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At least 73 records · Page 4

Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

Flynn, G. J.

Synchrotron X-ray fluorescence analyses of stratospheric cosmic dust - New results for chondritic and low-nickel particles

Trace element abundance determinations were performed using synchrotron X-ray fluorescence on nine particles collected from the stratosphere and classified as cosmic. Improvements to the Synchrotron Light Source allowed the detection of all elements between Cr and Mo, with the exceptions of Co and As, in our largest particle. The minor and trace element abundance patterns of three Ni-depleted particles were remarkably similar to those of extraterrestrial igneous rocks. Fe/Ni and Fe/Mn ratios suggest that one of these may be of lunar origin. All nine particles exhibited an enrichment in Br, ranging from 1.3 to 38 times the C1 concentration. Br concentrations were uncorrelated with particle size, as would be expected for a surface correlated component acquires from the stratosphere.

Flynn, G. J.

High-resolution absorption cross sections of carbon monoxide bands at 295 K between 91.7 and 100.4 nanometers

Theoretical descriptions of the abundance and excitation of carbon monoxide in interstellar clouds require accurate data on the vacuum-ultraviolet absorption spectrum of the molecule. The 6.65 m spectrometer at the Photon Factory synchrotron light source was used to measure photoabsorption cross sections of CO features between 91.2 and 100.4 nm. These data were recorded at a resolving power of 170,000, more than 20 times greater than that used in previous work.

Stark, G.

Reflectance calibrations of AXAF mirror samples at absorption edges using synchrotron radiation

We are developing a system to calibrate reflectances of witness coupons to the AXAF flight mirrors at the National Synchrotron Light Source over the 0.05-12 keV energy range. These witness coupons will be coated in the same process as the AXAF mirror elements. One of the key issues is the accurate determination of mirror efficiencies across the absorption edges of the mirror coating elements. We present a series of reflectance measurements with 2 eV resolution of a nickel-coated flat mirror in the region of the Ni L-II (870 eV) and L-III (853 eV) absorption edges. Scans of reflectance versus grazing angle at fixed energies in this region show distinct interference fringes at grazing angles larger than the critical angle which are extinguished as the photon energy is increased beyond the low point of the L-III edge, indicating total absorption of the evanescent wave within the Ni film. At 51 arc minutes grazing angle, measured reflectance decreases smoothly by 35 percent and then recovers in an 8 eV band at the L-III edge. We have also measured reflectances in the M absorption edge region for gold, platinum, and iridium coated mirrors. We derive optical parameters n and k specific to the film for comparison to the existing data tables.

Graessle, D. E.

Multilayer diffraction at 104 keV

We have measured the diffraction peak of a W:Si synthetic multilayer reflector at 104 keV using the High Energy Bonse-Hart Camera at the X-17B hard X-ray wiggler beam line of the National Synchrotron Light Source at Brookhaven National Laboratory. The characteristics of the diffraction peak are described and compared to theory.

Krieger, Allen S.

Feasibility study of the use of synchrotron radiation in the calibration of AXAF - Initial reflectivity results

The 1-percent calibration accuracy goal of the Advanced X-ray Astrophysics Facility is being approached by way of an experiment at the National Synchrotron Light Source that will demonstrate the accuracy achievable in reflectance measurements conducted on coated flat mirrors in the 50 eV-12 keV energy range. The coatings will be of commercially produced Au, Ni, and Ir, deposited either by sputtering or by e-beam deposition. Optical constants will be estimated via the reflectance vs. angle-of-incidence method.

Graessle, D. E.

Processing of semicrystalline polymers

Our research group has been interested in the processing-structure-property relationships in semicrystalline polymers and blends for many years. In situ real time x ray scattering at elevated temperatures is being used to monitor the development of structure. An ongoing collaboration with Dr. Malcolm Capel at the Brookhaven National Synchrotron Light Source allows the performance of real time wide and small angle x ray scattering to study the phase transformations in semicrystalline polymers. The first part of my presentation will be about our recent use of x ray scattering to study blends of poly(ethylene terephthalate) with polyarylates. The purpose of the next portion of the presentation is to show how we may study effects of self-deformation of polymers during processing in the gravity environment, using real time x ray scattering. In this way, how processing stresses alter the microstructure of semicrystalline polymers was learned, and ultimately microgravity processing strategies that will result in more uniform morphology in these polymers is hoped to be developed.

Cebe, Peggy

Trace Element Abundance Measurements on Cosmic Dust Particles

The X-Ray Microprobe on beamline X-26A at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory was used to determine the abundances of elements from Cr through Sr in individual interplanetary dust particles (IDPs) collected from the Earth's stratosphere and the Scanning Transmission X-ray Microscope (STXM) on beamline X-1A at the NSLS was used to determine the carbon abundances and spatial distributions in IDPs. In addition, modeling was performed in an attempt to associate particular types of IDPs with specific types of parent bodies, and thus to infer the chemistry, mineralogy, and structural properties of those parent bodies.

Flynn, George

X-Ray Topography of Tetragonal Lysozyme Grown by the Temperature-Controlled Technique

Growth-induced defects in lysozyme crystals were observed by white-beam and monochromatic X-ray topography at the National Synchrotron Light Source (NSLS) at the Brookhaven National Laboratory (BNL). The topographic methods were non-destructive to the extent that traditional diffraction data collection could be performed to high resolution after topography. It was found that changes in growth parameters, defect concentration as detected by X-ray topography, and the diffraction quality obtainable from the crystals were all strongly correlated. In addition, crystals with fewer defects showed lower mosaicity and higher diffraction resolution as expected.

Stojanoff, V.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Treiman, A. H.

Performance Verification of the Gravity and Extreme Magnetism Small Explorer GEMS X-Ray Polarimeter

olarimetry is a powerful tool for astrophysical observations that has yet to be exploited in the X-ray band. For satellite-borne and sounding rocket experiments, we have developed a photoelectric gas polarimeter to measure X-ray polarization in the 2-10 keV range utilizing a time projection chamber (TPC) and advanced micro-pattern gas electron multiplier (GEM) techniques. We carried out performance verification of a flight equivalent unit (1/4 model) which was planned to be launched on the NASA Gravity and Extreme Magnetism Small Explorer (GEMS) satellite. The test was performed at Brookhaven National Laboratory, National Synchrotron Light Source (NSLS) facility in April 2013. The polarimeter was irradiated with linearly-polarized monochromatic X-rays between 2.3 and 10.0 keV and scanned with a collimated beam at 5 different detector positions. After a systematic investigation of the detector response, a modulation factor greater than or equal to 35% above 4 keV was obtained with the expected polarization angle. At energies below 4 keV where the photoelectron track becomes short, diffusion in the region between the GEM and readout strips leaves an asymmetric photoelectron image. A correction method retrieves an expected modulation angle, and the expected modulation factor, approximately 20% at 2.7 keV. Folding the measured values of modulation through an instrument model gives sensitivity, parameterized by minimum detectable polarization (MDP), nearly identical to that assumed at the preliminary design review (PDR).

Time Projection

3d Crystallographic Orientation of Olivine in Bjurböle Chondrules

The crystallographic orientations of chondrule minerals can provide important insights into their formation and deformational history. For example, the orientations of the olivine bars and surrounding rim in barred olivine chondrules provide information and on the conditions of crystallization and the orientations and shapes of olivines within porphritic chondrules can record the reactions with the surrounding nebular gas during chondrule formation. Later deformation on the parent body can cause crystal-plastic deformation of chondrule minerals that is evident through their intracrystalline lattice misorientations. Typically these crystal orientations and lattice misorientations are determined using electron backscatter diffraction (EBSD) on thin sections but this gives only a 2D picture for what is actually a 3D texture. While it is possible to combine EBSD with serial sectioning to build a 3D dataset of texture, this is a destructive, time-intensive process. A recent technological development that enables non-destructive, 3D crystallographic orientation measurement is X-ray diffraction contrast tomography (DCT), which uses the X-ray diffraction of the crystal lattice to determine orientation. Originally only possible using monochromatic X-ray beams at 3rd generation synchrotron light sources, DCT has been recently adapted to polychromatic sources of laboratory X-ray microscopes (referred to as Lab-DCT). Up to this point LabDCT has only been applied to large, well-formed crystals of high symmetry (i.e., metals), but we recently acquired DCT datasets for a pair Bjurböle chondrules to determine the applicability of the technique to natural, mutlimineralic samples composed predominately of olivine (i.e., chondrules).

Hanna, R. D.

Determining the Quantum Detection Efficiency of A Soft X-Ray Micro-Channel Plate Detector for the Lunar Mission, LEXI

Micro-channel plate (MCP) detectors have long been a workhorse for space-based x-ray research and are advantageous over other imaging detectors because of their low size, weight and power. The Lunar Environment heliospheric x-ray Imager (LEXI), will utilize a MCP to image Earth’s magnetosphere in soft x-rays from the lunar surface. A critical element for interpreting on-orbit data is to understand the quantum detection efficiency (QDE) of the MCP. LEXI’s MCP is coated with potassium bromide (KBr) to increase the soft x-ray QDE. Historically, few measurements of QDE exist in the soft x-ray band for KBr detectors. This paper reviews the performance of LEXI’s detector, and the QDE experiment procedure conducted at and results from the Advanced Light Source synchrotron soft x-ray beam line (6.3.2) over the energy range 70eV-1300eV. A unique beam line setup was required to limit the photon flux as to not saturate the pores of the MCP or detector signal chain. The experimental results are similar to previous literature, with some caveats unique to this MCP and experimental setup.

X-ray imaging

Development of a Superconducting Adaptive Gap Undulator Prototype for NSLS-II

The photon flux and brightness of synchrotron radiation, crucial parameters for any light source, vary significantly depending on the type of source employed. Among the 23 Insertion Device (ID) sources at the National Synchrotron Light Source II (NSLS-II) at Brookhaven National Lab (BNL), the 12-year-old 3m-long In-Vacuum Undulator (IVU20) stands out for its superior performance, although it no longer represents the cutting edge of technology. Recently, there has been a shift in focus towards developing next-generation sources, particularly Superconducting Undulators (SCUs), characterized by smaller gaps, shorter periods, and maximum lengths. However, despite ongoing research and development efforts, SCUs have yet to surpass their predecessors, the Cryogenic Permanent Magnet Undulators (CPMUs), in terms of performance. This is largely attributed to the limitations posed by traditional superconducting wire, as well as challenges in the design of the magnetic structure and vacuum chamber. In this paper, we aim to overcome such limitations through the development of a unique prototype Superconducting Adaptive Gap Undulator (SC-AGU) magnet core and vacuum chamber design. This paper will outline a novel technical approach aimed at constructing a compact prototype magnet array utilizing state-of-the-art superconducting wire technology. This approach provides a more efficient magnetic structure, allowing for enhanced magnetic field strength and stability.

36 MATERIALS SCIENCE

Hard X-ray imaging with sub-10 nm resolution by scanning bonded 2D multilayer Laue lenses

Multilayer Laue lenses (MLLs) offer significant advantages over traditional diffractive focusing optics, such as zone plates (ZPs), in terms of efficiency and durability when focusing hard X-rays to 10 nm and below. Typically, a pair of 1D MLLs is aligned independently to achieve point focusing. This approach only permits scanning microscopy by moving the sample stage, which presents a limitation when it comes to scanning large or bulky objects at high speed. In this study, we present an experimental demonstration of scanning monolithically bonded 2D MLLs while keeping the sample stationary, effectively addressing the limitation of the sample’s size and weight. We characterized the system’s positional and angular stabilities during scanning, which are critical parameters to the nanofocusing performance of MLLs. In addition, we provided the X-ray measurement results and corresponding image resolution analysis.

36 MATERIALS SCIENCE

Reaction Mechanism of Electrodeposited ε-MnO 2 : A Proton-Centered Pathway in Aqueous Zn-Ion Systems

Aqueous Zn/MnO 2 batteries have garnered significant interests owing to their abundance, high theoretical specific capacity, safety, and low cost. However, large-scale application of these systems is limited by the incomplete understanding of the MnO 2 reaction chemistry. The different crystal lattice structures among MnO 2 polymorphs contribute to the variations in reported reaction mechanisms. Among them, ε-MnO 2 polymorph, the dominant phase in electrolytic manganese dioxide (EMD), is notably observed during the charge cycles of aqueous Zn/MnO 2 batteries. Here, in this work, we investigate the electrochemical behavior of an ε-MnO 2 cathode synthesized via electrodeposition from a ZnSO 4 and MnSO 4 electrolyte, onto a 3-dimensional carbon cloth substrate. Proton intercalation emerges as the dominant charge storage mechanism, critically enabling the reversibility of ε-MnO 2 during cycling, as revealed by operando synchrotron X-ray diffraction and X-ray absorption spectroscopy. Additionally, a proton-coupled dissolution/redeposition pathway operates alongside minor Zn 2+ intercalation, as quantified by Rietveld refinement. Morphological and chemical heterogeneities are studied by transmission X-ray microscopy further validates this reaction mechanism. These mechanistic insights provide the foundation for rationally designing Zn/MnO 2 batteries with optimized proton dynamics and charge transfer, advancing these systems as a viable solution for safe, cost-effective grid-scale energy storage.

36 MATERIALS SCIENCE

Advanced monolithic 2D multilayer Laue lens (MLL) optics for hard x-ray nanofocusing and nanotomography

We report on the development of a new generation of monolithic two-dimensional (2D) multilayer Laue lens (MLL) optics suitable for high-resolution hard x-ray nanoimaging. The 2D optics were assembled on microfabricated silicon templates with high orthogonality and lateral alignment precision, which were characterized using white-light interferometry and confirmed by x-ray measurements. The developed monolithic 2D MLL optics were successfully employed for hard x-ray nanofocusing and nanotomography experiments using the ptychography imaging modality, demonstrating sub-10 nm resolution in 2D and sample-limited ∼30 nm in three-dimensional while exhibiting excellent stability during extended measurements. The new 2D MLL templates with high alignment accuracy represent an important step forward in the development of 2D MLL optics toward direct nanoimaging experiments with sub-10 nm spatial resolution.

36 MATERIALS SCIENCE