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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 73 records · Page 4

Hard X-ray Fluorescence measurements with TESs at the Advanced Photon Source

Transition Edge Sensor (TES) spectrometers for hard X-ray beamline science will enable improved X-ray emission and absorption spectroscopy in the information-rich 2 to 20keV energy range. We are building a TES-based instrument for time Advanced Photon Source (APS) synchrotron, to be made available to beamline users. 24-pixel prototype arrays have recently been fabricated and tested. the first, spectroscopy measurements using these arrays are promising, with a best single-pixel energy resolution of 11.2 eV and saturation energy > 20 keV. We present a series of recent X-ray Fluorescence measurements involving transition metal elements and multi-element samples with closely spaced emission lines, in particular a Cu-Ni-Co thin film and a foil of Cu and Hf, The TES-measured spectra are directly compared to spectra measured with silicon drift detectors at an APS beamline, demonstrating the improved X-ray science made possible by TES spectrometers.

Guruswamy, Tejas↗

Report on the HP-CAT Workshop-2023 held at the Advanced Photon Source

The conceptual framework and the founding partner and institutional agreements for the High Pressure Collaborative Access Team (HP-CAT) were established in late 1990’s. In the following years, core infrastructure of HP-CAT was built at sector 16 of the Advanced Photon Source (APS) and the first x-ray light was delivered on July 19, 2002 at 7:00pm – followed by an official commemoration ceremony on July 26, 2002.

36 MATERIALS SCIENCE↗

A New Residual Strain Mapping Program Using Energy Dispersive X-Ray Diffraction at the Advanced Photon Source

Here, the ability to non-destructively map the residual strain field inside an engineering component is important for predicting its fatigue life or developing processing methods to prevent failure or enhance performance. In this paper, we describe a new residual strain mapping program at the Advanced Photon Source, Argonne National Laboratory. The new program is based on energy dispersive x-ray diffraction (EDXRD). It is capable of non-destructively penetrating a several- cm thick polycrystalline sample fabricated from engineering alloys using high-energy x-rays and measuring the residual strain field with mm or better spatial resolution and approximately ±1 x 10 -4 strain resolution. A multi-element detector array is employed to measure multiple strain components simultaneously. The residual strain mapping setup is augmented with a high-energy tomography capability, allowing precise alignment of the material volume of interest for residual strain mapping and providing a complementary view of the structure to understand the measured strain field. These measurement capabilities are demonstrated using several strain mapping examples ranging from polycrystalline structural alloys to biological materials. We also provide some guidance for the future users of the program for a successful residual strain mapping experiment. We are expanding the capabilities of the new setup with various in situ capabilities including thermo-mechanical loading.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

High-energy-resolution inelastic X-ray scattering spectrometer at beamline 30-ID of the Advanced Photon Source

Inelastic X-ray scattering is a powerful and versatile technique for studying lattice dynamics in materials of scientific and technological importance. In this article, the design and capabilities of the momentum-resolved high-energy-resolution inelastic X-ray spectrometer (HERIX) at beamline 30-ID of the Advanced Photon Source are reported. The instrument operates at 23.724 keV and has an energy resolution of 1.3–1.7 meV. It can accommodate momentum transfers of up to 72 nm -1 , at a typical X-ray flux of 4.5 × 10 9 photons s -1 meV -1 at the sample. A suite of in situ sample environments are provided, including high pressure, static magnetic fields and uniaxial strains, all at high or cryogenic temperatures.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

A High-Speed, High-Resolution Transition Edge Sensor Spectrometer for Soft X-Rays at the Advanced Photon Source

This project explores the design and development of a transition edge sensor (TES) spectrometer for resonant soft X-ray scattering (RSXS) measurements developed in collaboration between Argonne National Laboratory (ANL) and the National Institute of Standards and Technology (NIST). Soft X-ray scattering is a powerful technique for studying the electronic and magnetic properties of materials on a microscopic level. However, the lack of high-performance soft X-ray spectrometers has limited the potential of this technique. TES spectrometers have the potential to overcome these limitations due to their high energy resolution, high efficiency, and broad energy range. This project aims to optimize the design of a TES spectrometer for RSXS measurements and more generally soft X-ray spectroscopy at the Advanced Photon Source (APS) 29-ID, leading to improved understanding of advanced materials. We will present a detailed description of the instrument design and implementation. The spectrometer consists of a large array of approximately 250 high-speed and high-resolution pixels. The pixels have saturation energies of approximately 1 keV, sub-ms pulse duration and energy resolution of approximately 1 eV. The array is read out using microwave multiplexing chips with MHz bandwidth per channel, enabling efficient data throughput. To facilitate measurement of samples in situ under ultra-high vacuum conditions at the beamline, the spectrometer is integrated with an approximately 1 m long snout.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Repeatability and sensitivity characterization of the far-field high-energy diffraction microscopy instrument at the Advanced Photon Source

In the last two decades, far-field high-energy diffraction microscopy (FF-HEDM) and similar non-destructive techniques have been actively developed at synchrotron light sources around the world. As these techniques (and associated analysis tools) are becoming more available for the general users of these light sources, it is important and timely to characterize their performance and capabilities. In this work, the FF-HEDM instrument implemented at the 1-ID-E endstation of the Advanced Photon Source (APS) is summarized. The set of measurements conducted to characterize the instrument's repeatability and sensitivity to changes in grain orientation and position are also described. When an appropriate grain matching method is used, the FF-HEDM instrument's repeatability is approximately 5 µm in translation, 0.02° in rotation, and 2 × 10 −4 in strain; the instrument sensitivity is approximately 5 µm in translation and 0.05° in rotation.

3DXRD↗

HPCAT: A Static Compression Science Sector at the Advance Photon Source

Static compression is a useful tool to investigate the materials properties and phase behavior both under uniaxial stress and hydrostatic pressure. From evaluation of the equation of state (P-V-T relationship) to a discovery of near-room temperature superconductivity, the use of diamond anvil cells (DAC) and large-volume presses (LVP) as devices for static compression experiments that couple with synchrotron-based x-ray diffraction, spectroscopy, and imaging techniques achieved pioneering, paradigm defining scientific advancements in multidisciplinary fields for the past two decades. High-Pressure Collaborative Access Team (HPCAT) is a sector at the Advanced Photon Source dedicated to developing multiple synchrotron-based x-ray techniques to maximize the utility of DAC and portable-LVP techniques to advance compression science. The beamlines are optimized to adapt various sample environments under extreme P-T conditions. HPCAT is comprised of two insertion device beamlines, one for diffraction and the other for spectroscopy, and two bending magnet beamlines, one for general purpose and the other for white-beam application, respectively. As a result, each beamline’s specification and applications are introduced.

36 MATERIALS SCIENCE↗

Beamline Spectroscopy of Integrated Circuits With Hard X-Ray Transition Edge Sensors at the Advanced Photon Source

At Argonne National Laboratory, we are developing hard X-ray (2 to 20 keV) Transition Edge Sensor (TES) arrays for beamline science. The significantly improved energy resolution provided by superconducting detectors compared to semiconductor-based energy-dispersive detectors, but with better collection efficiency than wavelength-dispersive instruments, will enable greatly improved X-ray emission and absorption spectroscopic measurements. Additionally, a prototype instrument with 24 microwave-frequency multiplexed pixels is now in testing at the Advanced Photon Source (APS) 1-BM beamline. Initial measurements show an energy resolution ten times better (150 eV compared to < 15 eV) than the silicon-drift detectors currently available to APS beamline users, and in particular demonstrate the ability to resolve closely-spaced emission lines in samples containing multiple transition metal elements, such as integrated circuits. Comparing fluorescence spectra of integrated circuits measured with our TESs at the beamline to those measured with silicon detectors, we find emission lines and elements largely hidden (e.g. Hf alongside Cu) from a semiconductor-based detector but well resolved by a TES. This directly shows the strengths of TES-based instruments in fluorescence mapping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Methods for operando coherent X-ray diffraction of battery materials at the Advanced Photon Source

Bragg coherent X-ray diffraction imaging has become valuable for visualization of the structural, morphological and strain evolution of crystals in operando electrode materials. As the electrode material particles (either in a single-crystal form or an aggregation form of single crystals) are evenly dispersed and randomly oriented in the electrode laminate, the submicrometer-sized coherent X-ray beam can be used to probe the local properties of electrode material crystals using two approaches. Coherent multi-crystal diffraction provides collective structural information of phase transitions in tens of crystals simultaneously as well as the individual behavior from single crystals, which are oriented at the Bragg condition in the X-ray illumination volume. Bragg coherent diffractive imaging enables one to monitor the evolution of the morphology and strain in individual crystals. This work explores and highlights the Bragg coherent X-ray diffraction measurements of battery electrode materials in operando conditions at the 34-ID-C beamline at the Advanced Photon Source. The experiment is demonstrated with NaNi 1/3 Fe 1/3 Mn 1/3 O 2 , a sodium-ion cathode material loaded in a half cell. Furthermore, the paper will discuss, in detail, the beamline setup, sample mounting and handling, alignment strategies and the data acquisition protocols.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

2D/3D cryo x-ray fluorescence imaging at the bionanoprobe at the advanced photon source

Trace elements, particularly metals, play very important roles in biological systems. Synchrotron-based hard X-ray fluorescence microscopy offers the most suitable capabilities to quantitatively study trace metals in thick biological samples, such as whole cells and tissues. In this manuscript, we have demonstrated X-ray fluorescence imaging of frozen-hydrated whole cells using the recent developed Bionanoprobe (BNP). The BNP provides spatial resolution down to 30 nm and cryogenic capabilities. Frozen-hydrated biological cells have been directly examined on a sub-cellular level at liquid nitrogen temperatures with minimal sample preparation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Data Management at the Advanced Photon Source

Data are crucial to the scientific discoveries enabled by experiments performed at the APS. Presently the APS generates approximately 10 PB of raw experimental data per year from its sixty-six operating beamlines that house over 100 unique instruments. This data is generated as a part of over 6,000 annual experiments performed by over 5,500 facility users each year. Similar to other synchrotrons, the amount of data generated at the APS continues to quickly increase due to beamline advances, such as new measurement techniques, technological advances in detectors, high-throughput instrumentation, multi-modal instruments that can acquire several measurements in a single experiment, and advanced data processing algorithms. This trend is expected to continue in the future. The revolutionized high-energy synchrotron facility proposed in the APS-U project will increase brightness and coherence, leading to further increases in data rates. Successful management of data is of vital importance to the current and future scientific productivity of the APS.

96 KNOWLEDGE MANAGEMENT AND PRESERVATION↗

SEM/EBSD Characterization of Baffle-Former Bolts Designated for High Energy X-ray Microscopy Studies at the Advanced Photon Source

This report documents the microstructural and surface characterization of two high-fluence baffle-former bolts (BFBs) harvested from a commercial pressurized water reactor (PWR) after nearly four decades of service. These bolts experienced extreme conditions including high neutron fluence, elevated temperatures, corrosive primary water, and sustained mechanical loads, all of which contribute to degradation mechanisms such as irradiation-assisted stress corrosion cracking (IASCC). Using scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), the study assessed bulk and near-surface microstructures, grain boundary characteristics, and in-service oxide layers. The results revealed significant differences between bolts exposed to 41 dpa and 29 dpa, including differences in recrystallization extent, deformation structures, and oxidation morphology. These findings establish critical baseline data for integration with advanced synchrotron-based high-energy X-ray microscopy (HEXM) and computational crystal plasticity models. Ultimately, the work supports improved mechanistic understanding and predictive capability regarding the long-term performance of reactor core internal components.

Lach, Tim [Oak Ridge National Laboratory (ORNL), O↗

High-Energy-Resolution Resonant Inelastic (Hard) X-ray Scattering (RIXS) at the Advanced Photon Source

Resonant Inelastic X-ray Scattering (RIXS) is a powerful technique for studying electronic excitations in a wide variety of complex materials and environments with momentum-, energy- and potentially polarization resolution. Since its inception, the development of RIXS instrumentation and scientific subjects of study have benefited from a closely intertwined evolution; improvements in energy resolution and throughput, spurred by specific scientific cases, have in turn made new subjects of study feasible. Early RIXS work in the late 1990s was aimed at the study of charge transfer excitations in transition metal oxides (TMO), including the high-Tc superconducting Cuprates, the Nickelates and Manganites, in which the lowest lying excitations across the optical gap at a few eV from the elastic line could be accessed. As the understanding of strongly correlated electron systems progressed, scientific inquiries were directed towards the orbital degrees of freedom: in many Mott insulators the crystal field splits the degeneracy of the active d-orbitals, and the transitions between levels, the dd excitations, generate spectral features at energy losses of <2 eV. These features could reliably be observed with the state-of-the-art resolution at the time of 100-200 meV. In 2008, a ground-breaking paper appeared, that established RIXS as a probe of magnetic excitations. Magnetism and magnetic ordering are central questions in the study of correlated electron systems, however associated spectral features (“magnons”) lie at a fraction of an eV or even in the sub-10meV regime. A significant advance in energy resolution was necessary to study pressing scientific subjects, including magnetic excitations, in the newly discovered Iridate systems. Also, in 2011 a comprehensive review of the RIXS technique was published, which coined the terms “direct RIXS" and “indirect RIXS" and suggested that, for transition metal compounds, RIXS is most productive when employed at L-absorption edges. Thus, research assignments were divided between the soft- x-ray and hard x-ray communities according to L-edge energies: compounds with 3-d elements to the soft, compounds with 5-d elements to the hard x-ray side and other elements somewhere in-between.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗