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At least 55 records · Page 3

In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a pinhole camera (transmission geometry, flat two-dimensional detector perpendicular to the direct beam), the instrument (which we call CHEMIN, for Chemistry and Mineralogy) uses an X-ray sensitive CCD detector which will allow concurrent positional and energy-dispersive analysis of collected photons. Thus XRF (energy) and XRD (geometry) analysis of transmitted X-rays will be performed at the same time. Tests performed with single minerals and simple mixtures give promising results. Refinements of the prototype promise interpretable results on complex samples.

Sarrazin, P.↗

Understanding Electrochemical Sulfur-Based Phase Evolution via Complementary Insight from Operando Spatially Resolved X-ray Diffraction and X-ray Absorption Spectroscopy

Lithium/sulfur batteries are emerging as promising candidates for use in large-scale energy storage, but practical challenges, including insufficient power density and polysulfide shuttling, remain. Here, this work presents the first use of operando energy dispersive X-ray diffraction (EDXRD) to monitor Li/S electrochemistry within a liquid electrolyte. Complementary operando synchrotron-based EDXRD, X-ray absorption spectroscopy (XAS), X-ray powder diffraction (XPD), and ex situ laboratory Raman analysis provide evidence for α-S 8 conversion upon discharge into Li 2 S x polysulfide phases and conversion into β-S 8 during charge. Understanding the underlying mechanisms of sulfur reduction and oxidation within thick electrodes will enable advances in next-generation Li/S batteries and material design.

36 MATERIALS SCIENCE↗

Hard X-Ray Emission of X-Ray Bursters

The main results from this investigation were serendipitous. The long observation approved for the study of the hard X-ray emission of X-ray bursters lead, instead, to one of the largest early samples of the behavior of fast quasi-periodic oscillations (QPOS) in an atoll sources. Our analysis of this data set lead to the several important discoveries including the existence of a robust correlation between QPO frequency and the flux of a soft blackbody component of the X-ray spectrum in the atoll source 4U 0614+091.

Kaaret, Phillip↗

Long Term Hard X-ray Monitoring of X-ray Bursters

This grant supported our analysis of BATSE occultation data on x-ray bursters and neutron star low mass x-ray binaries (LMXBs) from the Compton Gamma-ray Observatory carried out under observing cycle 6. The work carried out under this grant was closely related to our separate investigation (NAG5-3808) to develop a prototype BATSE imaging survey for faint transients. In this Final Report, we summarize the Scientific Objectives of this investigation of hard x-ray studies of bursters and the Results Achieved; and finally the Papers Published.

Grindlay, Jonathan E.↗

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↗

Origins of X-ray Line Emissions in Circinus X-1 at Very Low X-ray Flux

Accretion conditions and morphologies of X-ray transients containing neutron stars are still poorly understood. Circinus X-1 is an enigmatic case where we observe X-ray flux changes covering four orders of magnitude. We observed Circinus X-1 several times at its very lowest X-ray flux using the high-energy transmission grating spectrometer on board the Chandra X-ray Observatory. At a flux of 1.8 ´ 10-11 erg cm−2 s−1 we observed a single 1.6 keV blackbody spectrum. The observed continuum luminosity of 1035 erg s−1 is about two orders of magnitude too low to explain the observed photoionized luminosity, suggesting a much more complex structure of the X-ray source that is partially or entirely obscured, as had been previously suggested. This affects most emissions from the accretion disk, including previously observed accretion-disk coronal line emissions. Instead, the strongest observed photoionized lines are blueshifted by about ∼400 km s−1, and we suggest that they originate in the ionized wind of a B5Ia supergiant companion, supporting a previous identification. The neutron star in Cir X-1 is very young and should have a high magnetic field. At the observed luminosity, the emission radius of the blackbody is small enough to be associated with the accretion hot spot as the X-ray-emitting region. The small emission radius then points to a field strength below 1012 G, which would be consistent with the observation of occasional type I X-ray bursts at high magnetic fields. We discuss Cir X-1 in the context of being a high-mass X-ray binary, with some emphasis on a possible Be-star X-ray binary nature.

N S Schulz↗

Demonstration of a laser-driven, narrow spectral bandwidth x-ray source for collective x-ray scattering experiments

X-ray Thomson scattering (XRTS) is a powerful diagnostic technique that involves an x-ray source interacting with a dense plasma sample, resulting in a spectrum of elastically and inelastically scattered x-rays. Depending on the plasma conditions, one can measure a range of parameters from the resulting spectrum, including plasma temperature, electron density, and ionization state. To achieve sensitivity to collective electron oscillations, XRTS measurements require limited momentum transfer where the spectral separation of elastic and inelastic scattering is small. Such measurements require an x-ray probe source with a narrow bandwidth in order to reduce the spectral overlap between scattering contributions, allowing for the different features to be more precisely deconvolved. In this investigation, we discuss the theory behind how the bandwidth for a common XRTS probe, Zn He-α emission at 9 keV, can be reduced using a Cu K-edge filter.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Correlative single-cell hard X-ray computed tomography and X-ray fluorescence imaging

Abstract X-ray computed tomography (XCT) and X-ray fluorescence (XRF) imaging are two non-invasive imaging techniques to study cellular structures and chemical element distributions, respectively. However, correlative X-ray computed tomography and fluorescence imaging for the same cell have yet to be routinely realized due to challenges in sample preparation and X-ray radiation damage. Here we report an integrated experimental and computational workflow for achieving correlative multi-modality X-ray imaging of a single cell. The method consists of the preparation of radiation-resistant single-cell samples using live-cell imaging-assisted chemical fixation and freeze-drying procedures, targeting and labeling cells for correlative XCT and XRF measurement, and computational reconstruction of the correlative and multi-modality images. With XCT, cellular structures including the overall structure and intracellular organelles are visualized, while XRF imaging reveals the distribution of multiple chemical elements within the same cell. Our correlative method demonstrates the feasibility and broad applicability of using X-rays to understand cellular structures and the roles of chemical elements and related proteins in signaling and other biological processes.

59 BASIC BIOLOGICAL SCIENCES↗

X-ray emission from cataclysmic variables with accretion disks. I - Hard X-rays. II - EUV/soft X-ray radiation

Theoretical models explaining the hard-X-ray, soft-X-ray, and EUV emission of accretion-disk cataclysmic variables in terms of the disk boundary layer (DBL) are developed on the basis of a survey of the published observational data. The data are compared with model predictions in graphs for systems with high or low (greater than or less than 10-Pg/s) accretion rates. Good agreement is obtained both at low accretion rates, where an optically thin rarefied hot (Te = 10 to the 8th K) DBL radiates most of its energy as hard X-rays, and at high accretion rates, where an optically thick 100,000-K DBL radiates most of its energy in the EUV and as soft X-rays. Detailed analysis of the old nova V603 Aql suggests that previous models predicting more detections of soft-X-ray/EUV emissions from thick-DBL objects (Ferland et al., 1982) used inappropriate dwarf masses, interstellar column densities, or classical-nova space densities.

Patterson, J.↗

"X-Ray Transients in Star-Forming Regions" and "Hard X-Ray Emission from X-Ray Bursters"

This grant funded work on the analysis of data obtained with the Burst and Transient Experiment (BATSE) on the Compton Gamma-Ray Observatory. The goal of the work was to search for hard x-ray transients in star forming regions using the all-sky hard x-ray monitoring capability of BATSE. Our initial work lead to the discovery of a hard x-ray transient, GRO J1849-03. Follow-up observations of this source made with the Wide Field Camera on BeppoSAX showed that the source should be identified with the previously known x-ray pulsar GS 1843-02 which itself is identified with the x-ray source X1845-024 originally discovered with the SAS-3 satellite. Our identification of the source and measurement of the outburst recurrence time, lead to the identification of the source as a Be/X-ray binary with a spin period of 94.8 s and an orbital period of 241 days. The funding was used primarily for partial salary and travel support for John Tomsick, then a graduate student at Columbia University. John Tomsick, now Dr. Tomsick, received his Ph.D. from Columbia University in July 1999, based partially on results obtained under this investigation. He is now a postdoctoral research scientist at the University of California, San Diego.

Halpern, Jules P.↗

Structural Evolution of Photoexcited Methylcobalamin toward a CarH-like Metastable State: Evidence from Time-Resolved X-ray Absorption and X-ray Emission

CarH is a protein photoreceptor that uses a form of B 12 , adenosylcobalamin (AdoCbl), to sense light via formation of a metastable excited state. Aside from AdoCbl bound to CarH, methylcobalamin (MeCbl) is the only other example – to date – of photoexcited cobalamins forming metastable excited states with lifetimes of nanoseconds or longer. The UV-visible spectra of the excited states of MeCbl and AdoCbl bound to CarH are similar. We have used transient Co K-edge X-ray absorption and X-ray emission spectroscopies in conjunction with transient absorption spectroscopy in the UV–visible region to characterize the excited states of MeCbl. These data show that the metastable excited state of MeCbl has a slightly expanded corrin ring and increased electron density on the cobalt, but only small changes in the axial bond lengths. Finally, this is similar to changes seen previously for CarH, suggesting that MeCbl may be a good model for AdoCbl in CarH.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CubeX: A Compact X-Ray Telescope Enables Both X-Ray Fluorescence Imaging Spectroscopy and Pulsar Timing Based Navigation

This paper describes the benefits of a miniaturized X-ray telescope payload in the context of a lunar mission. The first part describes the payload in detail, the second part summarizes a small satellite mission concept that utilizes its compact form factor and performance. The CubeX instrument can be used for both X-ray fluorescence (XRF) imaging spectroscopy and X-ray pulsar timing based navigation (XNAV). Using our recent technological advances in X-ray optics and sensors, CubeX combines high angular resolution (<1 arcminutes) Miniature Wolter-I X-ray optics (MiXO) with a common focal plane consisting of high spectral resolution (<150 eV at 1 keV) CMOS X-ray sensors and a high timing resolution (< 1 usec) SDD X-ray sensor. This novel combination of the instruments enables both XRF measurements and XNAV operations without moving parts. The high angular resolution of the MiXO opens a wide range of orbital configurations for observation. Given that performance, the instrument has unprecedented small volume (~1×1×6U), mass (<6 kg), and power (<9W) requirements and opens a wide range of applications for a variety of targets and missions including NEOs and Martian moons. In this paper we illustrate one potential application for a lunar mission concept: The elemental composition of the Moon holds keys to understanding the origin and evolution of both the Moon and the Earth. X-ray fluorescence (XRF), induced either by solar X-ray flux or energetic ions, carries decisive signatures of surface elemental composition. X-ray observations, therefore, give a unique, powerful diagnostic tool for remotely determining elemental abundances including major rock forming elements such as Mg, Al, Na, Si, Fe, and Ca. Through high-resolution XRF imaging spectroscopy, CubeX searches for small patches of elusive lower crust and mantle material excavated within and around impact craters. CubeX identifies regional compositional variations and allows straightforward comparison of elemental distributions with the surface topography from LRO and the gravity data from GRAIL. The elemental compositions of the lower crust and the mantle are sensitive to the conditions of the giant impact which led to the Moon's formation and the subsequent lunar magma ocean (LMO), and thus they are key missing pieces in understanding the formation and early evolution of the Moon. In between XRF observations, CubeX also leverages the technology of high resolution X-ray imaging and time series measurements to conduct XNAV operations and evaluate their performance. Deep space navigation is a critical issue for small planetary missions. XNAV can enable low-cost autonomous deep-space navigation, and has the potential to greatly assist, or even outperform, NASA's Deep Space Network (DSN) or ESA's European Space Tracking (ESTRACK). CubeX is designed to perform sequential observations of 3-4 millisecond pulsars (MSPs) to solve the spacecraft trajectory for absolute navigation, and explore the remote sensing capability of XNAV. In the presented mission concept, the Moon's relative proximity enables a straightforward evaluation of the XNAV performance through DSN.

x-ray spectroscopy↗

Cubex: A Compact X-Ray Telescope Enables Both X-Ray Fluorescence Imaging Spectroscopy and Pulsar Timing Based Navigation

This paper describes the miniaturized X-ray telescope payload, CubeX, in the context of a lunar mission. The first part describes the payload in detail, the second part summarizes a small satellite mission concept that utilizes its compact form factor and performance. This instrument can be used for both X-ray fluorescence (XRF) imaging spectroscopy and X-ray pulsar timing-based navigation (XNAV). It combines high angular resolution (<1 arcminutes) Miniature Wolter-I X-ray optics (MiXO) with a common focal plane consisting of high spectral resolution (<150 eV at 1 keV) CMOS X-ray sensors and a high timing resolution (< 1 Amp-microsecond) SDD X-ray sensor. This novel combination of the instruments enables both XRF measurements and XNAV operations without moving parts, in a small form factor (volume approximately 1 by 1 by 6 Units, and mass, < 6 kg). In this paper we illustrate one potential application for a lunar mission concept: The elemental composition of the Moon holds keys to understanding the origin and evolution of both the Moon and the Earth. X-ray fluorescence (XRF), induced either by solar X-ray flux or energetic ions, carries decisive signatures of surface elemental composition. In between XRF observations, CubeX also leverages the technology of high resolution X-ray imaging and time series measurements to conduct XNAV operations and evaluate their performance.

X-ray Fluorescence↗

Diamond formation kinetics in shock-compressed C$-$H$-$O samples recorded by small-angle x-ray scattering and x-ray diffraction

Extreme conditions inside ice giants such as Uranus and Neptune can result in peculiar chemistry and structural transitions, e.g., the precipitation of diamonds or superionic water, as so far experimentally observed only for pure C$-$H and H 2 O systems, respectively. Here, we investigate a stoichiometric mixture of C and H 2 O by shock-compressing polyethylene terephthalate (PET) plastics and performing in situ x-ray probing. We observe diamond formation at pressures between 72 ± 7 and 125 ± 13 GPa at temperatures ranging from ~3500 to ~6000 K. Combining x-ray diffraction and small-angle x-ray scattering, we access the kinetics of this exotic reaction. The observed demixing of C and H 2 O suggests that diamond precipitation inside the ice giants is enhanced by oxygen, which can lead to isolated water and thus the formation of superionic structures relevant to the planets’ magnetic fields. Moreover, our measurements indicate a way of producing nanodiamonds by simple laser-driven shock compression of cheap PET plastics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A Broad-Band X-Ray Telescope spectrum of the massive X-ray binary X Persei

The Broad Band X-Ray Telescope, covering the 0.3-12 keV bandpass with moderate spectral resolution, observed the Be/X-ray binary X Per in 1990 December during the Astro-l mission on the Space Shuttle Columbia. The data obtained are the best to date to search for lines and edges. The data are well fitted by a power-law spectrum with a high-energy cutoff. A low value for the high-energy cutoff is found, implying a slightly weaker magnetic field strength for the X-ray pulsar. No iron line is present at about 6.5 keV with an equivalent width greater than 30-40 eV. The BBXRT observation corresponded to the 'off' state of X Per's recent 'phase change'.

Schlegel, Eric M.↗

Glancing incidence X-ray optics for solar X-ray astronomy

Glancing incidence X-ray optics have been developed into a highly valuable tool for high-resolution investigations of the sun in the X-ray/XUV regime. A brief overview of the development of X-ray optics technology is presented. Techniques currently under study for increasing the plate scale and improving the off-axis performance of future X-ray telescopes for solar X-ray astronomy are briefly discussed.

Hoover, Richard B.↗

Modeling the X-Ray Process, and X-Ray Flaw Size Parameter for POD Studies

Nondestructive evaluation (NDE) method reliability can be determined by a statistical flaw detection study called probability of detection (POD) study. In many instances the NDE flaw detectability is given as a flaw size such as crack length. The flaw is either a crack or behaving like a crack in terms of affecting the structural integrity of the material. An alternate approach is to use a more complex flaw size parameter. The X-ray flaw size parameter, given here, takes into account many setup and geometric factors. The flaw size parameter relates to X-ray image contrast and is intended to have a monotonic correlation with the POD. Some factors such as set-up parameters including X-ray energy, exposure, detector sensitivity, and material type that are not accounted for in the flaw size parameter may be accounted for in the technique calibration and controlled to meet certain quality requirements. The proposed flaw size parameter and the computer application described here give an alternate approach to conduct the POD studies. Results of the POD study can be applied to reliably detect small flaws through better assessment of effect of interaction between various geometric parameters on the flaw detectability. Moreover, a contrast simulation algorithm for a simple part-source-detector geometry using calibration data is also provided for the POD estimation.

Khoshti, Ajay↗

Modeling the X-ray Process, and X-ray Flaw Size Parameter for POD Studies

Nondestructive evaluation (NDE) method reliability can be determined by a statistical flaw detection study called probability of detection (POD) study. In many instances, the NDE flaw detectability is given as a flaw size such as crack length. The flaw is either a crack or behaving like a crack in terms of affecting the structural integrity of the material. An alternate approach is to use a more complex flaw size parameter. The X-ray flaw size parameter, given here, takes into account many setup and geometric factors. The flaw size parameter relates to X-ray image contrast and is intended to have a monotonic correlation with the POD. Some factors such as set-up parameters, including X-ray energy, exposure, detector sensitivity, and material type that are not accounted for in the flaw size parameter may be accounted for in the technique calibration and controlled to meet certain quality requirements. The proposed flaw size parameter and the computer application described here give an alternate approach to conduct the POD studies. Results of the POD study can be applied to reliably detect small flaws through better assessment of effect of interaction between various geometric parameters on the flaw detectability. Moreover, a contrast simulation algorithm for a simple part-source-detector geometry using calibration data is also provided for the POD estimation.

Koshti, Ajay M.↗