 of the PETRA III synchrotron. This instrument has been named IRIXS (intermediate X-ray energy RIXS) and is dedicated to X-rays in the tender-energy regime (2.5–3.5 keV). The range covers the L 2,3 absorption edges of many of the 4delements (Mo, Tc, Ru, Rh, Pd and Ag), offering a unique opportunity to study their low-energy magnetic and charge excitations. The IRIXS instrument is currently operating at the Ru L 3 -edge (2840 eV) but can be extended to the other 4d elements using the existing concept. The incoming photons are monochromated with a four-bounce Si(111) monochromator, while the energy analysis of the outgoing photons is performed by a diced spherical crystal analyzer featuring (10$\bar{2}$ lattice planes of quartz (SiO 2 ). A total resolution of 100 meV (full width at half-maximum) has been achieved at the Ru L 3 -edge, a number that is in excellent agreement with ray-tracing simulations.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Evolution of Metastable Phases During Mg Metal Corrosion: An In Situ Cryogenic X-ray Photoelectron Spectroscopy Study

Magnesium and its alloys are potential structural materials candidates for a wide variety of applications due to their high strength-to-weight ratio. However, ductility and poor corrosion resistance under ambient environmental conditions are the bottleneck for industrial deployment. Designing passivation layers and/or corrosion resistant alloys requires fundamental understanding of the corrosion process. The traditional ex-situ spectroscopic measurements of polycrystalline metal surface with ubiquitous surface impurities and grain boundaries only provided an indistinct view of the corrosion process. To clearly distinguish the mechanism and sequence of corrosion process, we employed in-situ cryo-based x-ray photoelectron spectroscopy (XPS) measurements on Mg single crystal surface exposed to aqueous salt solution. Clean Mg (0001) surfaces were exposed to pure D2O and NaCl aqueous solution (5 wt% NaCl+95 wt% D2O). The interfacial reactions were studied using multimodal analysis including XPS, x-ray diffraction (XRD) and scanning electron microscopy (SEM). In contrast to previous studies, our experiments demonstrated the formation of magnesium chloride hydroxide hydrate during aqueous salt corrosion processes. Evidence of metastable ClO* radicals were also found during the initial aqueous salt solution exposure.

Shutthanandan, Vaithiyalingam↗
DOE OSTI2020

X-Ray Afterglows from the Gamma-Ray Burst “Large-angle” Emission

In this work, we derive basic analytical results for the timing and decay of the gamma-ray burst (GRB) counterpart and delayed afterglow light curves for a brief emission episode from a relativistic surface endowed with angular structure, consisting of a uniform core of size ${\theta }_{c}$ (Lorentz factor ${{\rm{\Gamma }}}_{c}$ and surface emissivity ${i}_{\nu ^{\prime} }^{{\prime} }$ are angle independent) and an axially symmetric power-law envelope (${\rm{\Gamma }}\sim {\theta }^{-g}$). In this "large-angle emission" model, radiation produced during the prompt emission phase (GRB) at angles $\theta \gt {\theta }_{c}$ arrives at the observer well after the burst (delayed emission). The dynamical time range of the very fast decaying GRB "tail" and of the flat afterglow "plateau" and the morphology of the GRB counterpart/afterglow are all determined by two parameters: the core's parameter ${{\rm{\Gamma }}}_{c}{\theta }_{c}$ and the envelope's Lorentz factor index g, leading to three types of light curves that display three post-GRB phases (type 1: tail, plateau/slow decay, post-plateau/normal decay), two post-GRB phases (type 2: tail and fast decay), or just one (type 3: normal decay). We show how X-ray light-curve features can be used to determine core and envelope dynamical and spectral parameters. Testing of the large-angle emission model is done using the Swift/XRT X-ray emission of two afterglows of type 1 (GRB 060607A, GRB 061121), one of type 2 (GRB 061110A), and one of type 3 (GRB 061007). We find that the X-ray afterglows with plateaus require an envelope Lorentz factor ${\rm{\Gamma }}\sim {\theta }^{-2}$ and a comoving-frame emissivity ${i}_{\nu ^{\prime} }^{{\prime} }\sim {\theta }^{2}$; thus, for a typical afterglow spectrum ${F}_{\nu }\sim {\nu }^{-1}$, the lab-frame energy release is uniform over the emitting surface.

79 ASTRONOMY AND ASTROPHYSICS↗